Figure 3. The simulated temperature distribution and single-layer multi-track isothermograms of LPBF Hastelloy X, located at the bottom of the powder bed, are presented for various laser energy densities. (a) depicts the single-point temperature distribution at the bottom of the powder bed, followed by the isothermograms corresponding to laser energy densities of (b) 31 J/mm3 , (c) 43 J/mm3 , (d) 53 J/mm3 , (e) 67 J/mm3 , and (f) 91 J/mm3 .

An integrated multiscale simulation guiding the processing optimisation for additively manufactured nickel-based superalloys

적층 가공된 니켈 기반 초합금의 가공 최적화를 안내하는 통합 멀티스케일 시뮬레이션

Xing He, Bing Yang, Decheng Kong, Kunjie Dai, Xiaoqing Ni, Zhanghua Chen
& Chaofang Dong

ABSTRACT

Microstructural defects in laser powder bed fusion (LPBF) metallic materials are correlated with processing parameters. A multi-physics model and a crystal plasticity framework are employed to predict microstructure growth in molten pools and assess the impact of manufacturing defects on plastic damage parameters. Criteria for optimising the LPBF process are identified, addressing microstructural defects and tensile properties of LPBF Hastelloy X at various volumetric energy densities (VED). The results show that higher VED levels foster a specific Goss texture {110} <001>, with irregular lack of fusion defects significantly affecting plastic damage, especially near the material surface. A critical threshold emerges between manufacturing defects and grain sizes in plastic strain accumulation. The optimal processing window for superior Hastelloy X mechanical properties ranges from 43 to 53 J/mm3 . This work accelerates the development of superior strengthductility alloys via LPBF, streamlining the trial-and-error process and reducing associated costs.

Figure 3. The simulated temperature distribution and single-layer multi-track isothermograms of LPBF Hastelloy X, located at the bottom of the powder bed, are presented for various laser energy densities. (a) depicts the single-point temperature distribution at the bottom of the powder bed, followed by the isothermograms corresponding to laser energy densities of (b) 31 J/mm3 , (c) 43 J/mm3 , (d) 53 J/mm3 , (e) 67 J/mm3 , and (f) 91 J/mm3 .
Figure 3. The simulated temperature distribution and single-layer multi-track isothermograms of LPBF Hastelloy X, located at the bottom of the powder bed, are presented for various laser energy densities. (a) depicts the single-point temperature distribution at the bottom of the powder bed, followed by the isothermograms corresponding to laser energy densities of (b) 31 J/mm3 , (c) 43 J/mm3 , (d) 53 J/mm3 , (e) 67 J/mm3 , and (f) 91 J/mm3 .

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Figure 1. Experimental setup and materials. (a) Schematic of the DED process, where three types of base materials were adopted—B1 (IN718), B2 (IN625), and B3 (SS316L), and two types of powder materials were adopted—P1 (IN718) and P2 (SS316L). (b) In situ high-speed imaging of powder flow and the SEM images of IN718 and SS316L powder particle. (c) Powder size statistics, and (d) element composition of powder IN718 (P1) and SS316L (P2).

Printability disparities in heterogeneous materialcombinations via laser directed energy deposition:a comparative stud

Jinsheng Ning1,6, Lida Zhu1,6,∗, Shuhao Wang2, Zhichao Yang1, Peihua Xu1,Pengsheng Xue3, Hao Lu1, Miao Yu1, Yunhang Zhao1, Jiachen Li4, Susmita Bose5 and Amit Bandyopadhyay5,∗

Abstract

적층 제조는 바이메탈 및 다중 재료 구조의 제작 가능성을 제공합니다. 그러나 재료 호환성과 접착성은 부품의 성형성과 최종 품질에 직접적인 영향을 미칩니다. 적합한 프로세스를 기반으로 다양한 재료 조합의 기본 인쇄 가능성을 이해하는 것이 중요합니다.

여기에서는 두 가지 일반적이고 매력적인 재료 조합(니켈 및 철 기반 합금)의 인쇄 적성 차이가 레이저 지향 에너지 증착(DED)을 통해 거시적 및 미시적 수준에서 평가됩니다.

증착 프로세스는 현장 고속 이미징을 사용하여 캡처되었으며, 용융 풀 특징 및 트랙 형태의 차이점은 특정 프로세스 창 내에서 정량적으로 조사되었습니다. 더욱이, 다양한 재료 쌍으로 처리된 트랙과 블록의 미세 구조 다양성이 비교적 정교해졌고, 유익한 다중 물리 모델링을 통해 이종 재료 쌍 사이에 제시된 기계적 특성(미세 경도)의 불균일성이 합리화되었습니다.

재료 쌍의 서로 다른 열물리적 특성에 의해 유발된 용융 흐름의 차이와 응고 중 결과적인 요소 혼합 및 국부적인 재합금은 재료 조합 간의 인쇄 적성에 나타난 차이점을 지배합니다.

이 작업은 서로 다른 재료의 증착에서 현상학적 차이에 대한 심층적인 이해를 제공하고 바이메탈 부품의 보다 안정적인 DED 성형을 안내하는 것을 목표로 합니다.

Additive manufacturing provides achievability for the fabrication of bimetallic and
multi-material structures; however, the material compatibility and bondability directly affect the
parts’ formability and final quality. It is essential to understand the underlying printability of
different material combinations based on an adapted process. Here, the printability disparities of
two common and attractive material combinations (nickel- and iron-based alloys) are evaluated
at the macro and micro levels via laser directed energy deposition (DED). The deposition
processes were captured using in situ high-speed imaging, and the dissimilarities in melt pool
features and track morphology were quantitatively investigated within specific process
windows. Moreover, the microstructure diversity of the tracks and blocks processed with varied
material pairs was comparatively elaborated and, complemented with the informative
multi-physics modeling, the presented non-uniformity in mechanical properties (microhardness)
among the heterogeneous material pairs was rationalized. The differences in melt flow induced
by the unlike thermophysical properties of the material pairs and the resulting element
intermixing and localized re-alloying during solidification dominate the presented dissimilarity
in printability among the material combinations. This work provides an in-depth understanding
of the phenomenological differences in the deposition of dissimilar materials and aims to guide
more reliable DED forming of bimetallic parts.

Figure 1. Experimental setup and materials. (a) Schematic of the DED process, where three types of base materials were adopted—B1
(IN718), B2 (IN625), and B3 (SS316L), and two types of powder materials were adopted—P1 (IN718) and P2 (SS316L). (b) In situ
high-speed imaging of powder flow and the SEM images of IN718 and SS316L powder particle. (c) Powder size statistics, and (d) element
composition of powder IN718 (P1) and SS316L (P2).
Figure 1. Experimental setup and materials. (a) Schematic of the DED process, where three types of base materials were adopted—B1 (IN718), B2 (IN625), and B3 (SS316L), and two types of powder materials were adopted—P1 (IN718) and P2 (SS316L). (b) In situ high-speed imaging of powder flow and the SEM images of IN718 and SS316L powder particle. (c) Powder size statistics, and (d) element composition of powder IN718 (P1) and SS316L (P2).
Figure 2. Deposition process and the track morphology. (a)–(c) Display the in situ captured tableaux of melt propagation and some physical
features during depositing for P1B1, P1B2, and P1B3, respectively. (d) The profiles of the melt pool at a frame of (t0 + 1) ms, and the flow
streamlines in the molten pool of each case. (e) The outer surface of the formed tracks, in which the colored arrows mark the scanning
direction. (f) Cross-section of the tracks. The parameter set used for in situ imaging was P-1000 W, S-600 mm·min–1, F-18 g·min–1. All the
scale bars are 2 mm.
Figure 2. Deposition process and the track morphology. (a)–(c) Display the in situ captured tableaux of melt propagation and some physical features during depositing for P1B1, P1B2, and P1B3, respectively. (d) The profiles of the melt pool at a frame of (t0 + 1) ms, and the flow streamlines in the molten pool of each case. (e) The outer surface of the formed tracks, in which the colored arrows mark the scanning direction. (f) Cross-section of the tracks. The parameter set used for in situ imaging was P-1000 W, S-600 mm·min–1, F-18 g·min–1. All the scale bars are 2 mm.

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Fig. 3. (a–c) Snapshots of the CtFD simulation of laser-beam irradiation: (a) Top, (b) longitudinal vertical cross-sectional, and (c) transversal vertical cross-sectional views. (d) z-position of the solid/liquid interface during melting and solidification.

Solute segregation in a rapidly solidified Hastelloy-X Ni-based superalloy during laser powder bed fusion investigated by phase-field simulations and computational thermal-fluid dynamics

Masayuki Okugawa ab, Kenji Saito a, Haruki Yoshima a, Katsuhiko Sawaizumi a, Sukeharu Nomoto c, Makoto Watanabe c, Takayoshi Nakano ab, Yuichiro Koizumi abShow moreAdd to MendeleyShareCite

https://doi.org/10.1016/j.addma.2024.104079

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Abstract

Solute segregation significantly affects material properties and is a critical issue in the laser powder-bed fusion (LPBF) additive manufacturing (AM) of Ni-based superalloys. To the best of our knowledge, this is the first study to demonstrate a computational thermal-fluid dynamics (CtFD) simulation coupled multi-phase-field (MPF) simulation with a multicomponent-composition model of Ni-based superalloy to predict solute segregation under solidification conditions in LPBF. The MPF simulation of the Hastelloy-X superalloy reproduced the experimentally observed submicron-sized cell structure. Significant solute segregations were formed within interdendritic regions during solidification at high cooling rates of up to 10K s-1, a characteristic feature of LPBF. Solute segregation caused a decrease in the solidus temperature (TS), with a reduction of up to 30.4 K, which increases the risk of liquation cracks during LPBF. In addition, the segregation triggers the formation of carbide phases, which increases the susceptibility to ductility dip cracking. Conversely, we found that the decrease in TS is suppressed at the melt-pool boundary regions, where re-remelting occurs during the stacking of the layer above. Controlling the re-remelting behavior is deemed to be crucial for designing crack-free alloys. Thus, we demonstrated that solute segregation at the various interfacial regions of Ni-based multicomponent alloys can be predicted by the conventional MPF simulation. The design of crack-free Ni-based superalloys can be expedited by MPF simulations of a broad range of element combinations and their concentrations in multicomponent Ni-based superalloys.

Graphical abstract

Keywords

Laser powder-bed fusion, Hastelloy-X Nickel-based superalloy, solute element segregation, computational thermal-fluid dynamics simulation, phase-field method

1. Introduction

Additive manufacturing (AM) technologies have attracted considerable attention as they allow us to easily build three-dimensional (3D) parts with complex geometries. Among the wide range of available AM techniques, laser powder-bed fusion (LPBF) has emerged as a preferred technique for metal AM [1][2][3][4][5]. In LPBF, metal products are built layer-by-layer by scanning laser, which fuse metal powder particles into bulk solids.

Significant attempts have been made to integrate LPBF techniques within the aerospace industry, with a particular focus on weldable Ni-based superalloys, such as IN718 [6][7][8], IN625 [9][10], and Hastelloy-X (HX) [11][12][13][14]. Non-weldable alloys, such as IN738LC [15][16] and CMSX-4 [1][17] are also suitable for their sufficient creep resistance under higher temperature conditions. However, non-weldable alloys are difficult to build using LPBF because of their susceptibility to cracking during the process. In general, a macro solute-segregation during solidification is suppressed by the rapid cooling conditions (up to 108 K s-1) unique to the LPBF process [18]. However, the solute segregation still occurs in the interdendritic regions that are smaller than the micrometer scale [5][19][20][21]; these regions are suggested to be related to the hot cracks in LPBF-fabricated parts. Therefore, an understanding of solute segregation is essential for the fabrication of reliable LPBF-fabricated parts while avoiding cracks.

The multiphase-field (MPF) method has gained popularity for modeling the microstructure evolution and solute segregation under rapid cooling conditions [5][20][21][22][23][24][25][26][27][28]. Moreover, quantifiable predictions have been achieved by combining the MPF method with temperature distribution analysis methods such as the finite-element method (FEM) [20] and computational thermal-fluid dynamics (CtFD) simulations [28]. These aforementioned studies have used binary-approximated multicomponent systems, such as Ni–Nb binary alloys, to simulate IN718 alloys. While MPF simulations using binary alloy systems can effectively reproduce microstructure formations and segregation behaviors, the binary approximation might be affected by the chemical interactions between the removed solute elements in the target multicomponent alloy. The limit of absolute stability predicted by the Mullins-Sekerka theory [29] is also crucial because the limit velocity is close to the solidification rate in the LPBF process and is different in multicomponent and binary-approximated systems. The difference between the solidus and liquidus temperatures, ΔT0, directly determines the absolute stability according to the Mullins-Sekerka theory. For example, the ΔT0 values of IN718 and its binary-approximated Ni–5 wt.%Nb alloy are 134 K [28] and 71 K [30], respectively. The solidification rate compared to the limit of absolute stability, i.e., the relative non-equilibrium of solidification, changes by simplification of the system. It is therefore important to use the composition of the actual multicomponent system in such simulations. However, to the best of our knowledge, there is no MPF simulation using a multicomponent model coupled with a temperature analysis simulation to predict solute segregation in a Ni-based superalloy.

In this study, we demonstrate that the conventional MPF model can reproduce experimentally observed dendritic structures by performing a phase-field simulation using the temperature distribution obtained by a CtFD simulation of a multicomponent Ni-based alloy (conventional solid-solution hardening-type HX). The MPF simulation revealed that the segregation behavior of solute elements largely depends on the regions of the melt pool, such as the cell boundary, the interior of the melt-pool boundary, and heat-affected regions. The sensitivities of the various interfaces to liquation and solidification cracks are compared based on the predicted concentration distributions. Moreover, the feasibility of using the conventional MPF model for LPBF is discussed in terms of the absolute stability limit.

2. Methods

2.1. Laser-beam irradiation experiments

Rolled and recrystallized HX ingots with dimensions of 20 × 50 × 10 mm were used as the specimens for laser-irradiation experiments. The specimens were irradiated with a laser beam scanned along straight lines of 10 mm in length using a laser AM machine (EOS 290 M, EOS) equipped with a 400 W Yb-fiber laser. Irradiation was performed with a beam power of P = 300 W and a scanning speed of V = 600 mm s-1, which are the conditions generally used in the LPBF fabrication of Ni-based superalloy [8]. The corresponding line energy was 0.5 J mm-1. The samples were cut perpendicular to the beam-scanning direction for cross-sectional observation using a field-emission scanning electron microscope (FE-SEM, JEOL JSM 6500). Crystal orientation analysis was performed by electron backscatter diffraction (EBSD). The sizes of each crystal grain and their aspect ratios were evaluated by analyzing the EBSD data.

2.2. CtFD simulation

CtFD simulations of the laser-beam irradiation of HX were performed using a 3D thermo-fluid analysis software (Flow Science FLOW-3D® with Flow-3D Weld module). A Gaussian heat source model was used, in which the irradiation intensity distribution of the beam is regarded as a symmetrical Gaussian distribution over the entire beam. The distribution of the beam irradiation intensity is expressed by the following equation.(1)q̇=2ηPπR2exp−2r2R2.

Here, P is the power, R is the effective beam radius, r is the actual beam radius, and η is the beam absorption rate of the substrate. To improve the accuracy of the model, η was calculated by assuming multiple reflections using the Fresnel equation:(2)�=1−121+1−�cos�21+1+�cos�2+�2−2�cos�+2cos2��2+2�cos�+2cos2�.

ε is the Fresnel coefficient and θ is the incident angle of the laser. A local laser melt causes the vaporization of the material and results in a high vapor pressure. This vapor pressure acts as a recoil pressure on the surface, pushing the weld pool down. The recoil pressure is reproduced using the following equation.(3)precoil=Ap0exp∆HLVRTV1−TVT.

Here, p0 is the atmospheric pressure, ∆HLV is the latent heat of vaporization, R is the gas constant, and TV is the boiling point at the saturated vapor pressure. A is a ratio coefficient that is generally assumed to be 0.54, indicating that the recoil pressure due to evaporation is 54% of the vapor pressure at equilibrium on the liquid surface.

Table 1 shows the parameters used in the simulations. Most parameters were evaluated using an alloy physical property calculation software (Sente software JMatPro v11). The values in a previously published study [31] were used for the emissivity and the Stefan–Boltzmann constant, and the values for pure Ni [32] were used for the heat of vaporization and vaporization temperatures. The Fresnel coefficient, which determines the beam absorption efficiency, was used as a fitting parameter to reproduce the morphology of the experimentally observed melt region, and a Fresnel coefficient of 0.12 was used in this study.

Table 1. Parameters used in the CtFD simulations.

ParameterSymbolValueReference
Density at 298.15 Kρ8.24 g cm-3[]
Liquidus temperatureTL1628.15 K[]
Solidus temperatureTS1533.15 K[]
Viscosity at TLη6.8 g m-1 s-1[]
Specific heat at 298.15 KCP0.439 J g-1 K-1[]
Thermal conductivity at 298.15 Kλ10.3 W m-1 K-1[]
Surface tension at TLγL1.85 J m-2[]
Temperature coefficient of surface tensiondγL/dT–2.5 × 10−4 J m-2 K-1[]
EmissivityΕ0.27[31]
Stefan–Boltzmann constantσ5.67 × 10-8 W m-2 K-4[31]
Heat of fusionΔHSL2.76 × 102 J g-1[32]
Heat of vaporizationΔHLV4.29 × 10J g-1[32]
Vaporization temperatureTV3110 K[32]

Calculated using JMatPro v11.

The dimensions of the computational domain of the numerical model were 4.0 mm in the beam-scanning direction, 0.4 mm in width, and 0.3 mm in height. A uniform mesh size of 10 μm was applied throughout the computational domain. The boundary condition of continuity was applied to all boundaries except for the top surface. The temperature was initially set to 300 K. P and V were set to their experimental values, i.e., 300 W and 600 mm s-1, respectively. Solidification conditions based on the temperature gradient, G, the solidification rate, R, and the cooling rate were evaluated, and the obtained temperature distribution was used in the MPF simulations.

2.3. MPF simulation

Two-dimensional MPF simulations weakly coupled with the CtFD simulation were performed using the Microstructure Evolution Simulation Software (MICRESS) [33][34][35][36][37] with the TQ-Interface for Thermo-Calc [38]. A simplified HX alloy composition of Ni-21.4Cr-17.6Fe-0.46Mn-8.80Mo-0.39Si-0.50W-1.10Co-0.08 C (mass %) was used in this study. The Gibbs free energy and diffusion coefficient of the system were calculated using the TCNI9 thermodynamic database [39] and the MOBNi5 mobility database [40]. Τhe equilibrium phase diagram calculated using Thermo-Calc indicates that the face-centered cubic (FCC) and σ phases appear as the equilibrium solid phases [19]. However, according to the time-temperature-transformation (TTT) diagram [41], the phases are formed after the sample is maintained for tens of hours in a temperature range of 1073 to 1173 K. Therefore, only the liquid and FCC phases were assumed to appear in the MPF simulations. The simulation domain was 5 × 100 μm, and the grid size Δx and interface width were set to 0.025 and 0.1 µm, respectively. The interfacial mobility between the solid and liquid phases was set to 1.0 × 10-8 m4 J-1 s-1. Initially, one crystalline nucleus with a [100] crystal orientation was placed at the left bottom of the simulation domain, with the liquid phase occupying the remainder of the domain. The model was solidified under the temperature field distribution obtained by the CtFD simulation. The concentration distribution and crystal orientation of the solidified model were examined. The primary dendrite arm space (PDAS) was compared to the experimental PDAS measured by the cross-sectional SEM observation.

In an actual LPBF process, solidified layers are remelted and resolidified during the stacking of the one layer above, thereby greatly affecting solute element distributions in those regions. Therefore, remelting and resolidification simulations were performed to examine the effect of remelting on solute segregation. The solidified model was remelted and resolidified by applying a time-dependent temperature field shifted by 60 μm in the height direction, assuming reheating during the stacking of the upper layer (i.e., the upper 40 μm region of the simulation box was remelted and resolidified). The changes in the composition distribution and formed microstructure were investigated.

3. Results

3.1. Experimental observation of melt pool

Fig. 1 shows a cross-sectional optical microscopy image and corresponding inverse pole figure (IPF) orientation maps obtained from the laser-melted region of HX. The dashed line indicates the fusion line. A deep melted region was formed by keyhole-mode melting due to the vaporization of the metal and resultant recoil pressure. Epitaxial growth from the unmelted region was observed. Columnar crystal grains with an average diameter of 5.46 ± 0.32 μm and an aspect ratio of 3.61 ± 0.13 appeared at the melt regions (Figs. 1b–1d). In addition, crystal grains growing in the z direction could be observed in the lower center.

Fig. 1

Fig. 2a shows a cross-sectional backscattering electron image (BEI) obtained from the laser-melted region indicated by the black square in Fig. 1a. The bright particles with a diameter of approximately 2 μm observed outside the melt pool. It is well known that M6C, M23C6, σ, and μ precipitate phases are formed in Hastelloy-X [41]. These precipitates mainly consisted of Mo, Cr, Fe, and Ni; The μ and M6C phases are rich in Mo, while the σ and M23C6 phases are rich in Cr. The SEM energy dispersive X-ray spectroscopy analysis suggested that the bright particles are the stable precipitates as shown in Fig. S2 and Table S1. Conversely, there are no carbides in the melt pool. This suggests that the cooling rate is extremely high during LPBF, which prevents the formation of a stable carbide during solidification. Figs. 2b–2f show magnified BEI images at different height positions indicated in Fig. 2a. Bright regions are observed between the cells, which become fragmentary at the center of the melt pool, as indicated by the yellow arrow heads in Figs. 2e and 2f.

Fig. 2

3.2. CtFD simulation

Figs. 3a–3c show snapshots of the CtFD simulation of HX at 2.72 ms, with the temperature indicated in color. A melt pool with an elongated teardrop shape formed and keyhole-mode melting was observed at the front of the melt region. The cooling rate, temperature gradient (G), and solidification rate (R) were evaluated from the temporal change in the temperature distribution of the CtFD simulation results. The z-position of the solid/liquid interface during the melting and solidification processes is shown in Fig. 3d. The interface goes down rapidly during melting and then rises during solidification. The MPF simulation of the microstructure formation during solidification was performed using the temperature distribution. Moreover, the microstructure formation process during the fabrication of the upper layer was investigated by remelting and resolidifying the solidified layer using the same temperature distribution with a 60 μm upward shift, corresponding to the layer thickness commonly used in the LPBF of Ni-based superalloys.

Fig. 3

Figs. 4a–4c show the changes in the cooling rate, temperature gradient, and solidification rate in the center line of the melt pool parallel to the z direction. To output the solidification conditions at the solid/liquid interface in the melt pool, only the data of the mesh where the solid phase ratio was close to 0.5 were plotted. Solidification occurred where the cooling rate was in the range of 2.1 × 105–1.6 × 10K s-1G was in the range of 3.6 × 105–1.9 × 10K m-1, and R was in the range of 8.2 × 10−2–6.3 × 10−1 m s-1. The cooling rate was the highest near the fusion line and decreased as the interface approached the center of the melt region (Fig. 4a). G also exhibited the highest value in the regions near the fusion line and decreased throughout the solid/liquid interface toward the center of the melt pool (Fig. 4b). R had the lowest value near the fusion line and increased as the interface approached the center of the melt region (Fig. 4c).

Fig. 4

3.3. MPF simulations coupled with CtFD simulation

MPF simulations of solidification, remelting, and resolidification were performed using the temperature-time distribution obtained by the CtFD simulation. Fig. 5 shows the MPF solidified models colored by phase and Mo concentration. All the computational domains show the FCC phase after the solidification (Fig. 5a). Dendrites grew parallel to the heat flow direction, and solute segregations were observed in the interdendritic regions. At the bottom of the melt pool (Fig. 5d), planar interface growth occurred before the formation of primary dendrites. The bottom of the melt pool is the turning point of the solid/liquid interface from the downward motion in melting to the upward motion in solidification. Thus, the solidification rate at the boundary is zero, and is extremely low immediately above the molt-pool boundary. Here, the lower limit of the solidification rate (R) for dendritic growth can be represented by the constitutional supercooling criterion [29]Vcs = (G × DL) / ΔT, and planar interface growth occurs at R < VcsDL and ΔT denote the diffusion coefficient in the liquid and the equilibrium freezing range, respectively. The results suggest that planar interface growth occurs at the bottom of the melt pool, resulting in a dark region with a different solute element distribution. Some of the primary dendrites were diminished by competition with other dendrites. In addition, secondary dendrite arms could be seen in the upper regions (Fig. 5c), where solidification occurred at a lower cooling rate. The fragmentation of the solute segregation near the secondary dendrite arms is similar to that observed in the experimental melt pool shown in Figs. 2e and 2f, and the secondary dendrite arms are suggested to have appeared at the center of the melt region. Fig. 6 shows the PDASs measured from the MPF simulation models, compared to the experimental PDASs measured by the cross-sectional SEM observation of the laser-melted regions (Fig. 2). The PDAS obtained by the MPF simulation become larger as the solidification progress. Ghosh et al. [21] evident by the phase-field method that the PDAS decreases as the cooling rate increases under the rapid cooling conditions obtained by the finite element analysis. In this study, the cooling rate was decreased as the interface approached the center of the melt region (Fig. 4a), and the trends in PDAS changes with respect to cooling rate is same as the reported trend [21]. The simulated trends of the PDAS with the position in the melt pool agreed well with the experimental trends. However, all PDASs in the simulation were larger than those observed in the experiment at the same positions. Ode et al. [42] reported that PDAS differences between 2D and 3D MPF simulations can be represented by PDAS2D = 1.12 × PDAS3D owing to differences in the effects of the interfacial energy and diffusivity. We also performed 2D and 3D MPF simulations under the solidification conditions of G = 1.94 × 10K m-1 and R = 0.82 m s-1 (Fig. S1), and found that the PDAS from the 2D MPF simulation was 1.26 times larger than that from the 3D simulation. Therefore, the cell structure obtained by the CtFD simulation coupled with the 2D MPF simulation agreed well with the experimental results over the entire melt pool region considering the dimensional effects.

Fig. 5
Fig. 6

Fig. 7b1 and 7c1 show the concentration profiles of the solidified model along the growth direction indicated by dashed lines in Fig. 7a. The differences in concentrations from the alloy composition are also shown in Fig. 7b2 and 7c2. Cr, Mo, C, Mn, and W were segregated to the interdendritic regions, while Si, Fe, and Co were depressed. The solute segregation behavior agrees with the experimentally observation [43] and the prediction by the Scheil-Gulliver simulation [19]. Segregation occurred to the highest degree in Mo, while the ratio of segregation to the alloy composition was remarkable in C. The concentration fluctuations correlated with the position in the melt pool and decreased at the center of the melt pool, which was suggested to correspond to the lower cooling rate in this region. Conversely, droplets that appeared between secondary dendrite arms in the upper regions of the simulation domain exhibited a locally high segregation of solute elements, with the same amount of segregation as that at the bottom of the melt pool.

Fig. 7

3.4. Remelting and resolidification simulation

The solidified model was subjected to remelting and resolidification conditions by shifting the temperature profile upward by 60 µm to reveal the effect of reheating on the solute segregation behavior. Figs. 8a and 8b shows the simulation domains of the HX model after resolidification, colored by phase and Mo concentration. The magnified MPF models during the resolidification of the regions indicated by rectangles in Figs. 8a and 8b are also shown as Figs. 8c and 8d. Dendrites grew from the bottom of the remelted region, with the segregation of solute elements occurring in the interdendritic regions. The entire domain become the FCC phase after the resolidification, as shown in Fig. 8a. The bottom of the remelted regions exhibited a different microstructure, and Mo was depressed at the remelted regions, rather than the interdendritic regions. The different solute segregation behavior [44] and the microstructure formation [45] at the melt pool boundary is also observed in LPBF manufactured 316 L stainless steel. We found that this microstructure was formed by further remelting during the resolidification process, which is shown in Fig. 9. Here, the solidified HX model was heated, and the interdendritic regions were preferentially melted while concentration fluctuations were maintained (Fig. 9a1 and 9a2). Subsequently, planer interface growth occurs near the melt pool boundary where the solidification rate is almost zero, and the dendrites outside of the boundary are grown epitaxially (Fig. 9b1 and 9b2). However, these remelted again because of the temperature rise (Fig. 9c1 and 9c2, and the temperature-time profile shown in Fig. 9e). The remelted regions then cooled and solidified with the abnormal solute segregations (Fig. 9d1 and 9d2). Then, dendrite grows from amplified fluctuations under the solidification rate larger than the criterion of constitutional supercooling (Fig. 9d1, 9d2, and Fig. 8d). It has been reported [46][47] that temperature rising owning to latent heat affects microstructure formation: phase-field simulations of a Ni–Al binary alloy suggest that the release of latent heat during solidification increases the average temperature of the system [46] and strongly influences the solidification conditions [47]. In this study, the release of latent heat during solidification is considered in CtFD simulations for calculating the temperature distribution, and the temperature increase is suggested to have also occurred due to the release of latent heat.

Fig. 8
Fig. 9

Fig. 10b1 and 10c1 show the solute element concentration line profiles of the resolidified model along the growth direction indicated by dashed lines in Fig. 10a. Fig. 10b2 and 10c2 show the corresponding differences in concentration from the alloy composition. The segregation behavior of solute elements at the interdendritic regions (Fig. 10b1 and 10b2) was the same as that in the solidified model (Figs. 7b1 and 7b2). Here, Cr, Mo, C, Mn, and W were segregated to the interdendritic regions, while Si, Fe, and Co were depressed. However, the concentration fluctuations at the interdendritic regions were larger than those in the solidified model. Moreover, the segregation of the outside of the melt pool, i.e., the heat-affected zone, was remarkable throughout remelting and resolidification. Different segregation behaviors were observed in the re-remelted region: Mo, Si, Mn, and W were segregated, while Ni, Fe, and Co were depressed. These solute segregations caused by remelting are expected to heavily influence the crack behavior.

Fig. 10

4. Discussion

4.1. Effect of segregation of solute elements on liquation cracking susceptibility

Strong solute segregation was observed between the interdendritic regions of the solidified alloy (Fig. 7). In addition, the solute segregation behavior was significantly affected by remelting and resolidification and varied across the alloy. Solute segregation can be categorized by the regions shown in Fig. 11a1–11a4, namely the cell boundary (Fig. 11a1), interior of the melt-pool boundary (Fig. 11a2), re-remelted regions (Fig. 11a3), and heat-affected regions (Fig. 11a4). The concentration profiles of these regions are shown in Fig. 11b1–11b4. Solute segregation was the highest in the cell boundary region. The solute segregation in the heat-affected region was almost the same as that in the cell boundary region, but seemed to have been attenuated by reheating during remelting and resolidification. The interior of the melt-pool boundary region also had the same tendency for solute segregation. However, the amount of Cr segregation was smaller than that of Mo. A decrease in the Cr concentration was also mitigated, and the concentration remained the same as that in the alloy composition. Fig. 11c1–11c4 show the chemical potentials of the solute elements for the FCC phase at 1073 K calculated using the compositions of those interfacial regions. All the interfacial regions showed non-constant chemical potentials for each element along the perpendicular direction, but the fluctuations of the chemical potentials differed by the type of interfaces. In particular, the fluctuation of the chemical potential of C at the cell boundary region was the largest, suggesting it can be relaxed easily by heat treatment. On the other hand, the fluctuations of the other elements in all the regions were small. The solute segregations are most likely to remain after the heat treatment and are supposed to affect the cracking susceptibilities.

Fig. 11

The solidus temperatures TS, the difference between the liquidus and solidus temperatures (i.e., the brittle temperature range (BTR)), and the fractions of the equilibrium precipitate phases at 1073 K of the interfacial regions were calculated as the liquation, solidification, and ductility dip cracking susceptibilities, respectively. At the cell boundary (Fig. 12a1), interior of the melt-pool boundary (Fig. 12a1), and heat-affected regions (Fig. 12a1), the internal and interfacial regions exhibited higher and lower TS compared to that of the alloy composition, respectively. The lowest Ts was obtained with the composition at the cell boundary region, which is the largest solute-segregated region. It has been suggested that strong segregations of solute elements in LPBF lead to liquation cracks [16]. This study also supports this suggestion, and liquation cracks are more likely to occur at the interfacial regions indicated by predicting the solute segregation behavior using the MPF model. Additionally, the BTRs of the cell boundary, interior of the melt-pool boundary, and heat-affected regions were wider at the interdendritic regions, and solidification cracks were also likely to occur in these regions. Moreover, within the solute segregation regions, the fraction of the precipitate phases in these interfacial regions was larger than that calculated using the alloy composition (Fig. 12c1, 12c2, and 12c4). This indicates that ductility dip cracking is also likely to occur at the cell boundary, interior of the melt-pool boundary, and in heat-affected regions. Contrarily, we found that the re-remelted region exhibited a higher TS and smaller BTR even in the interfacial region (Fig. 12a3 and 12b3), where the solute segregation behavior was different from that of the other regions. In addition, the re-remelting region exhibited less precipitation compared with the other segregated regions (Fig. 12c3). The re-remelting caused by the latent heat can attenuate solute segregation, prevent Ts from decreasing, decrease the BTR, and decrease the amount of precipitate phases. Alloys with a large amount of latent heat are expected to increase the re-remelting region, thereby decreasing the susceptibility to liquation and ductility dip cracks due to solute element segregation. This can be a guide for designing alloys for the LPBF process. As mentioned in Section 3.4, the microstructure [45] and the solute segregation behavior [44] at the melt pool boundary of LPBF-manufactured 316 L stainless steel are observed, and they are different from that of the interdendritic regions. Experimental observations of the solute segregation behavior in the LPBF-fabricated Ni-based alloys are currently underway.

Fig. 12

4.2. Applicability of the conventional MPF simulation to microstructure formation under LPBF

As the solidification growth rate increases, segregation coefficients approach 1, and the fluctuation of the solid/liquid interface is suppressed by the interfacial tension. The interface growth occurs in a flat fashion instead of having a cellular morphology at a velocity above the absolute stability limit, Ras, predicted by the Mullins-Sekerka theory [29]Ras = (ΔT0 DL) / (k Γ) where ΔT0DLk, and Γ are the difference between the liquidus and solidus temperatures, equilibrium segregation coefficient, the diffusivity of liquid, and the Gibbs-Thomson coefficient, respectively.

The Ras of HX was calculated using the equation and the thermodynamic parameters obtained by the TCNI9 thermodynamic database [39]. The calculated Ras of HX was 3.9 m s-1 and is ten times larger than that of the Ni–Nb alloy (approximately 0.4 m s-1[20]. The HX alloy was solidified under R values in the range of 8.2 × 10−2–6.3 × 10−1 m s-1. The theoretically calculated criterion is larger than the evaluated R, and is in agreement with the experiment in which dendritic growth is observed in the melt pool (Fig. 5). In contrast, Karayagiz et al. [20] reported that the R of the Ni–Nb binary alloy under LPBF was as high as approximately 2 m s-1, and planar interface growth was observed to be predominant under the high-growth-rate conditions. These experimentally observed microstructures agree well with the prediction by the Mullins-Sekerka theory about the relationship between the morphology and solidification rates.

In this study, the solidification microstructure formed by the laser-beam irradiation of an HX multicomponent Ni-based superalloy was reproduced by a conventional MPF simulation, in which the system was assumed to be in a quasi-equilibrium condition. Boussinot et al. [24] also suggested that the conventional phase-field model can be applied to simulate the microstructure of an IN718 multicomponent Ni-based superalloy in LPBF. In contrast, Kagayaski et al. [20] suggested that the conventional MPF simulation cannot be applied to the solidification of the Ni-Nb binary alloy system and that the finite interface dissipation model proposed by Steinbach et al. [48][49] is necessary to simulate the high solidification rates observed in LPBF. The difference in the applicability of the conventional MPF method to HX and Ni–Nb binary alloys is presumed to arise from the differences in the non-equilibrium degree of these systems under the high solidification rates of LPBF. The results suggest that Ras can be used as a simple index to apply the conventional MPF model for solidification in LPBF. Solidification becomes a non-equilibrium process as the solidification rate approaches the limit of absolute stability, Ras. In this study, the solidification of the HX multicomponent system occurred under a relatively low solidification rate compared to Ras, and the microstructure of the conventional MPF model was successfully reproduced in the physical experiment. However, note that the limit of absolute stability predicted by the Mullins-Sekerka theory was originally proposed for solidification in a binary alloy system, and further investigation is required to consider its applicability to multicomponent alloy systems. Moreover, the fast solidification, such as in the LPBF process, causes segregation coefficient approaching a value of 1 [20][21][25] corresponds to a diffusion length that is on the order of the atomic interface thickness. When the segregation coefficient approaches 1, solute undercooling disappears; hence, there is no driving force to amplify fluctuations regardless of whether interfacial tension is present. This phenomenon should be further investigated in future studies.

5. Conclusions

We simulated solute segregation in a multicomponent HX alloy under the LPBF process by an MPF simulation using the temperature distributions obtained by a CtFD simulation. We set the parameters of the CtFD simulation to match the melt pool shape formed in the laser-irradiation experiment and found that solidification occurred under high cooling rates of up to 1.6 × 10K s-1.

MPF simulations using the temperature distributions from CtFD simulation could reproduce the experimentally observed PDAS and revealed that significant solute segregation occurred at the interdendritic regions. Equilibrium thermodynamic calculations using the alloy compositions of the segregated regions when considering crack sensitivities suggested a decrease in the solidus temperature and an increase in the amount of carbide precipitation, thereby increasing the susceptibility to liquation and ductility dip cracks in these regions. Notably, these changes were suppressed at the melt-pool boundary region, where re-remelting occurred during the stacking of the layer above. This effect can be used to achieve a novel in-process segregation attenuation.

Our study revealed that a conventional MPF simulation weakly coupled with a CtFD simulation can be used to study the solidification of multicomponent alloys in LPBF, contrary to the cases of binary alloys investigated in previous studies. We discussed the applicability of the conventional MPF model to the LPBF process in terms of the limit of absolute stability, Ras, and suggested that alloys with a high limit velocity, i.e., multicomponent alloys, can be simulated using the conventional MPF model even under the high solidification velocity conditions of LPBF.

CRediT authorship contribution statement

Masayuki Okugawa: Writing – review & editing, Writing – original draft, Visualization, Validation, Software, Methodology, Investigation, Formal analysis, Data curation, Conceptualization. Takayoshi Nakano: Writing – review & editing, Validation, Supervision, Funding acquisition. Yuichiro Koizumi: Writing – review & editing, Visualization, Validation, Supervision, Project administration, Methodology, Investigation, Funding acquisition, Formal analysis, Data curation, Conceptualization. Sukeharu Nomoto: Writing – review & editing, Validation, Investigation. Makoto Watanabe: Writing – review & editing, Validation, Supervision, Funding acquisition. Katsuhiko Sawaizumi: Validation, Software, Investigation, Formal analysis, Data curation. Kenji Saito: Visualization, Validation, Software, Methodology, Investigation, Formal analysis, Data curation. Haruki Yoshima: Visualization, Validation, Software, Investigation, Formal analysis, Data curation.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper

Acknowledgments

This work was partly supported by the Cabinet Office, Government of Japan, Cross-ministerial Strategic Innovation Promotion Program (SIP), “Materials Integration for Revolutionary Design System of Structural Materials,” (funding agency: The Japan Science and Technology Agency), by JSPS KAKENHI Grant Numbers 21H05018 and 21H05193, and by CREST Nanomechanics: Elucidation of macroscale mechanical properties based on understanding nanoscale dynamics for innovative mechanical materials (Grant Number: JPMJCR2194) from the Japan Science and Technology Agency (JST). The authors would like to thank Mr. H. Kawabata and Mr. K. Kimura for their technical support with the sample preparations and laser beam irradiation experiments.

Appendix A. Supplementary material

Download : Download Word document (654KB)

Supplementary material.

Data availability

Data will be made available on request.

References

Schematic diagram of HP-LPBF melting process.

Modeling and numerical studies of high-precision laser powder bed fusion

Yi Wei ;Genyu Chen;Nengru Tao;Wei Zhou
https://doi.org/10.1063/5.0191504

In order to comprehensively reveal the evolutionary dynamics of the molten pool and the state of motion of the fluid during the high-precision laser powder bed fusion (HP-LPBF) process, this study aims to deeply investigate the specific manifestations of the multiphase flow, solidification phenomena, and heat transfer during the process by means of numerical simulation methods. Numerical simulation models of SS316L single-layer HP-LPBF formation with single and double tracks were constructed using the discrete element method and the computational fluid dynamics method. The effects of various factors such as Marangoni convection, surface tension, vapor recoil, gravity, thermal convection, thermal radiation, and evaporative heat dissipation on the heat and mass transfer in the molten pool have been paid attention to during the model construction process. The results show that the molten pool exhibits a “comet” shape, in which the temperature gradient at the front end of the pool is significantly larger than that at the tail end, with the highest temperature gradient up to 1.69 × 108 K/s. It is also found that the depth of the second track is larger than that of the first one, and the process parameter window has been determined preliminarily. In addition, the application of HP-LPBF technology helps to reduce the surface roughness and minimize the forming size.

Topics

Heat transferNonequilibrium thermodynamicsSolidification processComputer simulationDiscrete element methodLasersMass transferFluid mechanicsComputational fluid dynamicsMultiphase flows

I. INTRODUCTION

Laser powder bed fusion (LPBF) has become a research hotspot in the field of additive manufacturing of metals due to its advantages of high-dimensional accuracy, good surface quality, high density, and high material utilization.1,2 With the rapid development of electronics, medical, automotive, biotechnology, energy, communication, and optics, the demand for microfabrication technology is increasing day by day.3 High-precision laser powder bed fusion (HP-LPBF) is one of the key manufacturing technologies for tiny parts in the fields of electronics, medical, automotive, biotechnology, energy, communication, and optics because of its process characteristics such as small focal spot diameter, small powder particle size, and thin powder layup layer thickness.4–13 Compared with LPBF, HP-LPBF has the significant advantages of smaller focal spot diameter, smaller powder particle size, and thinner layer thickness. These advantages make HP-LPBF perform better in producing micro-fine parts, high surface quality, and parts with excellent mechanical properties.

HP-LPBF is in the exploratory stage, and researchers have already done some exploratory studies on the focal spot diameter, the amount of defocusing, and the powder particle size. In order to explore the influence of changing the laser focal spot diameter on the LPBF process characteristics of the law, Wildman et al.14 studied five groups of different focal spot diameter LPBF forming 316L stainless steel (SS316L) processing effect, the smallest focal spot diameter of 26 μm, and the results confirm that changing the focal spot diameter can be achieved to achieve the energy control, so as to control the quality of forming. Subsequently, Mclouth et al.15 proposed the laser out-of-focus amount (focal spot diameter) parameter, which characterizes the distance between the forming plane and the laser focal plane. The laser energy density was controlled by varying the defocusing amount while keeping the laser parameters constant. Sample preparation at different focal positions was investigated, and their microstructures were characterized. The results show that the samples at the focal plane have finer microstructure than those away from the focal plane, which is the effect of higher power density and smaller focal spot diameter. In order to explore the influence of changing the powder particle size on the characteristics of the LPBF process, Qian et al.16 carried out single-track scanning simulations on powder beds with average powder particle sizes of 70 and 40 μm, respectively, and the results showed that the melt tracks sizes were close to each other under the same process parameters for the two particle-size distributions and that the molten pool of powder beds with small particles was more elongated and the edges of the melt tracks were relatively flat. In order to explore the superiority of HP-LPBF technology, Xu et al.17 conducted a comparative analysis of HP-LPBF and conventional LPBF of SS316L. The results showed that the average surface roughness of the top surface after forming by HP-LPBF could reach 3.40 μm. Once again, it was verified that HP-LPBF had higher forming quality than conventional LPBF. On this basis, Wei et al.6 comparatively analyzed the effects of different laser focal spot diameters on different powder particle sizes formed by LPBF. The results showed that the smaller the laser focal spot diameter, the fewer the defects on the top and side surfaces. The above research results confirm that reducing the laser focal spot diameter can obtain higher energy density and thus better forming quality.

LPBF involves a variety of complex systems and mechanisms, and the final quality of the part is influenced by a large number of process parameters.18–24 Some research results have shown that there are more than 50 factors affecting the quality of the specimen. The influencing factors are mainly categorized into three main groups: (1) laser parameters, (2) powder parameters, and (3) equipment parameters, which interact with each other to determine the final specimen quality. With the continuous development of technologies such as computational materials science and computational fluid dynamics (CFD), the method of studying the influence of different factors on the forming quality of LPBF forming process has been shifted from time-consuming and laborious experimental characterization to the use of numerical simulation methods. As a result, more and more researchers are adopting this approach for their studies. Currently, numerical simulation studies on LPBF are mainly focused on the exploration of molten pool, temperature distribution, and residual stresses.

  1. Finite element simulation based on continuum mechanics and free surface fluid flow modeling based on fluid dynamics are two common approaches to study the behavior of LPBF molten pool.25–28 Finite element simulation focuses on the temperature and thermal stress fields, treats the powder bed as a continuum, and determines the molten pool size by plotting the elemental temperature above the melting point. In contrast, fluid dynamics modeling can simulate the 2D or 3D morphology of the metal powder pile and obtain the powder size and distribution by certain algorithms.29 The flow in the molten pool is mainly affected by recoil pressure and the Marangoni effect. By simulating the molten pool formation, it is possible to predict defects, molten pool shape, and flow characteristics, as well as the effect of process parameters on the molten pool geometry.30–34 In addition, other researchers have been conducted to optimize the laser processing parameters through different simulation methods and experimental data.35–46 Crystal growth during solidification is studied to further understand the effect of laser parameters on dendritic morphology and solute segregation.47–54 A multi-scale system has been developed to describe the fused deposition process during 3D printing, which is combined with the conductive heat transfer model and the dendritic solidification model.55,56
  2. Relevant scholars have adopted various different methods for simulation, such as sequential coupling theory,57 Lagrangian and Eulerian thermal models,58 birth–death element method,25 and finite element method,59 in order to reveal the physical phenomena of the laser melting process and optimize the process parameters. Luo et al.60 compared the LPBF temperature field and molten pool under double ellipsoidal and Gaussian heat sources by ANSYS APDL and found that the diffusion of the laser energy in the powder significantly affects the molten pool size and the temperature field.
  3. The thermal stresses obtained from the simulation correlate with the actual cracks,61 and local preheating can effectively reduce the residual stresses.62 A three-dimensional thermodynamic finite element model investigated the temperature and stress variations during laser-assisted fabrication and found that powder-to-solid conversion increases the temperature gradient, stresses, and warpage.63 Other scholars have predicted residual stresses and part deflection for LPBF specimens and investigated the effects of deposition pattern, heat, laser power, and scanning strategy on residual stresses, noting that high-temperature gradients lead to higher residual stresses.64–67 

In short, the process of LPBF forming SS316L is extremely complex and usually involves drastic multi-scale physicochemical changes that will only take place on a very small scale. Existing literature employs DEM-based mesoscopic-scale numerical simulations to investigate the effects of process parameters on the molten pool dynamics of LPBF-formed SS316L. However, a few studies have been reported on the key mechanisms of heating and solidification, spatter, and convective behavior of the molten pool of HP-LPBF-formed SS316L with small laser focal spot diameters. In this paper, the geometrical properties of coarse and fine powder particles under three-dimensional conditions were first calculated using DEM. Then, numerical simulation models for single-track and double-track cases in the single-layer HP-LPBF forming SS316L process were developed at mesoscopic scale using the CFD method. The flow genesis of the melt in the single-track and double-track molten pools is discussed, and their 3D morphology and dimensional characteristics are discussed. In addition, the effects of laser process parameters, powder particle size, and laser focal spot diameter on the temperature field, characterization information, and defects in the molten pool are discussed.

II. MODELING

A. 3D powder bed modeling

HP-LPBF is an advanced processing technique for preparing target parts layer by layer stacking, the process of which involves repetitive spreading and melting of powders. In this process, both the powder spreading and the morphology of the powder bed are closely related to the results of the subsequent melting process, while the melted surface also affects the uniform distribution of the next layer of powder. For this reason, this chapter focuses on the modeling of the physical action during the powder spreading process and the theory of DEM to establish the numerical model of the powder bed, so as to lay a solid foundation for the accuracy of volume of fluid (VOF) and CFD.

1. DEM

DEM is a numerical technique for calculating the interaction of a large number of particles, which calculates the forces and motions of the spheres by considering each powder sphere as an independent unit. The motion of the powder particles follows the laws of classical Newtonian mechanics, including translational and rotational,38,68–70 which are expressed as follows:����¨=���+∑��ij,

(1)����¨=∑�(�ij×�ij),

(2)

where �� is the mass of unit particle i in kg, ��¨ is the advective acceleration in m/s2, And g is the gravitational acceleration in m/s2. �ij is the force in contact with the neighboring particle � in N. �� is the rotational inertia of the unit particle � in kg · m2. ��¨ is the unit particle � angular acceleration in rad/s2. �ij is the vector pointing from unit particle � to the contact point of neighboring particle �⁠.

Equations (1) and (2) can be used to calculate the velocity and angular velocity variations of powder particles to determine their positions and velocities. A three-dimensional powder bed model of SS316L was developed using DEM. The powder particles are assumed to be perfect spheres, and the substrate and walls are assumed to be rigid. To describe the contact between the powder particles and between the particles and the substrate, a non-slip Hertz–Mindlin nonlinear spring-damping model71 was used with the following expression:�hz=��������+��[(�����ij−�eff����)−(�����+�eff����)],

(3)

where �hz is the force calculated using the Hertzian in M. �� and �� are the radius of unit particles � and � in m, respectively. �� is the overlap size of the two powder particles in m. ��⁠, �� are the elastic constants in the normal and tangential directions, respectively. �ij is the unit vector connecting the centerlines of the two powder particles. �eff is the effective mass of the two powder particles in kg. �� and �� are the viscoelastic damping constants in the normal and tangential directions, respectively. �� and �� are the components of the relative velocities of the two powder particles. ��� is the displacement vector between two spherical particles. The schematic diagram of overlapping powder particles is shown in Fig. 1.

FIG. 1.

VIEW LARGEDOWNLOAD SLIDE

Schematic diagram of overlapping powder particles.

Because the particle size of the powder used for HP-LPBF is much smaller than 100 μm, the effect of van der Waals forces must be considered. Therefore, the cohesive force �jkr of the Hertz–Mindlin model was used instead of van der Waals forces,72 with the following expression:�jkr=−4��0�*�1.5+4�*3�*�3,

(4)1�*=(1−��2)��+(1−��2)��,

(5)1�*=1��+1��,

(6)

where �* is the equivalent Young’s modulus in GPa; �* is the equivalent particle radius in m; �0 is the surface energy of the powder particles in J/m2; α is the contact radius in m; �� and �� are the Young’s modulus of the unit particles � and �⁠, respectively, in GPa; and �� and �� are the Poisson’s ratio of the unit particles � and �⁠, respectively.

2. Model building

Figure 2 shows a 3D powder bed model generated using DEM with a coarse powder geometry of 1000 × 400 × 30 μm3. The powder layer thickness is 30 μm, and the powder bed porosity is 40%. The average particle size of this spherical powder is 31.7 μm and is normally distributed in the range of 15–53 μm. The geometry of the fine powder was 1000 × 400 × 20 μm3, with a layer thickness of 20 μm, and the powder bed porosity of 40%. The average particle size of this spherical powder is 11.5 μm and is normally distributed in the range of 5–25 μm. After the 3D powder bed model is generated, it needs to be imported into the CFD simulation software for calculation, and the imported geometric model is shown in Fig. 3. This geometric model is mainly composed of three parts: protective gas, powder bed, and substrate. Under the premise of ensuring the accuracy of the calculation, the mesh size is set to 3 μm, and the total number of coarse powder meshes is 1 704 940. The total number of fine powder meshes is 3 982 250.

FIG. 2.

VIEW LARGEDOWNLOAD SLIDE

Three-dimensional powder bed model: (a) coarse powder, (b) fine powder.

FIG. 3.

VIEW LARGEDOWNLOAD SLIDE

Geometric modeling of the powder bed computational domain: (a) coarse powder, (b) fine powder.

B. Modeling of fluid mechanics simulation

In order to solve the flow, melting, and solidification problems involved in HP-LPBF molten pool, the study must follow the three governing equations of conservation of mass, conservation of energy, and conservation of momentum.73 The VOF method, which is the most widely used in fluid dynamics, is used to solve the molten pool dynamics model.

1. VOF

VOF is a method for tracking the free interface between the gas and liquid phases on the molten pool surface. The core idea of the method is to define a volume fraction function F within each grid, indicating the proportion of the grid space occupied by the material, 0 ≤ F ≤ 1 in Fig. 4. Specifically, when F = 0, the grid is empty and belongs to the gas-phase region; when F = 1, the grid is completely filled with material and belongs to the liquid-phase region; and when 0 < F < 1, the grid contains free surfaces and belongs to the mixed region. The direction normal to the free surface is the direction of the fastest change in the volume fraction F (the direction of the gradient of the volume fraction), and the direction of the gradient of the volume fraction can be calculated from the values of the volume fractions in the neighboring grids.74 The equations controlling the VOF are expressed as follows:𝛻����+�⋅(��→)=0,

(7)

where t is the time in s and �→ is the liquid velocity in m/s.

FIG. 4.

VIEW LARGEDOWNLOAD SLIDE

Schematic diagram of VOF.

The material parameters of the mixing zone are altered due to the inclusion of both the gas and liquid phases. Therefore, in order to represent the density of the mixing zone, the average density �¯ is used, which is expressed as follows:72�¯=(1−�1)�gas+�1�metal,

(8)

where �1 is the proportion of liquid phase, �gas is the density of protective gas in kg/m3, and �metal is the density of metal in kg/m3.

2. Control equations and boundary conditions

Figure 5 is a schematic diagram of the HP-LPBF melting process. First, the laser light strikes a localized area of the material and rapidly heats up the area. Next, the energy absorbed in the region is diffused through a variety of pathways (heat conduction, heat convection, and surface radiation), and this process triggers complex phase transition phenomena (melting, evaporation, and solidification). In metals undergoing melting, the driving forces include surface tension and the Marangoni effect, recoil due to evaporation, and buoyancy due to gravity and uneven density. The above physical phenomena interact with each other and do not occur independently.

FIG. 5.

VIEW LARGEDOWNLOAD SLIDE

Schematic diagram of HP-LPBF melting process.

  1. Laser heat sourceThe Gaussian surface heat source model is used as the laser heat source model with the following expression:�=2�0����2exp(−2�12��2),(9)where � is the heat flow density in W/m2, �0 is the absorption rate of SS316L, �� is the radius of the laser focal spot in m, and �1 is the radial distance from the center of the laser focal spot in m. The laser focal spot can be used for a wide range of applications.
  2. Energy absorptionThe formula for calculating the laser absorption �0 of SS316L is as follows:�0=0.365(�0[1+�0(�−20)]/�)0.5,(10)where �0 is the direct current resistivity of SS316L at 20 °C in Ω m, �0 is the resistance temperature coefficient in ppm/°C, � is the temperature in °C, and � is the laser wavelength in m.
  3. Heat transferThe basic principle of heat transfer is conservation of energy, which is expressed as follows:𝛻𝛻𝛻�(��)��+�·(��→�)=�·(�0����)+��,(11)where � is the density of liquid phase SS316L in kg/m3, �� is the specific heat capacity of SS316L in J/(kg K), 𝛻� is the gradient operator, t is the time in s, T is the temperature in K, 𝛻�� is the temperature gradient, �→ is the velocity vector, �0 is the coefficient of thermal conduction of SS316L in W/(m K), and  �� is the thermal energy dissipation term in the molten pool.
  4. Molten pool flowThe following three conditions need to be satisfied for the molten pool to flow:
    • Conservation of mass with the following expression:𝛻�·(��→)=0.(12)
    • Conservation of momentum (Navier–Stokes equation) with the following expression:𝛻𝛻𝛻𝛻���→��+�(�→·�)�→=�·[−pI+�(��→+(��→)�)]+�,(13)where � is the pressure in Pa exerted on the liquid phase SS316L microelement, � is the unit matrix, � is the fluid viscosity in N s/m2, and � is the volumetric force (gravity, atmospheric pressure, surface tension, vapor recoil, and the Marangoni effect).
    • Conservation of energy, see Eq. (11)
  5. Surface tension and the Marangoni effectThe effect of temperature on the surface tension coefficient is considered and set as a linear relationship with the following expression:�=�0−��dT(�−��),(14)where � is the surface tension of the molten pool at temperature T in N/m, �� is the melting temperature of SS316L in K, �0 is the surface tension of the molten pool at temperature �� in Pa, and σdσ/ dT is the surface tension temperature coefficient in N/(m K).In general, surface tension decreases with increasing temperature. A temperature gradient causes a gradient in surface tension that drives the liquid to flow, known as the Marangoni effect.
  6. Metal vapor recoilAt higher input energy densities, the maximum temperature of the molten pool surface reaches the evaporation temperature of the material, and a gasification recoil pressure occurs vertically downward toward the molten pool surface, which will be the dominant driving force for the molten pool flow.75 The expression is as follows:��=0.54�� exp ���−���0���,(15)where �� is the gasification recoil pressure in Pa, �� is the ambient pressure in kPa, �� is the latent heat of evaporation in J/kg, �0 is the gas constant in J/(mol K), T is the surface temperature of the molten pool in K, and Te is the evaporation temperature in K.
  7. Solid–liquid–gas phase transitionWhen the laser hits the powder layer, the powder goes through three stages: heating, melting, and solidification. During the solidification phase, mutual transformations between solid, liquid, and gaseous states occur. At this point, the latent heat of phase transition absorbed or released during the phase transition needs to be considered.68 The phase transition is represented based on the relationship between energy and temperature with the following expression:�=�����,(�<��),�(��)+�−����−����,(��<�<��)�(��)+(�−��)����,(��<�),,(16)where �� and �� are solid and liquid phase density, respectively, of SS316L in kg/m3. �� and �� unit volume of solid and liquid phase-specific heat capacity, respectively, of SS316L in J/(kg K). �� and ��⁠, respectively, are the solidification temperature and melting temperature of SS316L in K. �� is the latent heat of the phase transition of SS316L melting in J/kg.

3. Assumptions

The CFD model was computed using the commercial software package FLOW-3D.76 In order to simplify the calculation and solution process while ensuring the accuracy of the results, the model makes the following assumptions:

  1. It is assumed that the effects of thermal stress and material solid-phase thermal expansion on the calculation results are negligible.
  2. The molten pool flow is assumed to be a Newtonian incompressible laminar flow, while the effects of liquid thermal expansion and density on the results are neglected.
  3. It is assumed that the surface tension can be simplified to an equivalent pressure acting on the free surface of the molten pool, and the effect of chemical composition on the results is negligible.
  4. Neglecting the effect of the gas flow field on the molten pool.
  5. The mass loss due to evaporation of the liquid metal is not considered.
  6. The influence of the plasma effect of the molten metal on the calculation results is neglected.

It is worth noting that the formulation of assumptions requires a trade-off between accuracy and computational efficiency. In the above models, some physical phenomena that have a small effect or high difficulty on the calculation results are simplified or ignored. Such simplifications make numerical simulations more efficient and computationally tractable, while still yielding accurate results.

4. Initial conditions

The preheating temperature of the substrate was set to 393 K, at which time all materials were in the solid state and the flow rate was zero.

5. Material parameters

The material used is SS316L and the relevant parameters required for numerical simulations are shown in Table I.46,77,78

TABLE I.

SS316L-related parameters.

PropertySymbolValue
Density of solid metal (kg/m3�metal 7980 
Solid phase line temperature (K) �� 1658 
Liquid phase line temperature (K) �� 1723 
Vaporization temperature (K) �� 3090 
Latent heat of melting (⁠ J/kg⁠) �� 2.60×105 
Latent heat of evaporation (⁠ J/kg⁠) �� 7.45×106 
Surface tension of liquid phase (N /m⁠) � 1.60 
Liquid metal viscosity (kg/m s) �� 6×10−3 
Gaseous metal viscosity (kg/m s) �gas 1.85×10−5 
Temperature coefficient of surface tension (N/m K) ��/�T 0.80×10−3 
Molar mass (⁠ kg/mol⁠) 0.05 593 
Emissivity � 0.26 
Laser absorption �0 0.35 
Ambient pressure (kPa) �� 101 325 
Ambient temperature (K) �0 300 
Stefan–Boltzmann constant (W/m2 K4� 5.67×10−8 
Thermal conductivity of metals (⁠ W/m K⁠) � 24.55 
Density of protective gas (kg/m3�gas 1.25 
Coefficient of thermal expansion (/K) �� 16×10−6 
Generalized gas constant (⁠ J/mol K⁠) 8.314 

III. RESULTS AND DISCUSSION

With the objective of studying in depth the evolutionary patterns of single-track and double-track molten pool development, detailed observations were made for certain specific locations in the model, as shown in Fig. 6. In this figure, P1 and P2 represent the longitudinal tangents to the centers of the two melt tracks in the XZ plane, while L1 is the transverse profile in the YZ plane. The scanning direction is positive and negative along the X axis. Points A and B are the locations of the centers of the molten pool of the first and second melt tracks, respectively (x = 1.995 × 10−4, y = 5 × 10−7, and z = −4.85 × 10−5).

FIG. 6.

VIEW LARGEDOWNLOAD SLIDE

Schematic diagram of observation position.

A. Single-track simulation

A series of single-track molten pool simulation experiments were carried out in order to investigate the influence law of laser power as well as scanning speed on the HP-LPBF process. Figure 7 demonstrates the evolution of the 3D morphology and temperature field of the single-track molten pool in the time period of 50–500 μs under a laser power of 100 W and a scanning speed of 800 mm/s. The powder bed is in the natural cooling state. When t = 50 μs, the powder is heated by the laser heat and rapidly melts and settles to form the initial molten pool. This process is accompanied by partial melting of the substrate and solidification together with the melted powder. The molten pool rapidly expands with increasing width, depth, length, and temperature, as shown in Fig. 7(a). When t = 150 μs, the molten pool expands more obviously, and the temperature starts to transfer to the surrounding area, forming a heat-affected zone. At this point, the width of the molten pool tends to stabilize, and the temperature in the center of the molten pool has reached its peak and remains largely stable. However, the phenomenon of molten pool spatter was also observed in this process, as shown in Fig. 7(b). As time advances, when t = 300 μs, solidification begins to occur at the tail of the molten pool, and tiny ripples are produced on the solidified surface. This is due to the fact that the melt flows toward the region with large temperature gradient under the influence of Marangoni convection and solidifies together with the melt at the end of the bath. At this point, the temperature gradient at the front of the bath is significantly larger than at the end. While the width of the molten pool was gradually reduced, the shape of the molten pool was gradually changed to a “comet” shape. In addition, a slight depression was observed at the top of the bath because the peak temperature at the surface of the bath reached the evaporation temperature, which resulted in a recoil pressure perpendicular to the surface of the bath downward, creating a depressed region. As the laser focal spot moves and is paired with the Marangoni convection of the melt, these recessed areas will be filled in as shown in Fig. 7(c). It has been shown that the depressed regions are the result of the coupled effect of Marangoni convection, recoil pressure, and surface tension.79 By t = 500 μs, the width and height of the molten pool stabilize and show a “comet” shape in Fig. 7(d).

FIG. 7.

VIEW LARGEDOWNLOAD SLIDE

Single-track molten pool process: (a) t = 50  ��⁠, (b) t = 150  ��⁠, (c) t = 300  ��⁠, (d) t = 500  ��⁠.

Figure 8 depicts the velocity vector diagram of the P1 profile in a single-track molten pool, the length of the arrows represents the magnitude of the velocity, and the maximum velocity is about 2.36 m/s. When t = 50 μs, the molten pool takes shape, and the velocities at the two ends of the pool are the largest. The variation of the velocities at the front end is especially more significant in Fig. 8(a). As the time advances to t = 150 μs, the molten pool expands rapidly, in which the velocity at the tail increases and changes more significantly, while the velocity at the front is relatively small. At this stage, the melt moves backward from the center of the molten pool, which in turn expands the molten pool area. The melt at the back end of the molten pool center flows backward along the edge of the molten pool surface and then converges along the edge of the molten pool to the bottom center, rising to form a closed loop. Similarly, a similar closed loop is formed at the front end of the center of the bath, but with a shorter path. However, a large portion of the melt in the center of the closed loop formed at the front end of the bath is in a nearly stationary state. The main cause of this melt flow phenomenon is the effect of temperature gradient and surface tension (the Marangoni effect), as shown in Figs. 8(b) and 8(e). This dynamic behavior of the melt tends to form an “elliptical” pool. At t = 300 μs, the tendency of the above two melt flows to close the loop is more prominent and faster in Fig. 8(c). When t = 500 μs, the velocity vector of the molten pool shows a stable trend, and the closed loop of melt flow also remains stable. With the gradual laser focal spot movement, the melt is gradually solidified at its tail, and finally, a continuous and stable single track is formed in Fig. 8(d).

FIG. 8.

VIEW LARGEDOWNLOAD SLIDE

Vector plot of single-track molten pool velocity in XZ longitudinal section: (a) t = 50  ��⁠, (b) t = 150  ��⁠, (c) t = 300  ��⁠, (d) t = 500  ��⁠, (e) molten pool flow.

In order to explore in depth the transient evolution of the molten pool, the evolution of the single-track temperature field and the melt flow was monitored in the YZ cross section. Figure 9(a) shows the state of the powder bed at the initial moment. When t = 250 μs, the laser focal spot acts on the powder bed and the powder starts to melt and gradually collects in the molten pool. At this time, the substrate will also start to melt, and the melt flow mainly moves in the downward and outward directions and the velocity is maximum at the edges in Fig. 9(b). When t = 300 μs, the width and depth of the molten pool increase due to the recoil pressure. At this time, the melt flows more slowly at the center, but the direction of motion is still downward in Fig. 9(c). When t = 350 μs, the width and depth of the molten pool further increase, at which time the intensity of the melt flow reaches its peak and the direction of motion remains the same in Fig. 9(d). When t = 400 μs, the melt starts to move upward, and the surrounding powder or molten material gradually fills up, causing the surface of the molten pool to begin to flatten. At this time, the maximum velocity of the melt is at the center of the bath, while the velocity at the edge is close to zero, and the edge of the melt starts to solidify in Fig. 9(e). When t = 450 μs, the melt continues to move upward, forming a convex surface of the melt track. However, the melt movement slows down, as shown in Fig. 9(f). When t = 500 μs, the melt further moves upward and its speed gradually becomes smaller. At the same time, the melt solidifies further, as shown in Fig. 9(g). When t = 550 μs, the melt track is basically formed into a single track with a similar “mountain” shape. At this stage, the velocity is close to zero only at the center of the molten pool, and the flow behavior of the melt is poor in Fig. 9(h). At t = 600 μs, the melt stops moving and solidification is rapidly completed. Up to this point, a single track is formed in Fig. 9(i). During the laser action on the powder bed, the substrate melts and combines with the molten state powder. The powder-to-powder fusion is like the convergence of water droplets, which are rapidly fused by surface tension. However, the fusion between the molten state powder and the substrate occurs driven by surface tension, and the molten powder around the molten pool is pulled toward the substrate (a wetting effect occurs), which ultimately results in the formation of a monolithic whole.38,80,81

FIG. 9.

VIEW LARGEDOWNLOAD SLIDE

Evolution of single-track molten pool temperature and melt flow in the YZ cross section: (a) t = 0  ��⁠, (b) t = 250  ��⁠, (c) t = 300  ��⁠, (d) t = 350  ��⁠, (e) t = 400  ��⁠, (f) t = 450  ��⁠, (g) t = 500  ��⁠, (h) t = 550  ��⁠, (i) t = 600  ��⁠.

The wetting ability between the liquid metal and the solid substrate in the molten pool directly affects the degree of balling of the melt,82,83 and the wetting ability can be measured by the contact angle of a single track in Fig. 10. A smaller value of contact angle represents better wettability. The contact angle α can be calculated by�=�1−�22,

(17)

where �1 and �2 are the contact angles of the left and right regions, respectively.

FIG. 10.

VIEW LARGEDOWNLOAD SLIDE

Schematic of contact angle.

Relevant studies have confirmed that the wettability is better at a contact angle α around or below 40°.84 After measurement, a single-track contact angle α of about 33° was obtained under this process parameter, which further confirms the good wettability.

B. Double-track simulation

In order to deeply investigate the influence of hatch spacing on the characteristics of the HP-LPBF process, a series of double-track molten pool simulation experiments were systematically carried out. Figure 11 shows in detail the dynamic changes of the 3D morphology and temperature field of the double-track molten pool in the time period of 2050–2500 μs under the conditions of laser power of 100 W, scanning speed of 800 mm/s, and hatch spacing of 0.06 mm. By comparing the study with Fig. 7, it is observed that the basic characteristics of the 3D morphology and temperature field of the second track are similar to those of the first track. However, there are subtle differences between them. The first track exhibits a basically symmetric shape, but the second track morphology shows a slight deviation influenced by the difference in thermal diffusion rate between the solidified metal and the powder. Otherwise, the other characteristic information is almost the same as that of the first track. Figure 12 shows the velocity vector plot of the P2 profile in the double-track molten pool, with a maximum velocity of about 2.63 m/s. The melt dynamics at both ends of the pool are more stable at t = 2050 μs, where the maximum rate of the second track is only 1/3 of that of the first one. Other than that, the rest of the information is almost no significant difference from the characteristic information of the first track. Figure 13 demonstrates a detailed observation of the double-track temperature field and melts flow in the YZ cross section, and a comparative study with Fig. 9 reveals that the width of the second track is slightly wider. In addition, after the melt direction shifts from bottom to top, the first track undergoes four time periods (50 μs) to reach full solidification, while the second track takes five time periods. This is due to the presence of significant heat buildup in the powder bed after the forming of the first track, resulting in a longer dynamic time of the melt and an increased molten pool lifetime. In conclusion, the level of specimen forming can be significantly optimized by adjusting the laser power and hatch spacing.

FIG. 11.

VIEW LARGEDOWNLOAD SLIDE

Double-track molten pool process: (a) t = 2050  ��⁠, (b) t = 2150  ��⁠, (c) t = 2300  ��⁠, (d) t = 2500  ��⁠.

FIG. 12.

VIEW LARGEDOWNLOAD SLIDE

Vector plot of double-track molten pool velocity in XZ longitudinal section: (a) t = 2050  ��⁠, (b) t = 2150  ��⁠, (c) t = 2300  ��⁠, (d) t = 2500  ��⁠.

FIG. 13.

VIEW LARGEDOWNLOAD SLIDE

Evolution of double-track molten pool temperature and melt flow in the YZ cross section: (a) t = 2250  ��⁠, (b) t = 2300  ��⁠, (c) t = 2350  ��⁠, (d) t = 2400  ��⁠, (e) t = 2450  ��⁠, (f) t = 2500  ��⁠, (g) t = 2550  ��⁠, (h) t = 2600  ��⁠, (i) t = 2650  ��⁠.

In order to quantitatively detect the molten pool dimensions as well as the remolten region dimensions, the molten pool characterization information in Fig. 14 is constructed by drawing the boundary on the YZ cross section based on the isothermal surface of the liquid phase line. It can be observed that the heights of the first track and second track are basically the same, but the depth of the second track increases relative to the first track. The molten pool width is mainly positively correlated with the laser power as well as the scanning speed (the laser line energy density �⁠). However, the remelted zone width is negatively correlated with the hatch spacing (the overlapping ratio). Overall, the forming quality of the specimens can be directly influenced by adjusting the laser power, scanning speed, and hatch spacing.

FIG. 14.

VIEW LARGEDOWNLOAD SLIDE

Double-track molten pool characterization information on YZ cross section.

In order to study the variation rule of the temperature in the center of the molten pool with time, Fig. 15 demonstrates the temperature variation curves with time for two reference points, A and B. Among them, the red dotted line indicates the liquid phase line temperature of SS316L. From the figure, it can be seen that the maximum temperature at the center of the molten pool in the first track is lower than that in the second track, which is mainly due to the heat accumulation generated after passing through the first track. The maximum temperature gradient was calculated to be 1.69 × 108 K/s. When the laser scanned the first track, the temperature in the center of the molten pool of the second track increased slightly. Similarly, when the laser scanned the second track, a similar situation existed in the first track. Since the temperature gradient in the second track is larger than that in the first track, the residence time of the liquid phase in the molten pool of the first track is longer than that of the second track.

FIG. 15.

VIEW LARGEDOWNLOAD SLIDE

Temperature profiles as a function of time for two reference points A and B.

C. Simulation analysis of molten pool under different process parameters

In order to deeply investigate the effects of various process parameters on the mesoscopic-scale temperature field, molten pool characteristic information and defects of HP-LPBF, numerical simulation experiments on mesoscopic-scale laser power, scanning speed, and hatch spacing of double-track molten pools were carried out.

1. Laser power

Figure 16 shows the effects of different laser power on the morphology and temperature field of the double-track molten pool at a scanning speed of 800 mm/s and a hatch spacing of 0.06 mm. When P = 50 W, a smaller molten pool is formed due to the lower heat generated by the Gaussian light source per unit time. This leads to a smaller track width, which results in adjacent track not lapping properly and the presence of a large number of unmelted powder particles, resulting in an increase in the number of defects, such as pores in the specimen. The surface of the track is relatively flat, and the depth is small. In addition, the temperature gradient before and after the molten pool was large, and the depression location appeared at the biased front end in Fig. 16(a). When P = 100 W, the surface of the track is flat and smooth with excellent lap. Due to the Marangoni effect, the velocity field of the molten pool is in the form of “vortex,” and the melt has good fluidity, and the maximum velocity reaches 2.15 m/s in Fig. 16(b). When P = 200 W, the heat generated by the Gaussian light source per unit time is too large, resulting in the melt rapidly reaching the evaporation temperature, generating a huge recoil pressure, forming a large molten pool, and the surface of the track is obviously raised. The melt movement is intense, especially the closed loop at the center end of the molten pool. At this time, the depth and width of the molten pool are large, leading to the expansion of the remolten region and the increased chance of the appearance of porosity defects in Fig. 16(c). The results show that at low laser power, the surface tension in the molten pool is dominant. At high laser power, recoil pressure is its main role.

FIG. 16.

VIEW LARGEDOWNLOAD SLIDE

Simulation results of double-track molten pool under different laser powers: (a) P = 50 W, (b) P = 100 W, (c) P = 200 W.

Table II shows the effect of different laser powers on the characteristic information of the double-track molten pool at a scanning speed of 800 mm/s and a hatch spacing of 0.06 mm. The negative overlapping ratio in the table indicates that the melt tracks are not lapped, and 26/29 indicates the melt depth of the first track/second track. It can be seen that with the increase in laser power, the melt depth, melt width, melt height, and remelted zone show a gradual increase. At the same time, the overlapping ratio also increases. Especially in the process of laser power from 50 to 200 W, the melting depth and melting width increased the most, which increased nearly 2 and 1.5 times, respectively. Meanwhile, the overlapping ratio also increases with the increase in laser power, which indicates that the melting and fusion of materials are better at high laser power. On the other hand, the dimensions of the molten pool did not change uniformly with the change of laser power. Specifically, the depth-to-width ratio of the molten pool increased from about 0.30 to 0.39 during the increase from 50 to 120 W, which further indicates that the effective heat transfer in the vertical direction is greater than that in the horizontal direction with the increase in laser power. This dimensional response to laser power is mainly affected by the recoil pressure and also by the difference in the densification degree between the powder layer and the metal substrate. In addition, according to the experimental results, the contact angle shows a tendency to increase and then decrease during the process of laser power increase, and always stays within the range of less than 33°. Therefore, in practical applications, it is necessary to select the appropriate laser power according to the specific needs in order to achieve the best processing results.

TABLE II.

Double-track molten pool characterization information at different laser powers.

Laser power (W)Depth (μm)Width (μm)Height (μm)Remolten region (μm)Overlapping ratio (%)Contact angle (°)
50 16 54 11 −10 23 
100 26/29 74 14 18 23.33 33 
200 37/45 116 21 52 93.33 28 

2. Scanning speed

Figure 17 demonstrates the effect of different scanning speeds on the morphology and temperature field of the double-track molten pool at a laser power of 100 W and a hatch spacing of 0.06 mm. With the gradual increase in scanning speed, the surface morphology of the molten pool evolves from circular to elliptical. When � = 200 mm/s, the slow scanning speed causes the material to absorb too much heat, which is very easy to trigger the overburning phenomenon. At this point, the molten pool is larger and the surface morphology is uneven. This situation is consistent with the previously discussed scenario with high laser power in Fig. 17(a). However, when � = 1600 mm/s, the scanning speed is too fast, resulting in the material not being able to absorb sufficient heat, which triggers the powder particles that fail to melt completely to have a direct effect on the bonding of the melt to the substrate. At this time, the molten pool volume is relatively small and the neighboring melt track cannot lap properly. This result is consistent with the previously discussed case of low laser power in Fig. 17(b). Overall, the ratio of the laser power to the scanning speed (the line energy density �⁠) has a direct effect on the temperature field and surface morphology of the molten pool.

FIG. 17.

VIEW LARGEDOWNLOAD SLIDE

Simulation results of double-track molten pool under different scanning speed: (a)  � = 200 mm/s, (b)  � = 1600 mm/s.

Table III shows the effects of different scanning speed on the characteristic information of the double-track molten pool under the condition of laser power of 100 W and hatch spacing of 0.06 mm. It can be seen that the scanning speed has a significant effect on the melt depth, melt width, melt height, remolten region, and overlapping ratio. With the increase in scanning speed, the melt depth, melt width, melt height, remelted zone, and overlapping ratio show a gradual decreasing trend. Among them, the melt depth and melt width decreased faster, while the melt height and remolten region decreased relatively slowly. In addition, when the scanning speed was increased from 200 to 800 mm/s, the decreasing speeds of melt depth and melt width were significantly accelerated, while the decreasing speeds of overlapping ratio were relatively slow. When the scanning speed was further increased to 1600 mm/s, the decreasing speeds of melt depth and melt width were further accelerated, and the un-lapped condition of the melt channel also appeared. In addition, the contact angle increases and then decreases with the scanning speed, and both are lower than 33°. Therefore, when selecting the scanning speed, it is necessary to make reasonable trade-offs according to the specific situation, and take into account the factors of melt depth, melt width, melt height, remolten region, and overlapping ratio, in order to achieve the best processing results.

TABLE III.

Double-track molten pool characterization information at different scanning speeds.

Scanning speed (mm/s)Depth (μm)Width (μm)Height (μm)Remolten region (μm)Overlapping ratio (%)Contact angle (°)
200 55/68 182 19/32 124 203.33 22 
1600 13 50 11 −16.67 31 

3. Hatch spacing

Figure 18 shows the effect of different hatch spacing on the morphology and temperature field of the double-track molten pool under the condition of laser power of 100 W and scanning speed of 800 mm/s. The surface morphology and temperature field of the first track and second track are basically the same, but slightly different. The first track shows a basically symmetric morphology along the scanning direction, while the second track shows a slight offset due to the difference in the heat transfer rate between the solidified material and the powder particles. When the hatch spacing is too small, the overlapping ratio increases and the probability of defects caused by remelting phenomenon grows. When the hatch spacing is too large, the neighboring melt track cannot overlap properly, and the powder particles are not completely melted, leading to an increase in the number of holes. In conclusion, the ratio of the line energy density � to the hatch spacing (the volume energy density E) has a significant effect on the temperature field and surface morphology of the molten pool.

FIG. 18.

VIEW LARGEDOWNLOAD SLIDE

Simulation results of double-track molten pool under different hatch spacings: (a) H = 0.03 mm, (b) H = 0.12 mm.

Table IV shows the effects of different hatch spacing on the characteristic information of the double-track molten pool under the condition of laser power of 100 W and scanning speed of 800 mm/s. It can be seen that the hatch spacing has little effect on the melt depth, melt width, and melt height, but has some effect on the remolten region. With the gradual expansion of hatch spacing, the remolten region shows a gradual decrease. At the same time, the overlapping ratio also decreased with the increase in hatch spacing. In addition, it is observed that the contact angle shows a tendency to increase and then remain stable when the hatch spacing increases, which has a more limited effect on it. Therefore, trade-offs and decisions need to be made on a case-by-case basis when selecting the hatch spacing.

TABLE IV.

Double-track molten pool characterization information at different hatch spacings.

Hatch spacing (mm)Depth (μm)Width (μm)Height (μm)Remolten region (μm)Overlapping ratio (%)Contact angle (°)
0.03 25/27 82 14 59 173.33 30 
0.12 26 78 14 −35 33 

In summary, the laser power, scanning speed, and hatch spacing have a significant effect on the formation of the molten pool, and the correct selection of these three process parameters is crucial to ensure the forming quality. In addition, the melt depth of the second track is slightly larger than that of the first track at higher line energy density � and volume energy density E. This is mainly due to the fact that a large amount of heat accumulation is generated after the first track, forming a larger molten pool volume, which leads to an increase in the melt depth.

D. Simulation analysis of molten pool with powder particle size and laser focal spot diameter

Figure 19 demonstrates the effect of different powder particle sizes and laser focal spot diameters on the morphology and temperature field of the double-track molten pool under a laser power of 100 W, a scanning speed of 800 mm/s, and a hatch spacing of 0.06 mm. In the process of melting coarse powder with small laser focal spot diameter, the laser energy cannot completely melt the larger powder particles, resulting in their partial melting and further generating excessive pore defects. The larger powder particles tend to generate zigzag molten pool edges, which cause an increase in the roughness of the melt track surface. In addition, the molten pool is also prone to generate the present spatter phenomenon, which can directly affect the quality of forming. The volume of the formed molten pool is relatively small, while the melt depth, melt width, and melt height are all smaller relative to the fine powder in Fig. 19(a). In the process of melting fine powders with a large laser focal spot diameter, the laser energy is able to melt the fine powder particles sufficiently, even to the point of overmelting. This results in a large number of fine spatters being generated at the edge of the molten pool, which causes porosity defects in the melt track in Fig. 19(b). In addition, the maximum velocity of the molten pool is larger for large powder particle sizes compared to small powder particle sizes, which indicates that the temperature gradient in the molten pool is larger for large powder particle sizes and the melt motion is more intense. However, the size of the laser focal spot diameter has a relatively small effect on the melt motion. However, a larger focal spot diameter induces a larger melt volume with greater depth, width, and height. In conclusion, a small powder size helps to reduce the surface roughness of the specimen, and a small laser spot diameter reduces the minimum forming size of a single track.

FIG. 19.

VIEW LARGEDOWNLOAD SLIDE

Simulation results of double-track molten pool with different powder particle size and laser focal spot diameter: (a) focal spot = 25 μm, coarse powder, (b) focal spot = 80 μm, fine powder.

Table V shows the maximum temperature gradient at the reference point for different powder sizes and laser focal spot diameters. As can be seen from the table, the maximum temperature gradient is lower than that of HP-LPBF for both coarse powders with a small laser spot diameter and fine powders with a large spot diameter, a phenomenon that leads to an increase in the heat transfer rate of HP-LPBF, which in turn leads to a corresponding increase in the cooling rate and, ultimately, to the formation of finer microstructures.

TABLE V.

Maximum temperature gradient at the reference point for different powder particle sizes and laser focal spot diameters.

Laser power (W)Scanning speed (mm/s)Hatch spacing (mm)Average powder size (μm)Laser focal spot diameter (μm)Maximum temperature gradient (×107 K/s)
100 800 0.06 31.7 25 7.89 
11.5 80 7.11 

IV. CONCLUSIONS

In this study, the geometrical characteristics of 3D coarse and fine powder particles were first calculated using DEM and then numerical simulations of single track and double track in the process of forming SS316L from monolayer HP-LPBF at mesoscopic scale were developed using CFD method. The effects of Marangoni convection, surface tension, recoil pressure, gravity, thermal convection, thermal radiation, and evaporative heat dissipation on the heat and mass transfer in the molten pool were considered in this model. The effects of laser power, scanning speed, and hatch spacing on the dynamics of the single-track and double-track molten pools, as well as on other characteristic information, were investigated. The effects of the powder particle size on the molten pool were investigated comparatively with the laser focal spot diameter. The main conclusions are as follows:

  1. The results show that the temperature gradient at the front of the molten pool is significantly larger than that at the tail, and the molten pool exhibits a “comet” morphology. At the top of the molten pool, there is a slightly concave region, which is the result of the coupling of Marangoni convection, recoil pressure, and surface tension. The melt flow forms two closed loops, which are mainly influenced by temperature gradients and surface tension. This special dynamic behavior of the melt tends to form an “elliptical” molten pool and an almost “mountain” shape in single-track forming.
  2. The basic characteristics of the three-dimensional morphology and temperature field of the second track are similar to those of the first track, but there are subtle differences. The first track exhibits a basically symmetrical shape; however, due to the difference in thermal diffusion rates between the solidified metal and the powder, a slight asymmetry in the molten pool morphology of the second track occurs. After forming through the first track, there is a significant heat buildup in the powder bed, resulting in a longer dynamic time of the melt, which increases the life of the molten pool. The heights of the first track and second track remained essentially the same, but the depth of the second track was greater relative to the first track. In addition, the maximum temperature gradient was 1.69 × 108 K/s during HP-LPBF forming.
  3. At low laser power, the surface tension in the molten pool plays a dominant role. At high laser power, recoil pressure becomes the main influencing factor. With the increase of laser power, the effective heat transfer in the vertical direction is superior to that in the horizontal direction. With the gradual increase of scanning speed, the surface morphology of the molten pool evolves from circular to elliptical. In addition, the scanning speed has a significant effect on the melt depth, melt width, melt height, remolten region, and overlapping ratio. Too large or too small hatch spacing will lead to remelting or non-lap phenomenon, which in turn causes the formation of defects.
  4. When using a small laser focal spot diameter, it is difficult to completely melt large powder particle sizes, resulting in partial melting and excessive porosity generation. At the same time, large powder particles produce curved edges of the molten pool, resulting in increased surface roughness of the melt track. In addition, spatter occurs, which directly affects the forming quality. At small focal spot diameters, the molten pool volume is relatively small, and the melt depth, the melt width, and the melt height are correspondingly small. Taken together, the small powder particle size helps to reduce surface roughness, while the small spot diameter reduces the forming size.

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Predicting solid-state phase transformations during metal additive manufacturing: A case study on electron-beam powder bed fusion of Inconel-738

Predicting solid-state phase transformations during metal additive manufacturing: A case study on electron-beam powder bed fusion of Inconel-738

금속 적층 제조 중 고체 상 변형 예측: Inconel-738의 전자빔 분말층 융합에 대한 사례 연구

Nana Kwabena Adomako a, Nima Haghdadi a, James F.L. Dingle bc, Ernst Kozeschnik d, Xiaozhou Liao bc, Simon P. Ringer bc, Sophie Primig a

Abstract

Metal additive manufacturing (AM) has now become the perhaps most desirable technique for producing complex shaped engineering parts. However, to truly take advantage of its capabilities, advanced control of AM microstructures and properties is required, and this is often enabled via modeling. The current work presents a computational modeling approach to studying the solid-state phase transformation kinetics and the microstructural evolution during AM. Our approach combines thermal and thermo-kinetic modelling. A semi-analytical heat transfer model is employed to simulate the thermal history throughout AM builds. Thermal profiles of individual layers are then used as input for the MatCalc thermo-kinetic software. The microstructural evolution (e.g., fractions, morphology, and composition of individual phases) for any region of interest throughout the build is predicted by MatCalc. The simulation is applied to an IN738 part produced by electron beam powder bed fusion to provide insights into how γ′ precipitates evolve during thermal cycling. Our simulations show qualitative agreement with our experimental results in predicting the size distribution of γ′ along the build height, its multimodal size character, as well as the volume fraction of MC carbides. Our findings indicate that our method is suitable for a range of AM processes and alloys, to predict and engineer their microstructures and properties.

Graphical Abstract

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Keywords

Additive manufacturing, Simulation, Thermal cycles, γ′ phase, IN738

1. Introduction

Additive manufacturing (AM) is an advanced manufacturing method that enables engineering parts with intricate shapes to be fabricated with high efficiency and minimal materials waste. AM involves building up 3D components layer-by-layer from feedstocks such as powder [1]. Various alloys, including steel, Ti, Al, and Ni-based superalloys, have been produced using different AM techniques. These techniques include directed energy deposition (DED), electron- and laser powder bed fusion (E-PBF and L-PBF), and have found applications in a variety of industries such as aerospace and power generation [2][3][4]. Despite the growing interest, certain challenges limit broader applications of AM fabricated components in these industries and others. One of such limitations is obtaining a suitable and reproducible microstructure that offers the desired mechanical properties consistently. In fact, the AM as-built microstructure is highly complex and considerably distinctive from its conventionally processed counterparts owing to the complicated thermal cycles arising from the deposition of several layers upon each other [5][6].

Several studies have reported that the solid-state phases and solidification microstructure of AM processed alloys such as CMSX-4, CoCr [7][8], Ti-6Al-4V [9][10][11]IN738 [6]304L stainless steel [12], and IN718 [13][14] exhibit considerable variations along the build direction. For instance, references [9][10] have reported that there is a variation in the distribution of α and β phases along the build direction in Ti-alloys. Similarly, the microstructure of an L-PBF fabricated martensitic steel exhibits variations in the fraction of martensite [15]. Furthermore, some of the present authors and others [6][16][17][18][19][20] have recently reviewed and reported that there is a difference in the morphology and fraction of nanoscale precipitates as a function of build height in Ni-based superalloys. These non-uniformities in the as-built microstructure result in an undesired heterogeneity in mechanical and other important properties such as corrosion and oxidation [19][21][22][23]. To obtain the desired microstructure and properties, additional processing treatments are utilized, but this incurs extra costs and may lead to precipitation of detrimental phases and grain coarsening. Therefore, a through-process understanding of the microstructure evolution under repeated heating and cooling is now needed to further advance 3D printed microstructure and property control.

It is now commonly understood that the microstructure evolution during printing is complex, and most AM studies concentrate on the microstructure and mechanical properties of the final build only. Post-printing studies of microstructure characteristics at room temperature miss crucial information on how they evolve. In-situ measurements and modelling approaches are required to better understand the complex microstructural evolution under repeated heating and cooling. Most in-situ measurements in AM focus on monitoring the microstructural changes, such as phase transformations and melt pool dynamics during fabrication using X-ray scattering and high-speed X-ray imaging [24][25][26][27]. For example, Zhao et al. [25] measured the rate of solidification and described the α/β phase transformation during L-PBF of Ti-6Al-4V in-situ. Also, Wahlmann et al. [21] recently used an L-PBF machine coupled with X-ray scattering to investigate the changes in CMSX-4 phase during successive melting processes. Although these techniques provide significant understanding of the basic principles of AM, they are not widely accessible. This is due to the great cost of the instrument, competitive application process, and complexities in terms of the experimental set-up, data collection, and analysis [26][28].

Computational modeling techniques are promising and more widely accessible tools that enable advanced understanding, prediction, and engineering of microstructures and properties during AM. So far, the majority of computational studies have concentrated on physics based process models for metal AM, with the goal of predicting the temperature profile, heat transfer, powder dynamics, and defect formation (e.g., porosity) [29][30]. In recent times, there have been efforts in modeling of the AM microstructure evolution using approaches such as phase-field [31], Monte Carlo (MC) [32], and cellular automata (CA) [33], coupled with finite element simulations for temperature profiles. However, these techniques are often restricted to simulating the evolution of solidification microstructures (e.g., grain and dendrite structure) and defects (e.g., porosity). For example, Zinovieva et al. [33] predicted the grain structure of L-PBF Ti-6Al-4V using finite difference and cellular automata methods. However, studies on the computational modelling of the solid-state phase transformations, which largely determine the resulting properties, remain limited. This can be attributed to the multi-component and multi-phase nature of most engineering alloys in AM, along with the complex transformation kinetics during thermal cycling. This kind of research involves predictions of the thermal cycle in AM builds, and connecting it to essential thermodynamic and kinetic data as inputs for the model. Based on the information provided, the thermokinetic model predicts the history of solid-state phase microstructure evolution during deposition as output. For example, a multi-phase, multi-component mean-field model has been developed to simulate the intermetallic precipitation kinetics in IN718 [34] and IN625 [35] during AM. Also, Basoalto et al. [36] employed a computational framework to examine the contrasting distributions of process-induced microvoids and precipitates in two Ni-based superalloys, namely IN718 and CM247LC. Furthermore, McNamara et al. [37] established a computational model based on the Johnson-Mehl-Avrami model for non-isothermal conditions to predict solid-state phase transformation kinetics in L-PBF IN718 and DED Ti-6Al-4V. These models successfully predicted the size and volume fraction of individual phases and captured the repeated nucleation and dissolution of precipitates that occur during AM.

In the current study, we propose a modeling approach with appreciably short computational time to investigate the detailed microstructural evolution during metal AM. This may include obtaining more detailed information on the morphologies of phases, such as size distribution, phase fraction, dissolution and nucleation kinetics, as well as chemistry during thermal cycling and final cooling to room temperature. We utilize the combination of the MatCalc thermo-kinetic simulator and a semi-analytical heat conduction model. MatCalc is a software suite for simulation of phase transformations, microstructure evolution and certain mechanical properties in engineering alloys. It has successfully been employed to simulate solid-state phase transformations in Ni-based superalloys [38][39], steels [40], and Al alloys [41] during complex thermo-mechanical processes. MatCalc uses the classical nucleation theory as well as the so-called Svoboda-Fischer-Fratzl-Kozeschnik (SFFK) growth model as the basis for simulating precipitation kinetics [42]. Although MatCalc was originally developed for conventional thermo-mechanical processes, we will show that it is also applicable for AM if the detailed time-temperature profile of the AM build is known. The semi-analytical heat transfer code developed by Stump and Plotkowski [43] is used to simulate these profile throughout the AM build.

1.1. Application to IN738

Inconel-738 (IN738) is a precipitation hardening Ni-based superalloy mainly employed in high-temperature components, e.g. in gas turbines and aero-engines owing to its exceptional mechanical properties at temperatures up to 980 °C, coupled with high resistance to oxidation and corrosion [44]. Its superior high-temperature strength (∼1090 MPa tensile strength) is provided by the L12 ordered Ni3(Al,Ti) γ′ phase that precipitates in a face-centered cubic (FCC) γ matrix [45][46]. Despite offering great properties, IN738, like most superalloys with high γ′ fractions, is challenging to process owing to its propensity to hot cracking [47][48]. Further, machining of such alloys is challenging because of their high strength and work-hardening rates. It is therefore difficult to fabricate complex INC738 parts using traditional manufacturing techniques like casting, welding, and forging.

The emergence of AM has now made it possible to fabricate such parts from IN738 and other superalloys. Some of the current authors’ recent research successfully applied E-PBF to fabricate defect-free IN738 containing γ′ throughout the build [16][17]. The precipitated γ′ were heterogeneously distributed. In particular, Haghdadi et al. [16] studied the origin of the multimodal size distribution of γ′, while Lim et al. [17] investigated the gradient in γ′ character with build height and its correlation to mechanical properties. Based on these results, the present study aims to extend the understanding of the complex and site-specific microstructural evolution in E-PBF IN738 by using a computational modelling approach. New experimental evidence (e.g., micrographs not published previously) is presented here to support the computational results.

2. Materials and Methods

2.1. Materials preparation

IN738 Ni-based superalloy (59.61Ni-8.48Co-7.00Al-17.47Cr-3.96Ti-1.01Mo-0.81W-0.56Ta-0.49Nb-0.47C-0.09Zr-0.05B, at%) gas-atomized powder was used as feedstock. The powders, with average size of 60 ± 7 µm, were manufactured by Praxair and distributed by Astro Alloys Inc. An Arcam Q10 machine by GE Additive with an acceleration voltage of 60 kV was used to fabricate a 15 × 15 × 25 mm3 block (XYZ, Z: build direction) on a 316 stainless steel substrate. The block was 3D-printed using a ‘random’ spot melt pattern. The random spot melt pattern involves randomly selecting points in any given layer, with an equal chance of each point being melted. Each spot melt experienced a dwell time of 0.3 ms, and the layer thickness was 50 µm. Some of the current authors have previously characterized the microstructure of the very same and similar builds in more detail [16][17]. A preheat temperature of ∼1000 °C was set and kept during printing to reduce temperature gradients and, in turn, thermal stresses [49][50][51]. Following printing, the build was separated from the substrate through electrical discharge machining. It should be noted that this sample was simultaneously printed with the one used in [17] during the same build process and on the same build plate, under identical conditions.

2.2. Microstructural characterization

The printed sample was longitudinally cut in the direction of the build using a Struers Accutom-50, ground, and then polished to 0.25 µm suspension via standard techniques. The polished x-z surface was electropolished and etched using Struers A2 solution (perchloric acid in ethanol). Specimens for image analysis were polished using a 0.06 µm colloidal silica. Microstructure analyses were carried out across the height of the build using optical microscopy (OM) and scanning electron microscopy (SEM) with focus on the microstructure evolution (γ′ precipitates) in individual layers. The position of each layer being analyzed was determined by multiplying the layer number by the layer thickness (50 µm). It should be noted that the position of the first layer starts where the thermal profile is tracked (in this case, 2 mm from the bottom). SEM images were acquired using a JEOL 7001 field emission microscope. The brightness and contrast settings, acceleration voltage of 15 kV, working distance of 10 mm, and other SEM imaging parameters were all held constant for analysis of the entire build. The ImageJ software was used for automated image analysis to determine the phase fraction and size of γ′ precipitates and carbides. A 2-pixel radius Gaussian blur, following a greyscale thresholding and watershed segmentation was used [52]. Primary γ′ sizes (>50 nm), were measured using equivalent spherical diameters. The phase fractions were considered equal to the measured area fraction. Secondary γ′ particles (<50 nm) were not considered here. The γ′ size in the following refers to the diameter of a precipitate.

2.3. Hardness testing

A Struers DuraScan tester was utilized for Vickers hardness mapping on a polished x-z surface, from top to bottom under a maximum load of 100 mN and 10 s dwell time. 30 micro-indentations were performed per row. According to the ASTM standard [53], the indentations were sufficiently distant (∼500 µm) to assure that strain-hardened areas did not interfere with one another.

2.4. Computational simulation of E-PBF IN738 build

2.4.1. Thermal profile modeling

The thermal history was generated using the semi-analytical heat transfer code (also known as the 3DThesis code) developed by Stump and Plotkowski [43]. This code is an open-source C++ program which provides a way to quickly simulate the conductive heat transfer found in welding and AM. The key use case for the code is the simulation of larger domains than is practicable with Computational Fluid Dynamics/Finite Element Analysis programs like FLOW-3D AM. Although simulating conductive heat transfer will not be an appropriate simplification for some investigations (for example the modelling of keyholding or pore formation), the 3DThesis code does provide fast estimates of temperature, thermal gradient, and solidification rate which can be useful for elucidating microstructure formation across entire layers of an AM build. The mathematics involved in the code is as follows:

In transient thermal conduction during welding and AM, with uniform and constant thermophysical properties and without considering fluid convection and latent heat effects, energy conservation can be expressed as:(1)��∂�∂�=�∇2�+�̇where � is density, � specific heat, � temperature, � time, � thermal conductivity, and �̇ a volumetric heat source. By assuming a semi-infinite domain, Eq. 1 can be analytically solved. The solution for temperature at a given time (t) using a volumetric Gaussian heat source is presented as:(2)��,�,�,�−�0=33�����32∫0�1������exp−3�′�′2��+�′�′2��+�′�′2����′(3)and��=12��−�′+��2for�=�,�,�(4)and�′�′=�−���′Where � is the vector �,�,� and �� is the location of the heat source.

The numerical integration scheme used is an adaptive Gaussian quadrature method based on the following nondimensionalization:(5)�=��xy2�,�′=��xy2�′,�=��xy,�=��xy,�=��xy,�=���xy

A more detailed explanation of the mathematics can be found in reference [43].

The main source of the thermal cycling present within a powder-bed fusion process is the fusion of subsequent layers. Therefore, regions near the top of a build are expected to undergo fewer thermal cycles than those closer to the bottom. For this purpose, data from the single scan’s thermal influence on multiple layers was spliced to represent the thermal cycles experienced at a single location caused by multiple subsequent layers being fused.

The cross-sectional area simulated by this model was kept constant at 1 × 1 mm2, and the depth was dependent on the build location modelled with MatCalc. For a build location 2 mm from the bottom, the maximum number of layers to simulate is 460. Fig. 1a shows a stitched overview OM image of the entire build indicating the region where this thermal cycle is simulated and tracked. To increase similarity with the conditions of the physical build, each thermal history was constructed from the results of two simulations generated with different versions of a random scan path. The parameters used for these thermal simulations can be found in Table 1. It should be noted that the main purpose of the thermal profile modelling was to demonstrate how the conditions at different locations of the build change relative to each other. Accurately predicting the absolute temperature during the build would require validation via a temperature sensor measurement during the build process which is beyond the scope of the study. Nonetheless, to establish the viability of the heat source as a suitable approximation for this study, an additional sensitivity analysis was conducted. This analysis focused on the influence of energy input on γ′ precipitation behavior, the central aim of this paper. This was achieved by employing varying beam absorption energies (0.76, 0.82 – the values utilized in the simulation, and 0.9). The direct impact of beam absorption efficiency on energy input into the material was investigated. Specifically, the initial 20 layers of the build were simulated and subsequently compared to experimental data derived from SEM. While phase fractions were found to be consistent across all conditions, disparities emerged in the mean size of γ′ precipitates. An absorption efficiency of 0.76 yielded a mean size of approximately 70 nm. Conversely, absorption efficiencies of 0.82 and 0.9 exhibited remarkably similar mean sizes of around 130 nm, aligning closely with the outcomes of the experiments.

Fig. 1

Table 1. A list of parameters used in thermal simulation of E-PBF.

ParameterValue
Spatial resolution5 µm
Time step0.5 s
Beam diameter200 µm
Beam penetration depth1 µm
Beam power1200 W
Beam absorption efficiency0.82
Thermal conductivity25.37 W/(m⋅K)
Chamber temperature1000 °C
Specific heat711.756 J/(kg⋅K)
Density8110 kg/m3

2.4.2. Thermo-kinetic simulation

The numerical analyses of the evolution of precipitates was performed using MatCalc version 6.04 (rel 0.011). The thermodynamic (‘mc_ni.tdb’, version 2.034) and diffusion (‘mc_ni.ddb’, version 2.007) databases were used. MatCalc’s basic principles are elaborated as follows:

The nucleation kinetics of precipitates are computed using a computational technique based on a classical nucleation theory [54] that has been modified for systems with multiple components [42][55]. Accordingly, the transient nucleation rate (�), which expresses the rate at which nuclei are formed per unit volume and time, is calculated as:(6)�=�0��*∙�xp−�*�∙�∙exp−��where �0 denotes the number of active nucleation sites, �* the rate of atomic attachment, � the Boltzmann constant, � the temperature, �* the critical energy for nucleus formation, τ the incubation time, and t the time. � (Zeldovich factor) takes into consideration that thermal excitation destabilizes the nucleus as opposed to its inactive state [54]. Z is defined as follows:(7)�=−12�kT∂2∆�∂�2�*12where ∆� is the overall change in free energy due to the formation of a nucleus and n is the nucleus’ number of atoms. ∆�’s derivative is evaluated at n* (critical nucleus size). �* accounts for the long-range diffusion of atoms required for nucleation, provided that the matrix’ and precipitates’ composition differ. Svoboda et al. [42] developed an appropriate multi-component equation for �*, which is given by:(8)�*=4��*2�4�∑�=1��ki−�0�2�0��0�−1where �* denotes the critical radius for nucleation, � represents atomic distance, and � is the molar volume. �ki and �0� represent the concentration of elements in the precipitate and matrix, respectively. The parameter �0� denotes the rate of diffusion of the ith element within the matrix. The expression for the incubation time � is expressed as [54]:(9)�=12�*�2

and �*, which represents the critical energy for nucleation:(10)�*=16�3�3∆�vol2where � is the interfacial energy, and ∆Gvol the change in the volume free energy. The critical nucleus’ composition is similar to the γ′ phase’s equilibrium composition at the same temperature. � is computed based on the precipitate and matrix compositions, using a generalized nearest neighbor broken bond model, with the assumption of interfaces being planar, sharp, and coherent [56][57][58].

In Eq. 7, it is worth noting that �* represents the fundamental variable in the nucleation theory. It contains �3/∆�vol2 and is in the exponent of the nucleation rate. Therefore, even small variations in γ and/or ∆�vol can result in notable changes in �, especially if �* is in the order of �∙�. This is demonstrated in [38] for UDIMET 720 Li during continuous cooling, where these quantities change steadily during precipitation due to their dependence on matrix’ and precipitate’s temperature and composition. In the current work, these changes will be even more significant as the system is exposed to multiple cycles of rapid cooling and heating.

Once nucleated, the growth of a precipitate is assessed using the radius and composition evolution equations developed by Svoboda et al. [42] with a mean-field method that employs the thermodynamic extremal principle. The expression for the total Gibbs free energy of a thermodynamic system G, which consists of n components and m precipitates, is given as follows:(11)�=∑���0��0�+∑�=1�4���33��+∑�=1��ki�ki+∑�=1�4���2��.

The chemical potential of component � in the matrix is denoted as �0�(�=1,…,�), while the chemical potential of component � in the precipitate is represented by �ki(�=1,…,�,�=1,…,�). These chemical potentials are defined as functions of the concentrations �ki(�=1,…,�,�=1,…,�). The interface energy density is denoted as �, and �� incorporates the effects of elastic energy and plastic work resulting from the volume change of each precipitate.

Eq. (12) establishes that the total free energy of the system in its current state relies on the independent state variables: the sizes (radii) of the precipitates �� and the concentrations of each component �ki. The remaining variables can be determined by applying the law of mass conservation to each component �. This can be represented by the equation:(12)��=�0�+∑�=1�4���33�ki,

Furthermore, the global mass conservation can be expressed by equation:(13)�=∑�=1���When a thermodynamic system transitions to a more stable state, the energy difference between the initial and final stages is dissipated. This model considers three distinct forms of dissipation effects [42]. These include dissipations caused by the movement of interfaces, diffusion within the precipitate and diffusion within the matrix.

Consequently, �̇� (growth rate) and �̇ki (chemical composition’s rate of change) of the precipitate with index � are derived from the linear system of equation system:(14)�ij��=��where �� symbolizes the rates �̇� and �̇ki [42]. Index i contains variables for precipitate radius, chemical composition, and stoichiometric boundary conditions suggested by the precipitate’s crystal structure. Eq. (10) is computed separately for every precipitate �. For a more detailed description of the formulae for the coefficients �ij and �� employed in this work please refer to [59].

The MatCalc software was used to perform the numerical time integration of �̇� and �̇ki of precipitates based on the classical numerical method by Kampmann and Wagner [60]. Detailed information on this method can be found in [61]. Using this computational method, calculations for E-PBF thermal cycles (cyclic heating and cooling) were computed and compared to experimental data. The simulation took approximately 2–4 hrs to complete on a standard laptop.

3. Results

3.1. Microstructure

Fig. 1 displays a stitched overview image and selected SEM micrographs of various γ′ morphologies and carbides after observations of the X-Z surface of the build from the top to 2 mm above the bottom. Fig. 2 depicts a graph that charts the average size and phase fraction of the primary γ′, as it changes with distance from the top to the bottom of the build. The SEM micrographs show widespread primary γ′ precipitation throughout the entire build, with the size increasing in the top to bottom direction. Particularly, at the topmost height, representing the 460th layer (Z = 22.95 mm), as seen in Fig. 1b, the average size of γ′ is 110 ± 4 nm, exhibiting spherical shapes. This is representative of the microstructure after it solidifies and cools to room temperature, without experiencing additional thermal cycles. The γ′ size slightly increases to 147 ± 6 nm below this layer and remains constant until 0.4 mm (∼453rd layer) from the top. At this position, the microstructure still closely resembles that of the 460th layer. After the 453rd layer, the γ′ size grows rapidly to ∼503 ± 19 nm until reaching the 437th layer (1.2 mm from top). The γ′ particles here have a cuboidal shape, and a small fraction is coarser than 600 nm. γ′ continue to grow steadily from this position to the bottom (23 mm from the top). A small fraction of γ′ is > 800 nm.

Fig. 2

Besides primary γ′, secondary γ′ with sizes ranging from 5 to 50 nm were also found. These secondary γ′ precipitates, as seen in Fig. 1f, were present only in the bottom and middle regions. A detailed analysis of the multimodal size distribution of γ′ can be found in [16]. There is no significant variation in the phase fraction of the γ′ along the build. The phase fraction is ∼ 52%, as displayed in Fig. 2. It is worth mentioning that the total phase fraction of γ′ was estimated based on the primary γ′ phase fraction because of the small size of secondary γ′. Spherical MC carbides with sizes ranging from 50 to 400 nm and a phase fraction of 0.8% were also observed throughout the build. The carbides are the light grey precipitates in Fig. 1g. The light grey shade of carbides in the SEM images is due to their composition and crystal structure [52]. These carbides are not visible in Fig. 1b-e because they were dissolved during electro-etching carried out after electropolishing. In Fig. 1g, however, the sample was examined directly after electropolishing, without electro-etching.

Table 2 shows the nominal and measured composition of γ′ precipitates throughout the build by atom probe microscopy as determined in our previous study [17]. No build height-dependent composition difference was observed in either of the γ′ precipitate populations. However, there was a slight disparity between the composition of primary and secondary γ′. Among the main γ′ forming elements, the primary γ′ has a high Ti concentration while secondary γ′ has a high Al concentration. A detailed description of the atom distribution maps and the proxigrams of the constituent elements of γ′ throughout the build can be found in [17].

Table 2. Bulk IN738 composition determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES). Compositions of γ, primary γ′, and secondary γ′ at various locations in the build measured by APT. This information is reproduced from data in Ref. [17] with permission.

at%NiCrCoAlMoWTiNbCBZrTaOthers
Bulk59.1217.478.487.001.010.813.960.490.470.050.090.560.46
γ matrix
Top50.4832.9111.591.941.390.820.440.80.030.030.020.24
Mid50.3732.6111.931.791.540.890.440.10.030.020.020.010.23
Bot48.1034.5712.082.141.430.880.480.080.040.030.010.12
Primary γ′
Top72.172.513.4412.710.250.397.780.560.030.020.050.08
Mid71.602.573.2813.550.420.687.040.730.010.030.040.04
Bot72.342.473.8612.500.260.447.460.500.050.020.020.030.04
Secondary γ′
Mid70.424.203.2314.190.631.035.340.790.030.040.040.05
Bot69.914.063.6814.320.811.045.220.650.050.100.020.11

3.2. Hardness

Fig. 3a shows the Vickers hardness mapping performed along the entire X-Z surface, while Fig. 3b shows the plot of average hardness at different build heights. This hardness distribution is consistent with the γ′ precipitate size gradient across the build direction in Fig. 1Fig. 2. The maximum hardness of ∼530 HV1 is found at ∼0.5 mm away from the top surface (Z = 22.5), where γ′ particles exhibit the smallest observed size in Fig. 2b. Further down the build (∼ 2 mm from the top), the hardness drops to the 440–490 HV1 range. This represents the region where γ′ begins to coarsen. The hardness drops further to 380–430 HV1 at the bottom of the build.

Fig. 3

3.3. Modeling of the microstructural evolution during E-PBF

3.3.1. Thermal profile modeling

Fig. 4 shows the simulated thermal profile of the E-PBF build at a location of 23 mm from the top of the build, using a semi-analytical heat conduction model. This profile consists of the time taken to deposit 460 layers until final cooling, as shown in Fig. 4a. Fig. 4b-d show the magnified regions of Fig. 4a and reveal the first 20 layers from the top, a single layer (first layer from the top), and the time taken for the build to cool after the last layer deposition, respectively.

Fig. 4

The peak temperatures experienced by previous layers decrease progressively as the number of layers increases but never fall below the build preheat temperature (1000 °C). Our simulated thermal cycle may not completely capture the complexity of the actual thermal cycle utilized in the E-PBF build. For instance, the top layer (Fig. 4c), also representing the first deposit’s thermal profile without additional cycles (from powder heating, melting, to solidification), recorded the highest peak temperature of 1390 °C. Although this temperature is above the melting range of the alloy (1230–1360 °C) [62], we believe a much higher temperature was produced by the electron beam to melt the powder. Nevertheless, the solidification temperature and dynamics are outside the scope of this study as our focus is on the solid-state phase transformations during deposition. It takes ∼25 s for each layer to be deposited and cooled to the build temperature. The interlayer dwell time is 125 s. The time taken for the build to cool to room temperature (RT) after final layer deposition is ∼4.7 hrs (17,000 s).

3.3.2. MatCalc simulation

During the MatCalc simulation, the matrix phase is defined as γ. γ′, and MC carbide are included as possible precipitates. The domain of these precipitates is set to be the matrix (γ), and nucleation is assumed to be homogenous. In homogeneous nucleation, all atoms of the unit volume are assumed to be potential nucleation sitesTable 3 shows the computational parameters used in the simulation. All other parameters were set at default values as recommended in the version 6.04.0011 of MatCalc. The values for the interfacial energies are automatically calculated according to the generalized nearest neighbor broken bond model and is one of the most outstanding features in MatCalc [56][57][58]. It should be noted that the elastic misfit strain was not included in the calculation. The output of MatCalc includes phase fraction, size, nucleation rate, and composition of the precipitates. The phase fraction in MatCalc is the volume fraction. Although the experimental phase fraction is the measured area fraction, it is relatively similar to the volume fraction. This is because of the generally larger precipitate size and similar morphology at the various locations along the build [63]. A reliable phase fraction comparison between experiment and simulation can therefore be made.

Table 3. Computational parameters used in the simulation.

Precipitation domainγ
Nucleation site γ′Bulk (homogenous)
Nucleation site MC carbideBulk (Homogenous)
Precipitates class size250
Regular solution critical temperature γ′2500 K[64]
Calculated interfacial energyγ′ = 0.080–0.140 J/m2 and MC carbide = 0.410–0.430 J/m2
3.3.2.1. Precipitate phase fraction

Fig. 5a shows the simulated phase fraction of γ′ and MC carbide during thermal cycling. Fig. 5b is a magnified view of 5a showing the simulated phase fraction at the center points of the top 70 layers, whereas Fig. 5c corresponds to the first two layers from the top. As mentioned earlier, the top layer (460th layer) represents the microstructure after solidification. The microstructure of the layers below is determined by the number of thermal cycles, which increases with distance to the top. For example, layers 459, 458, 457, up to layer 1 (region of interest) experience 1, 2, 3 and 459 thermal cycles, respectively. In the top layer in Fig. 5c, the volume fraction of γ′ and carbides increases with temperature. For γ′, it decreases to zero when the temperature is above the solvus temperature after a few seconds. Carbides, however, remain constant in their volume fraction reaching equilibrium (phase fraction ∼ 0.9%) in a short time. The topmost layer can be compared to the first deposit, and the peak in temperature symbolizes the stage where the electron beam heats the powder until melting. This means γ′ and carbide precipitation might have started in the powder particles during heating from the build temperature and electron beam until the onset of melting, where γ′ dissolves, but carbides remain stable [28].

Fig. 5

During cooling after deposition, γ′ reprecipitates at a temperature of 1085 °C, which is below its solvus temperature. As cooling progresses, the phase fraction increases steadily to ∼27% and remains constant at 1000 °C (elevated build temperature). The calculated equilibrium fraction of phases by MatCalc is used to show the complex precipitation characteristics in this alloy. Fig. 6 shows that MC carbides form during solidification at 1320 °C, followed by γ′, which precipitate when the solidified layer cools to 1140 °C. This indicates that all deposited layers might contain a negligible amount of these precipitates before subsequent layer deposition, while being at the 1000 °C build temperature or during cooling to RT. The phase diagram also shows that the equilibrium fraction of the γ′ increases as temperature decreases. For instance, at 1000, 900, and 800 °C, the phase fractions are ∼30%, 38%, and 42%, respectively.

Fig. 6

Deposition of subsequent layers causes previous layers to undergo phase transformations as they are exposed to several thermal cycles with different peak temperatures. In Fig. 5c, as the subsequent layer is being deposited, γ′ in the previous layer (459th layer) begins to dissolve as the temperature crosses the solvus temperature. This is witnessed by the reduction of the γ′ phase fraction. This graph also shows how this phase dissolves during heating. However, the phase fraction of MC carbide remains stable at high temperatures and no dissolution is seen during thermal cycling. Upon cooling, the γ′ that was dissolved during heating reprecipitates with a surge in the phase fraction until 1000 °C, after which it remains constant. This microstructure is similar to the solidification microstructure (layer 460), with a similar γ′ phase fraction (∼27%).

The complete dissolution and reprecipitation of γ′ continue for several cycles until the 50th layer from the top (layer 411), where the phase fraction does not reach zero during heating to the peak temperature (see Fig. 5d). This indicates the ‘partial’ dissolution of γ′, which continues progressively with additional layers. It should be noted that the peak temperatures for layers that underwent complete dissolution were much higher (1170–1300 °C) than the γ′ solvus.

The dissolution and reprecipitation of γ′ during thermal cycling are further confirmed in Fig. 7, which summarizes the nucleation rate, phase fraction, and concentration of major elements that form γ′ in the matrix. Fig. 7b magnifies a single layer (3rd layer from top) within the full dissolution region in Fig. 7a to help identify the nucleation and growth mechanisms. From Fig. 7b, γ′ nucleation begins during cooling whereby the nucleation rate increases to reach a maximum value of approximately 1 × 1020 m−3s−1. This fast kinetics implies that some rearrangement of atoms is required for γ′ precipitates to form in the matrix [65][66]. The matrix at this stage is in a non-equilibrium condition. Its composition is similar to the nominal composition and remains unchanged. The phase fraction remains insignificant at this stage although nucleation has started. The nucleation rate starts declining upon reaching the peak value. Simultaneously, diffusion-controlled growth of existing nuclei occurs, depleting the matrix of γ′ forming elements (Al and Ti). Thus, from (7)(11), ∆�vol continuously decreases until nucleation ceases. The growth of nuclei is witnessed by the increase in phase fraction until a constant level is reached at 27% upon cooling to and holding at build temperature. This nucleation event is repeated several times.

Fig. 7

At the onset of partial dissolution, the nucleation rate jumps to 1 × 1021 m−3s−1, and then reduces sharply at the middle stage of partial dissolution. The nucleation rate reaches 0 at a later stage. Supplementary Fig. S1 shows a magnified view of the nucleation rate, phase fraction, and thermal profile, underpinning this trend. The jump in nucleation rate at the onset is followed by a progressive reduction in the solute content of the matrix. The peak temperatures (∼1130–1160 °C) are lower than those in complete dissolution regions but still above or close to the γ′ solvus. The maximum phase fraction (∼27%) is similar to that of the complete dissolution regions. At the middle stage, the reduction in nucleation rate is accompanied by a sharp drop in the matrix composition. The γ′ fraction drops to ∼24%, where the peak temperatures of the layers are just below or at γ′ solvus. The phase fraction then increases progressively through the later stage of partial dissolution to ∼30% towards the end of thermal cycling. The matrix solute content continues to drop although no nucleation event is seen. The peak temperatures are then far below the γ′ solvus. It should be noted that the matrix concentration after complete dissolution remains constant. Upon cooling to RT after final layer deposition, the nucleation rate increases again, indicating new nucleation events. The phase fraction reaches ∼40%, with a further depletion of the matrix in major γ′ forming elements.

3.3.2.2. γ′ size distribution

Fig. 8 shows histograms of the γ′ precipitate size distributions (PSD) along the build height during deposition. These PSDs are predicted at the end of each layer of interest just before final cooling to room temperature, to separate the role of thermal cycles from final cooling on the evolution of γ′. The PSD for the top layer (layer 460) is shown in Fig. 8a (last solidified region with solidification microstructure). The γ′ size ranges from 120 to 230 nm and is similar to the 44 layers below (2.2 mm from the top).

Fig. 8

Further down the build, γ′ begins to coarsen after layer 417 (44th layer from top). Fig. 8c shows the PSD after the 44th layer, where the γ′ size exhibits two peaks at ∼120–230 and ∼300 nm, with most of the population being in the former range. This is the onset of partial dissolution where simultaneously with the reprecipitation and growth of fresh γ′, the undissolved γ′ grows rapidly through diffusive transport of atoms to the precipitates. This is shown in Fig. 8c, where the precipitate class sizes between 250 and 350 represent the growth of undissolved γ′. Although this continues in the 416th layer, the phase fractions plot indicates that the onset of partial dissolution begins after the 411th layer. This implies that partial dissolution started early, but the fraction of undissolved γ′ was too low to impact the phase fraction. The reprecipitated γ′ are mostly in the 100–220 nm class range and similar to those observed during full dissolution.

As the number of layers increases, coarsening intensifies with continued growth of more undissolved γ′, and reprecipitation and growth of partially dissolved ones. Fig. 8d, e, and f show this sequence. Further down the build, coarsening progresses rapidly, as shown in Figs. 8d, 8e, and 8f. The γ′ size ranges from 120 to 1100 nm, with the peaks at 160, 180, and 220 nm in Figs. 8d, 8e, and 8f, respectively. Coarsening continues until nucleation ends during dissolution, where only the already formed γ′ precipitates continue to grow during further thermal cycling. The γ′ size at this point is much larger, as observed in layers 361 and 261, and continues to increase steadily towards the bottom (layer 1). Two populations in the ranges of ∼380–700 and ∼750–1100 nm, respectively, can be seen. The steady growth of γ′ towards the bottom is confirmed by the gradual decrease in the concentration of solute elements in the matrix (Fig. 7a). It should be noted that for each layer, the γ′ class with the largest size originates from continuous growth of the earliest set of the undissolved precipitates.

Fig. 9Fig. 10 and supplementary Figs. S2 and S3 show the γ′ size evolution during heating and cooling of a single layer in the full dissolution region, and early, middle stages, and later stages of partial dissolution, respectively. In all, the size of γ′ reduces during layer heating. Depending on the peak temperature of the layer which varies with build height, γ′ are either fully or partially dissolved as mentioned earlier. Upon cooling, the dissolved γ′ reprecipitate.

Fig. 9
Fig. 10

In Fig. 9, those layers that underwent complete dissolution (top layers) were held above γ′ solvus temperature for longer. In Fig. 10, layers at the early stage of partial dissolution spend less time in the γ′ solvus temperature region during heating, leading to incomplete dissolution. In such conditions, smaller precipitates are fully dissolved while larger ones shrink [67]. Layers in the middle stages of partial dissolution have peak temperatures just below or at γ′ solvus, not sufficient to achieve significant γ′ dissolution. As seen in supplementary Fig. S2, only a few smaller γ′ are dissolved back into the matrix during heating, i.e., growth of precipitates is more significant than dissolution. This explains the sharp decrease in concentration of Al and Ti in the matrix in this layer.

The previous sections indicate various phenomena such as an increase in phase fraction, further depletion of matrix composition, and new nucleation bursts during cooling. Analysis of the PSD after the final cooling of the build to room temperature allows a direct comparison to post-printing microstructural characterization. Fig. 11 shows the γ′ size distribution of layer 1 (460th layer from the top) after final cooling to room temperature. Precipitation of secondary γ′ is observed, leading to the multimodal size distribution of secondary and primary γ′. The secondary γ′ size falls within the 10–80 nm range. As expected, a further growth of the existing primary γ′ is also observed during cooling.

Fig. 11
3.3.2.3. γ′ chemistry after deposition

Fig. 12 shows the concentration of the major elements that form γ′ (Al, Ti, and Ni) in the primary and secondary γ′ at the bottom of the build, as calculated by MatCalc. The secondary γ′ has a higher Al content (13.5–14.5 at% Al), compared to 13 at% Al in the primary γ′. Additionally, within the secondary γ′, the smallest particles (∼10 nm) have higher Al contents than larger ones (∼70 nm). In contrast, for the primary γ′, there is no significant variation in the Al content as a function of their size. The Ni concentration in secondary γ′ (71.1–72 at%) is also higher in comparison to the primary γ′ (70 at%). The smallest secondary γ′ (∼10 nm) have higher Ni contents than larger ones (∼70 nm), whereas there is no substantial change in the Ni content of primary γ′, based on their size. As expected, Ti shows an opposite size-dependent variation. It ranges from ∼ 7.7–8.7 at% Ti in secondary γ′ to ∼9.2 at% in primary γ′. Similarly, within the secondary γ′, the smallest (∼10 nm) have lower Al contents than the larger ones (∼70 nm). No significant variation is observed for Ti content in primary γ′.

Fig. 12

4. Discussion

A combined modelling method is utilized to study the microstructural evolution during E-PBF of IN738. The presented results are discussed by examining the precipitation and dissolution mechanism of γ′ during thermal cycling. This is followed by a discussion on the phase fraction and size evolution of γ′ during thermal cycling and after final cooling. A brief discussion on carbide morphology is also made. Finally, a comparison is made between the simulation and experimental results to assess their agreement.

4.1. γ′ morphology as a function of build height

4.1.1. Nucleation of γ′

The fast precipitation kinetics of the γ′ phase enables formation of γ′ upon quenching from higher temperatures (above solvus) during thermal cycling [66]. In Fig. 7b, for a single layer in the full dissolution region, during cooling, the initial increase in nucleation rate signifies the first formation of nuclei. The slight increase in nucleation rate during partial dissolution, despite a decrease in the concentration of γ′ forming elements, may be explained by the nucleation kinetics. During partial dissolution and as the precipitates shrink, it is assumed that the regions at the vicinity of partially dissolved precipitates are enriched in γ′ forming elements [68][69]. This differs from the full dissolution region, in which case the chemical composition is evenly distributed in the matrix. Several authors have attributed the solute supersaturation of the matrix around primary γ′ to partial dissolution during isothermal ageing [69][70][71][72]. The enhanced supersaturation in the regions close to the precipitates results in a much higher driving force for nucleation, leading to a higher nucleation rate upon cooling. This phenomenon can be closely related to the several nucleation bursts upon continuous cooling of Ni-based superalloys, where second nucleation bursts exhibit higher nucleation rates [38][68][73][74].

At middle stages of partial dissolution, the reduction in the nucleation rate indicates that the existing composition and low supersaturation did not trigger nucleation as the matrix was closer to the equilibrium state. The end of a nucleation burst means that the supersaturation of Al and Ti has reached a low level, incapable of providing sufficient driving force during cooling to or holding at 1000 °C for further nucleation [73]. Earlier studies on Ni-based superalloys have reported the same phenomenon during ageing or continuous cooling from the solvus temperature to RT [38][73][74].

4.1.2. Dissolution of γ′ during thermal cycling

γ′ dissolution kinetics during heating are fast when compared to nucleation due to exponential increase in phase transformation and diffusion activities with temperature [65]. As shown in Fig. 9Fig. 10, and supplementary Figs. S2 and S3, the reduction in γ′ phase fraction and size during heating indicates γ′ dissolution. This is also revealed in Fig. 5 where phase fraction decreases upon heating. The extent of γ′ dissolution mostly depends on the temperature, time spent above γ′ solvus, and precipitate size [75][76][77]. Smaller γ′ precipitates are first to be dissolved [67][77][78]. This is mainly because more solute elements need to be transported away from large γ′ precipitates than from smaller ones [79]. Also, a high temperature above γ′ solvus temperature leads to a faster dissolution rate [80]. The equilibrium solvus temperature of γ′ in IN738 in our MatCalc simulation (Fig. 6) and as reported by Ojo et al. [47] is 1140 °C and 1130–1180 °C, respectively. This means the peak temperature experienced by previous layers decreases progressively from γ′ supersolvus to subsolvus, near-solvus, and far from solvus as the number of subsequent layers increases. Based on the above, it can be inferred that the degree of dissolution of γ′ contributes to the gradient in precipitate distribution.

Although the peak temperatures during later stages of partial dissolution are much lower than the equilibrium γ′ solvus, γ′ dissolution still occurs but at a significantly lower rate (supplementary Fig. S3). Wahlmann et al. [28] also reported a similar case where they observed the rapid dissolution of γ′ in CMSX-4 during fast heating and cooling cycles at temperatures below the γ′ solvus. They attributed this to the γ′ phase transformation process taking place in conditions far from the equilibrium. While the same reasoning may be valid for our study, we further believe that the greater surface area to volume ratio of the small γ′ precipitates contributed to this. This ratio means a larger area is available for solute atoms to diffuse into the matrix even at temperatures much below the solvus [81].

4.2. γ′ phase fraction and size evolution

4.2.1. During thermal cycling

In the first layer, the steep increase in γ′ phase fraction during heating (Fig. 5), which also represents γ′ precipitation in the powder before melting, has qualitatively been validated in [28]. The maximum phase fraction of 27% during the first few layers of thermal cycling indicates that IN738 theoretically could reach the equilibrium state (∼30%), but the short interlayer time at the build temperature counteracts this. The drop in phase fraction at middle stages of partial dissolution is due to the low number of γ′ nucleation sites [73]. It has been reported that a reduction of γ′ nucleation sites leads to a delay in obtaining the final volume fraction as more time is required for γ′ precipitates to grow and reach equilibrium [82]. This explains why even upon holding for 150 s before subsequent layer deposition, the phase fraction does not increase to those values that were observed in the previous full γ′ dissolution regions. Towards the end of deposition, the increase in phase fraction to the equilibrium value of 30% is as a result of the longer holding at build temperature or close to it [83].

During thermal cycling, γ′ particles begin to grow immediately after they first precipitate upon cooling. This is reflected in the rapid increase in phase fraction and size during cooling in Fig. 5 and supplementary Fig. S2, respectively. The rapid growth is due to the fast diffusion of solute elements at high temperatures [84]. The similar size of γ′ for the first 44 layers from the top can be attributed to the fact that all layers underwent complete dissolution and hence, experienced the same nucleation event and growth during deposition. This corresponds with the findings by Balikci et al. [85], who reported that the degree of γ′ precipitation in IN738LC does not change when a solution heat treatment is conducted above a certain critical temperature.

The increase in coarsening rate (Fig. 8) during thermal cycling can first be ascribed to the high peak temperature of the layers [86]. The coarsening rate of γ′ is known to increase rapidly with temperature due to the exponential growth of diffusion activity. Also, the simultaneous dissolution with coarsening could be another reason for the high coarsening rate, as γ′ coarsening is a diffusion-driven process where large particles grow by consuming smaller ones [78][84][86][87]. The steady growth of γ′ towards the bottom of the build is due to the much lower layer peak temperature, which is almost close to the build temperature, and reduced dissolution activity, as is seen in the much lower solute concentration in γ′ compared to those in the full and partial dissolution regions.

4.2.2. During cooling

The much higher phase fraction of ∼40% upon cooling signifies the tendency of γ′ to reach equilibrium at lower temperatures (Fig. 4). This is due to the precipitation of secondary γ′ and a further increase in the size of existing primary γ′, which leads to a multimodal size distribution of γ′ after cooling [38][73][88][89][90]. The reason for secondary γ′ formation during cooling is as follows: As cooling progresses, it becomes increasingly challenging to redistribute solute elements in the matrix owing to their lower mobility [38][73]. A higher supersaturation level in regions away from or free of the existing γ′ precipitates is achieved, making them suitable sites for additional nucleation bursts. More cooling leads to the growth of these secondary γ′ precipitates, but as the temperature and in turn, the solute diffusivity is low, growth remains slow.

4.3. Carbides

MC carbides in IN738 are known to have a significant impact on the high-temperature strength. They can also act as effective hardening particles and improve the creep resistance [91]. Precipitation of MC carbides in IN738 and several other superalloys is known to occur during solidification or thermal treatments (e.g., hot isostatic pressing) [92]. In our case, this means that the MC carbides within the E-PBF build formed because of the thermal exposure from the E-PBF thermal cycle in addition to initial solidification. Our simulation confirms this as MC carbides appear during layer heating (Fig. 5). The constant and stable phase fraction of MC carbides during thermal cycling can be attributed to their high melting point (∼1360 °C) and the short holding time at peak temperatures [75][93][94]. The solvus temperature for most MC carbides exceeds most of the peak temperatures observed in our simulation, and carbide dissolution kinetics at temperatures above the solvus are known to be comparably slow [95]. The stable phase fraction and random distribution of MC carbides signifies the slight influence on the gradient in hardness.

4.4. Comparison of simulations and experiments

4.4.1. Precipitate phase fraction and morphology as a function of build height

A qualitative agreement is observed for the phase fraction of carbides, i.e. ∼0.8% in the experiment and ∼0.9% in the simulation. The phase fraction of γ′ differs, with the experiment reporting a value of ∼51% and the simulation, 40%. Despite this, the size distribution of primary γ′ along the build shows remarkable consistency between experimental and computational analyses. It is worth noting that the primary γ′ morphology in the experimental analysis is observed in the as-fabricated state, whereas the simulation (Fig. 8) captures it during deposition process. The primary γ′ size in the experiment is expected to experience additional growth during the cooling phase. Regardless, both show similar trends in primary γ′ size increments from the top to the bottom of the build. The larger primary γ’ size in the simulation versus the experiment can be attributed to the fact that experimental and simulation results are based on 2D and 3D data, respectively. The absence of stereological considerations [96] in our analysis could have led to an underestimation of the precipitate sizes from SEM measurements. The early starts of coarsening (8th layer) in the experiment compared to the simulation (45th layer) can be attributed to a higher actual γ′ solvus temperature than considered in our simulation [47]. The solvus temperature of γ′ in a Ni-based superalloy is mainly determined by the detailed composition. A high amount of Cr and Co are known to reduce the solvus temperature, whereas Ta and Mo will increase it [97][98][99]. The elemental composition from our experimental work was used for the simulation except for Ta. It should be noted that Ta is not included in the thermodynamic database in MatCalc used, and this may have reduced the solvus temperature. This could also explain the relatively higher γ′ phase fraction in the experiment than in simulation, as a higher γ′ solvus temperature will cause more γ′ to precipitate and grow early during cooling [99][100].

Another possible cause of this deviation can be attributed to the extent of γ′ dissolution, which is mainly determined by the peak temperature. It can be speculated that individual peak temperatures at different layers in the simulation may have been over-predicted. However, one needs to consider that the true thermal profile is likely more complicated in the actual E-PBF process [101]. For example, the current model assumes that the thermophysical properties of the material are temperature-independent, which is not realistic. Many materials, including IN738, exhibit temperature-dependent properties such as thermal conductivityspecific heat capacity, and density [102]. This means that heat transfer simulations may underestimate or overestimate the temperature gradients and cooling rates within the powder bed and the solidified part. Additionally, the model does not account for the reduced thermal diffusivity through unmelted powder, where gas separating the powder acts as insulation, impeding the heat flow [1]. In E-PBF, the unmelted powder regions with trapped gas have lower thermal diffusivity compared to the fully melted regions, leading to localized temperature variations, and altered solidification behavior. These limitations can impact the predictions, particularly in relation to the carbide dissolution, as the peak temperatures may be underestimated.

While acknowledging these limitations, it is worth emphasizing that achieving a detailed and accurate representation of each layer’s heat source would impose tough computational challenges. Given the substantial layer count in E-PBF, our decision to employ a semi-analytical approximation strikes a balance between computational feasibility and the capture of essential trends in thermal profiles across diverse build layers. In future work, a dual-calibration strategy is proposed to further reduce simulation-experiment disparities. By refining temperature-independent thermophysical property approximations and absorptivity in the heat source model, and by optimizing interfacial energy descriptions in the kinetic model, the predictive precision could be enhanced. Further refining the simulation controls, such as adjusting the precipitate class size may enhance quantitative comparisons between modeling outcomes and experimental data in future work.

4.4.2. Multimodal size distribution of γ′ and concentration

Another interesting feature that sees qualitative agreement between the simulation and the experiment is the multimodal size distribution of γ′. The formation of secondary γ′ particles in the experiment and most E-PBF Ni-based superalloys is suggested to occur at low temperatures, during final cooling to RT [16][73][90]. However, so far, this conclusion has been based on findings from various continuous cooling experiments, as the study of the evolution during AM would require an in-situ approach. Our simulation unambiguously confirms this in an AM context by providing evidence for secondary γ′ precipitation during slow cooling to RT. Additionally, it is possible to speculate that the chemical segregation occurring during solidification, due to the preferential partitioning of certain elements between the solid and liquid phases, can contribute to the multimodal size distribution during deposition [51]. This is because chemical segregation can result in variations in the local composition of superalloys, which subsequently affects the nucleation and growth of γ′. Regions with higher concentrations of alloying elements will encourage the formation of larger γ′ particles, while regions with lower concentrations may favor the nucleation of smaller precipitates. However, it is important to acknowledge that the elevated temperature during the E-PBF process will largely homogenize these compositional differences [103][104].

A good correlation is also shown in the composition of major γ′ forming elements (Al and Ti) in primary and secondary γ′. Both experiment and simulation show an increasing trend for Al content and a decreasing trend for Ti content from primary to secondary γ′. The slight composition differences between primary and secondary γ′ particles are due to the different diffusivity of γ′ stabilizers at different thermal conditions [105][106]. As the formation of multimodal γ′ particles with different sizes occurs over a broad temperature range, the phase chemistry of γ′ will be highly size dependent. The changes in the chemistry of various γ′ (primary, secondary, and tertiary) have received significant attention since they have a direct influence on the performance [68][105][107][108][109]. Chen et al. [108][109], reported a high Al content in the smallest γ′ precipitates compared to the largest, while Ti showed an opposite trend during continuous cooling in a RR1000 Ni-based superalloy. This was attributed to the temperature and cooling rate at which the γ′ precipitates were formed. The smallest precipitates formed last, at the lowest temperature and cooling rate. A comparable observation is evident in the present investigation, where the secondary γ′ forms at a low temperature and cooling rate in comparison to the primary. The temperature dependence of γ′ chemical composition is further evidenced in supplementary Fig. S4, which shows the equilibrium chemical composition of γ′ as a function of temperature.

5. Conclusions

A correlative modelling approach capable of predicting solid-state phase transformations kinetics in metal AM was developed. This approach involves computational simulations with a semi-analytical heat transfer model and the MatCalc thermo-kinetic software. The method was used to predict the phase transformation kinetics and detailed morphology and chemistry of γ′ and MC during E-PBF of IN738 Ni-based superalloy. The main conclusions are:

  • 1.The computational simulations are in qualitative agreement with the experimental observations. This is particularly true for the γ′ size distribution along the build height, the multimodal size distribution of particles, and the phase fraction of MC carbides.
  • 2.The deviations between simulation and experiment in terms of γ′ phase fraction and location in the build are most likely attributed to a higher γ′ solvus temperature during the experiment than in the simulation, which is argued to be related to the absence of Ta in the MatCalc database.
  • 3.The dissolution and precipitation of γ′ occur fast and under non-equilibrium conditions. The level of γ′ dissolution determines the gradient in γ′ size distribution along the build. After thermal cycling, the final cooling to room temperature has further significant impacts on the final γ′ size, morphology, and distribution.
  • 4.A negligible amount of γ′ forms in the first deposited layer before subsequent layer deposition, and a small amount of γ′ may also form in the powder induced by the 1000 °C elevated build temperature before melting.

Our findings confirm the suitability of MatCalc to predict the microstructural evolution at various positions throughout a build in a Ni-based superalloy during E-PBF. It also showcases the suitability of a tool which was originally developed for traditional thermo-mechanical processing of alloys to the new additive manufacturing context. Our simulation capabilities are likely extendable to other alloy systems that undergo solid-state phase transformations implemented in MatCalc (various steels, Ni-based superalloys, and Al-alloys amongst others) as well as other AM processes such as L-DED and L-PBF which have different thermal cycle characteristics. New tools to predict the microstructural evolution and properties during metal AM are important as they provide new insights into the complexities of AM. This will enable control and design of AM microstructures towards advanced materials properties and performances.

CRediT authorship contribution statement

Primig Sophie: Writing – review & editing, Supervision, Resources, Project administration, Funding acquisition, Conceptualization. Adomako Nana Kwabena: Writing – original draft, Writing – review & editing, Visualization, Software, Investigation, Formal analysis, Conceptualization. Haghdadi Nima: Writing – review & editing, Supervision, Project administration, Methodology, Conceptualization. Dingle James F.L.: Methodology, Conceptualization, Software, Writing – review & editing, Visualization. Kozeschnik Ernst: Writing – review & editing, Software, Methodology. Liao Xiaozhou: Writing – review & editing, Project administration, Funding acquisition. Ringer Simon P: Writing – review & editing, Project administration, Funding acquisition.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgements

This research was sponsored by the Department of Industry, Innovation, and Science under the auspices of the AUSMURI program – which is a part of the Commonwealth’s Next Generation Technologies Fund. The authors acknowledge the facilities and the scientific and technical assistance at the Electron Microscope Unit (EMU) within the Mark Wainwright Analytical Centre (MWAC) at UNSW Sydney and Microscopy Australia. Nana Adomako is supported by a UNSW Scientia PhD scholarship. Michael Haines’ (UNSW Sydney) contribution to the revised version of the original manuscript is thankfully acknowledged.

Appendix A. Supplementary material

Download : Download Word document (462KB)

Supplementary material.

Data Availability

Data will be made available on request.

References

Figure 3. Different parts of a Searaser; 1) Buoy 2) Chamber 3) Valves 4) Generator 5) Anchor system

데이터 기반 방법을 활용한 재생 가능 에너지 변환기의 전력 및 수소 생성 예측 지속 가능한 스마트 그리드 사례 연구

Fatemehsadat Mirshafiee1, Emad Shahbazi 2, Mohadeseh Safi 3, Rituraj Rituraj 4,*
1Department of Electrical and Computer Engineering, K.N. Toosi University of Technology, Tehran 1999143344 , Iran
2Department of Mechatronic, Amirkabir University of Technology, Tehran 158754413, Iran
3Department of Mechatronic, Electrical and Computer Engineering, University of Tehran, Tehran 1416634793, Iran
4 Faculty of Informatics, Obuda University, 1023, Budapest, Hungary

  • Correspondence: rituraj88@stud.uni-obuda.hu

ABSTRACT

본 연구는 지속가능한 에너지 변환기의 전력 및 수소 발생 모델링을 위한 데이터 기반 방법론을 제안합니다. 파고와 풍속을 달리하여 파고와 수소생산을 예측합니다.

또한 이 연구는 파도에서 수소를 추출할 수 있는 가능성을 강조하고 장려합니다. FLOW-3D 소프트웨어 시뮬레이션에서 추출한 데이터와 해양 특수 테스트의 실험 데이터를 사용하여 두 가지 데이터 기반 학습 방법의 비교 분석을 수행합니다.

결과는 수소 생산의 양은 생성된 전력의 양에 비례한다는 것을 보여줍니다. 제안된 재생 에너지 변환기의 신뢰성은 지속 가능한 스마트 그리드 애플리케이션으로 추가로 논의됩니다.

This study proposes a data-driven methodology for modeling power and hydrogen generation of a sustainable energy converter. The wave and hydrogen production at different wave heights and wind speeds are predicted. Furthermore, this research emphasizes and encourages the possibility of extracting hydrogen from ocean waves. By using the extracted data from FLOW-3D software simulation and the experimental data from the special test in the ocean, the comparison analysis of two data-driven learning methods is conducted. The results show that the amount of hydrogen production is proportional to the amount of generated electrical power. The reliability of the proposed renewable energy converter is further discussed as a sustainable smart grid application.

Key words

Cavity, Combustion efficiency, hydrogen fuel, Computational Fluent and Gambit.

Figure 1. The process of power and hydrogen production with Searaser.
Figure 1. The process of power and hydrogen production with Searaser.
Figure 2. The cross-section A-A of the two essential parts of a Searaser
Figure 2. The cross-section A-A of the two essential parts of a Searaser
Figure 3. Different parts of a Searaser; 1) Buoy 2) Chamber 3) Valves 4) Generator 5) Anchor system
Figure 3. Different parts of a Searaser; 1) Buoy 2) Chamber 3) Valves 4) Generator 5) Anchor system
Figure 4. The boundary conditions of the control volume
Figure 4. The boundary conditions of the control volume
Figure 5. The wind velocity during the period of the experimental test
Figure 5. The wind velocity during the period of the experimental test

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Figure 14. Defects: (a) Unmelt defects(Scheme NO.4);(b) Pores defects(Scheme NO.1); (c); Spattering defect (Scheme NO.3); (d) Low overlapping rate defects(Scheme NO.5).

Molten pool structure, temperature and velocity
flow in selective laser melting AlCu5MnCdVA alloy

용융 풀 구조, 선택적 온도 및 속도 흐름 레이저 용융 AlCu5MnCdVA 합금

Pan Lu1 , Zhang Cheng-Lin2,6,Wang Liang3, Liu Tong4 and Liu Jiang-lin5
1 Aviation and Materials College, Anhui Technical College of Mechanical and Electrical Engineering, Wuhu Anhui 241000, People’s
Republic of China 2 School of Engineering Science, University of Science and Technology of China, Hefei Anhui 230026, People’s Republic of China 3 Anhui Top Additive Manufacturing Technology Co., Ltd., Wuhu Anhui 241300, People’s Republic of China 4 Anhui Chungu 3D Printing Institute of Intelligent Equipment and Industrial Technology, Anhui 241300, People’s Republic of China 5 School of Mechanical and Transportation Engineering, Taiyuan University of Technology, Taiyuan Shanxi 030024, People’s Republic of
China 6 Author to whom any correspondence should be addressed.
E-mail: ahjdpanlu@126.com, jiao__zg@126.com, ahjdjxx001@126.com,tongliu1988@126.com and liujianglin@tyut.edu.cn

Keywords

SLM, molten pool, AlCu5MnCdVA alloy, heat flow, velocity flow, numerical simulation

Abstract

선택적 레이저 용융(SLM)은 열 전달, 용융, 상전이, 기화 및 물질 전달을 포함하는 복잡한 동적 비평형 프로세스인 금속 적층 제조(MAM)에서 가장 유망한 기술 중 하나가 되었습니다. 용융 풀의 특성(구조, 온도 흐름 및 속도 흐름)은 SLM의 최종 성형 품질에 결정적인 영향을 미칩니다. 이 연구에서는 선택적 레이저 용융 AlCu5MnCdVA 합금의 용융 풀 구조, 온도 흐름 및 속도장을 연구하기 위해 수치 시뮬레이션과 실험을 모두 사용했습니다.

그 결과 용융풀의 구조는 다양한 형태(깊은 오목 구조, 이중 오목 구조, 평면 구조, 돌출 구조 및 이상적인 평면 구조)를 나타냈으며, 용융 풀의 크기는 약 132 μm × 107 μm × 50 μm였습니다. : 용융풀은 초기에는 여러 구동력에 의해 깊이 15μm의 깊은 오목형상이었으나, 성형 후기에는 장력구배에 의해 높이 10μm의 돌출형상이 되었다. 용융 풀 내부의 금속 흐름은 주로 레이저 충격력, 금속 액체 중력, 표면 장력 및 반동 압력에 의해 구동되었습니다.

AlCu5MnCdVA 합금의 경우, 금속 액체 응고 속도가 매우 빠르며(3.5 × 10-4 S), 가열 속도 및 냉각 속도는 각각 6.5 × 107 K S-1 및 1.6 × 106 K S-1 에 도달했습니다. 시각적 표준으로 표면 거칠기를 선택하고, 낮은 레이저 에너지 AlCu5MnCdVA 합금 최적 공정 매개변수 창을 수치 시뮬레이션으로 얻었습니다: 레이저 출력 250W, 부화 공간 0.11mm, 층 두께 0.03mm, 레이저 스캔 속도 1.5m s-1 .

또한, 실험 프린팅과 수치 시뮬레이션과 비교할 때, 용융 풀의 폭은 각각 약 205um 및 약 210um이었고, 인접한 두 용융 트랙 사이의 중첩은 모두 약 65um이었다. 결과는 수치 시뮬레이션 결과가 실험 인쇄 결과와 기본적으로 일치함을 보여 수치 시뮬레이션 모델의 정확성을 입증했습니다.

Selective Laser Melting (SLM) has become one of the most promising technologies in Metal Additive Manufacturing (MAM), which is a complex dynamic non-equilibrium process involving heat transfer, melting, phase transition, vaporization and mass transfer. The characteristics of the molten pool (structure, temperature flow and velocity flow) have a decisive influence on the final forming quality of SLM. In this study, both numerical simulation and experiments were employed to study molten pool structure, temperature flow and velocity field in Selective Laser Melting AlCu5MnCdVA alloy. The results showed the structure of molten pool showed different forms(deep-concave structure, double-concave structure, plane structure, protruding structure and ideal planar structure), and the size of the molten pool was approximately 132 μm × 107 μm × 50 μm: in the early stage, molten pool was in a state of deep-concave shape with a depth of 15 μm due to multiple driving forces, while a protruding shape with a height of 10 μm duo to tension gradient in the later stages of forming. The metal flow inside the molten pool was mainly driven by laser impact force, metal liquid gravity, surface tension and recoil pressure. For AlCu5MnCdVA alloy, metal liquid solidification speed was extremely fast(3.5 × 10−4 S), the heating rate and cooling rate reached 6.5 × 107 K S−1 and 1.6 × 106 K S−1 , respectively. Choosing surface roughness as a visual standard, low-laser energy AlCu5MnCdVA alloy optimum process parameters window was obtained by numerical simulation: laser power 250 W, hatching space 0.11 mm, layer thickness 0.03 mm, laser scanning velocity 1.5 m s−1 . In addition, compared with experimental printing and numerical simulation, the width of the molten pool was about 205 um and about 210 um, respectively, and overlapping between two adjacent molten tracks was all about 65 um. The results showed that the numerical simulation results were basically consistent with the experimental print results, which proved the correctness of the numerical simulation model.

Figure 1. AlCu5MnCdVA powder particle size distribution.
Figure 1. AlCu5MnCdVA powder particle size distribution.
Figure 2. AlCu5MnCdVA powder
Figure 2. AlCu5MnCdVA powder
Figure 3. Finite element model and calculation domains of SLM.
Figure 3. Finite element model and calculation domains of SLM.
Figure 4. SLM heat transfer process.
Figure 4. SLM heat transfer process.
Figure 14. Defects: (a) Unmelt defects(Scheme NO.4);(b) Pores defects(Scheme NO.1); (c); Spattering defect (Scheme NO.3); (d) Low
overlapping rate defects(Scheme NO.5).
Figure 17. Two-pass molten tracks overlapping for Scheme NO.2.
Figure 17. Two-pass molten tracks overlapping for Scheme NO.2.

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[2] Zhanfei Z 2017 Study on theta phase segregation and room temperature properties of high strength cast Al–Cu–Mn alloy Lanzhou University of Technology
[3] Nie X et al 2018 Analysis of processing parameters and characteristics of selective laser melted high strength Al–Cu–Mg alloys: from single tracks to cubic samplesJ. Mater. Process. Technol. 256 69–77
[4] Shenping Y et al 2017 Laser absorptance measurement of commonly used metal materials in laser additive manufacturing technology Aviation Manufacturing Technology 12 23–9
[5] Wenqing W 2007 Relationship between cooling rate and grain size of AlCu5MnCdVA alloy Harbin University of Technology
[6] Majeed M, Vural M, Raja S and Bilal Naim Shaikh M 2019 Finite element analysis of thermal behavior in maraging steel during SLM process Optik 208 113–24
[7] Khairallah S A, Anderson A T, Rubenchik A and King W E 2016 Laser powder-bed fusion additive manufacturing: physics of complex melt flow and formation mechanisms of pores, spatter, and denudation zones Acta Mater. 108 36–45
[8] Bo C, Zhiyu X, Quanquan Z, Yuanbiao W, Liping W and Jin C 2020 Process optimization and microstructure and properties of SLM forming Cu6AlNiSnInCe imitation gold alloy Chin. J. Nonferr. Met. 30 372–82
[9] Li W 2012 Research on performance of metal parts formed by selective laser melting Huazhong University of Science and Technology
[10] Yu Q 2013 The influence of different laser heat sources on the surface shape of the molten pool in laser cladding Surf. Technol. 42 40–3

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in SLM processing Applied Laser 35 155–9
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[19] Genwang W 2017 Research on the establishment of laser heat source model based on energy distribution and its simulation application
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Figure 1: Mold drawings

3D Flow and Temperature Analysis of Filling a Plutonium Mold

플루토늄 주형 충전의 3D 유동 및 온도 분석

Authors: Orenstein, Nicholas P. [1]

Publication Date:2013-07-24
Research Org.: Los Alamos National Lab. (LANL), Los Alamos, NM (United States)
Sponsoring Org.: DOE/LANL
OSTI Identifier: 1088904
Report Number(s): LA-UR-13-25537
DOE Contract Number: AC52-06NA25396
Resource Type: Technical Report
Country of Publication: United States
Language: English
Subject: Engineering(42); Materials Science(36); Radiation Chemistry, Radiochemistry, & Nuclear Chemistry(38)

Introduction

The plutonium foundry at Los Alamos National Laboratory casts products for various special nuclear applications. However, plutonium’s radioactivity, material properties, and security constraints complicate the ability to perform experimental analysis of mold behavior. The Manufacturing Engineering and Technologies (MET-2) group previously developed a graphite mold to vacuum cast small plutonium disks to be used by the Department of Homeland Security as point sources for radiation sensor testing.

A two-stage pouring basin consisting of a funnel and an angled cavity directs the liquid into a vertical runner. A stack of ten disk castings connect to the runner by horizontal gates. Volumetric flow rates were implemented to limit overflow into the funnel and minimize foundry returns. Models using Flow-3D computational fluid dynamics software are employed here to determine liquid Pu flow paths, optimal pour regimes, temperature changes, and pressure variations.

Setup

Hardcopy drawings provided necessary information to create 3D .stl models for import into Flow-3D (Figs. 1 and 2). The mesh was refined over several iterations to isolate the disk cavities, runner, angled cavity, funnel, and input pour. The final flow and mold-filling simulation utilizes a fine mesh with ~5.5 million total cells. For the temperature study, the mesh contained 1/8 as many cells to reduce computational time and set temperatures to 850 °C for the molten plutonium and 500 °C for the solid graphite mold components (Fig. 3).

Flow-3D solves mass continuity and Navier-Stokes momentum equations over the structured rectangular grid model using finite difference and finite volume numerical algorithms. The solver includes terms in the momentum equation for body and viscous accelerations and uses convective heat transfer.

Simulation settings enabled Flow-3D physics calculations for gravity at 980.665 cm/s 2 in the negative Z direction (top of mold to bottom); viscous, turbulent, incompressible flow using dynamically-computed Renormalized Group Model turbulence calculations and no-slip/partial slip wall shear, and; first order, full energy equation heat transfer.

Mesh boundaries were all set to symmetric boundary conditions except for the Zmin boundary set to outflow and the Zmax boundary set to a volume flow. Vacuum casting conditions and the high reactivity of remaining air molecules with Pu validate the assumption of an initially fluidless void.

Results

The flow follows a unique three-dimensional path. The mold fills upwards with two to three disks receiving fluid in a staggered sequence. Figures 5-9 show how the fluid fills the cavity, and Figure 7 includes the color scale for pressure levels in these four figures. The narrow gate causes a high pressure region which forces the fluid to flow down the cavity centerline.

It proceeds to splash against the far wall and then wrap around the circumference back to the gate (Figs. 5 and 6). Flow in the angled region of the pouring basin cascades over the bottom ledge and attaches to the far wall of the runner, as seen in Figure 7.

This channeling becomes less pronounced as fluid volume levels increase. Finally, two similar but non-uniform depressed regions form about the centerline. These regions fill from their perimeter and bottom until completion (Fig. 8). Such a pattern is counter, for example, to a steady scenario in which a circle of molten Pu encompassing the entire bottom surface rises as a growing cylinder.

Cavity pressure becomes uniform when the cavity is full. Pressure levels build in the rising well section of the runner, where impurities were found to settle in actual casting. Early test simulations optimized the flow as three pours so that the fluid would never overflow to the funnel, the cavities would all fill completely, and small amounts of fluid would remain as foundry returns in the angled cavity.

These rates and durations were translated to the single 2.7s pour at 100 cm 3 per second used here. Figure 9 shows anomalous pressure fluctuations which occurred as the cavities became completely filled. Multiple simulations exhibited a rapid change in pressure from positive to negative and back within the newly-full disk and surrounding, already-full disks.

The time required to completely fill each cavity is plotted in Figure 10. Results show negligible temperature change within the molten Pu during mold filling and, as seen in Figure 11, at fill completion.

Figure 1: Mold drawings
Figure 1: Mold drawings
Figure 2: Mold Assembly
Figure 2: Mold Assembly
Figure 4: Actual mold and cast Pu
Figure 4: Actual mold and cast Pu
Figure 5: Bottom cavity filling
from runner
Figure 5: Bottom cavity filling from runner
Figure 6: Pouring and filling
Figure 6: Pouring and filling
Figure 8: Edge detection of cavity fill geometry. Two similar depressed areas form
about the centerline. Top cavity shown; same pressure scale as other figures
Figure 8: Edge detection of cavity fill geometry. Two similar depressed areas form about the centerline. Top cavity shown; same pressure scale as other figures
Figure 10: Cavity fill times,from first fluid contact with pouring basin, Figure 11:Fluid temperature remains essentially constant
Figure 10: Cavity fill times,from first fluid contact with pouring basin, Figure 11:Fluid temperature remains essentially constant

Conclusions

Non-uniform cavity filling could cause crystal microstructure irregularities during solidification. However, the small temperature changes seen – due to large differences in specific heat between Pu and graphite – over a relatively short time make such problems unlikely in this case.

In the actual casting, cooling required approximately ten minutes. This large difference in time scales further reduces the chance for temperature effects in such a superheated scenario. Pouring basin emptying decreases pressure at the gate which extends fill time of the top two cavities.

The bottom cavity takes longer to fill because fluid must first enter the runner and fill the well. Fill times continue linearly until the top two cavities. The anomalous pressure fluctuations may be due to physical attempts by the system to reach equilibrium, but they are more likely due to numerical errors in the Flow3D solver.

Unsuccessful tests were performed to remove them by halving fluid viscosity. The fine mesh reduced, but did not eliminate, the extent of the fluctuations. Future work is planned to study induction and heat transfer in the full Pu furnace system, including quantifying temporal lag of the cavity void temperature to the mold wall temperature during pre-heat and comparing heat flux levels between furnace components during cool-down.

Thanks to Doug Kautz for the opportunity to work with MET-2 and for assigning an interesting unclassified project. Additional thanks to Mike Bange for CFD guidance, insight of the project’s history, and draft review.

Development of macro-defect-free PBF-EB-processed Ti–6Al–4V alloys with superior plasticity using PREP-synthesized powder and machine learning-assisted process optimization

Development of macro-defect-free PBF-EB-processed Ti–6Al–4V alloys with superior plasticity using PREP-synthesized powder and machine learning-assisted process optimization

Yunwei GuiabKenta Aoyagib Akihiko Chibab
aDepartment of Materials Processing, Graduate School of Engineering, Tohoku University, 6-6 Aramaki Aza Aoba, Aoba-ku, Sendai, 980-8579, Japan
bInstitute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, 980-8577, Japan

Received 14 October 2022, Revised 23 December 2022, Accepted 3 January 2023, Available online 5 January 2023.Show lessAdd to MendeleyShareCite

https://doi.org/10.1016/j.msea.2023.144595Get rights and content

Abstract

The elimination of internal macro-defects is a key issue in Ti–6Al–4V alloys fabricated via powder bed fusion using electron beams (PBF-EB), wherein internal macro-defects mainly originate from the virgin powder and inappropriate printing parameters. This study compares different types powders by combining support vector machine techniques to determine the most suitable powder for PBF-EB and to predict the processing window for the printing parameters without internal macro-defects. The results show that powders fabricated via plasma rotating electrode process have the best sphericity, flowability, and minimal porosity and are most suitable for printing. Surface roughness criterion was also applied to determine the quality of the even surfaces, and support vector machine was used to construct processing maps capable of predicting a wide range of four-dimensional printing parameters to obtain macro-defect-free samples, offering the possibility of subsequent development of Ti–6Al–4V alloys with excellent properties. The macro-defect-free samples exhibited good elongation, with the best overall mechanical properties being the ultimate tensile strength and elongation of 934.7 MPa and 24.3%, respectively. The elongation of the three macro-defect-free samples was much higher than that previously reported for additively manufactured Ti–6Al–4V alloys. The high elongation of the samples in this work is mainly attributed to the elimination of internal macro-defects.

Introduction

Additive manufacturing (AM) technologies can rapidly manufacture complex or custom parts, reducing process steps and saving manufacturing time [[1], [2], [3], [4]], and are widely used in the aerospace, automotive, and other precision industries [5,6]. Powder bed fusion using an electron beam (PBF-EB) is an additive manufacturing method that uses a high-energy electron beam to melt metal powders layer by layer to produce parts. In contrast to selective laser melting, PBF-EB involves the preparation of samples in a high vacuum environment, which effectively prevents the introduction of impurities such as O and N. It also involves a preheating process for the print substrate and powder, which reduces residual thermal stress on the sample and subsequent heat treatment processes [[2], [3], [4],7]. Due to these features and advantages, PBF-EB technology is a very important AM technology with great potential in metallic materials. Moreover, PBF-EB is the ideal AM technology for the manufacture of complex components made of many alloys, such as titanium alloys, nickel-based superalloys, aluminum alloys and stainless steels [[2], [3], [4],8].

Ti–6Al–4V alloy is one of the prevalent commercial titanium alloys possessing high specific strength, excellent mechanical properties, excellent corrosion resistance, and good biocompatibility [9,10]. It is widely used in applications requiring low density and excellent corrosion resistance, such as the aerospace industry and biomechanical applications [11,12]. The mechanical properties of PBF-EB-processed Ti–6Al–4V alloys are superior to those fabricated by casting or forging, because the rapid cooling rate in PBF-EB results in finer grains [[12], [13], [14], [15], [16], [17], [18]]. However, the PBF-EB-fabricated parts often include internal macro-defects, which compromises their mechanical properties [[19], [20], [21], [22]]. This study focused on the elimination of macro-defects, such as porosity, lack of fusion, incomplete penetration and unmelted powders, which distinguishes them from micro-defects such as vacancies, dislocations, grain boundaries and secondary phases, etc. Large-sized fusion defects cause a severe reduction in mechanical strength. Smaller defects, such as pores and cracks, lead to the initiation of fatigue cracking and rapidly accelerate the cracking process [23]. The issue of internal macro-defects must be addressed to expand the application of the PBF-EB technology. The main studies for controlling internal macro-defects are online monitoring of defects, remelting and hot isostatic pressing (HIP). The literatures [24,25] report the use of infrared imaging or other imaging techniques to identify defects, but the monitoring of smaller sized defects is still not adequate. And in some cases remelting does not reduce the internal macro-defects of the part, but instead causes coarsening of the macrostructure and volatilization of some metal elements [23]. The HIP treatment does not completely eliminate the internal macro-defects, the original defect location may still act as a point of origin of the crack, and the subsequent treatment will consume more time and economic costs [23]. Therefore, optimizing suitable printing parameters to avoid internal macro-defects in printed parts at source is of great industrial value and research significance, and is an urgent issue in PBF-EB related technology.

There are two causes of internal macro-defects in the AM process: gas pores trapped in the virgin powder and the inappropriate printing parameters [7,23]. Gui et al. [26] classify internal macro-defects during PBF-EB process according to their shape, such as spherical defects, elongated shape defects, flat shape defects and other irregular shape defects. Of these, spherical defects mainly originate from raw material powders. Other shape defects mainly originate from lack of fusion or unmelted powders caused by unsuitable printing parameters, etc. The PBF-EB process requires powders with good flowability, and spherical powders are typically chosen as raw materials. The prevalent techniques for the fabrication of pre-alloyed powders are gas atomization (GA), plasma atomization (PA), and the plasma rotating electrode process (PREP) [27,28]. These methods yield powders with different characteristics that affect the subsequent fabrication. The selection of a suitable powder for PBF-EB is particularly important to produce Ti–6Al–4V alloys without internal macro-defects. The need to optimize several printing parameters such as beam current, scan speed, line offset, and focus offset make it difficult to eliminate internal macro-defects that occur during printing [23]. Most of the studies [11,12,22,[29], [30], [31], [32], [33]] on the optimization of AM processes for Ti–6Al–4V alloys have focused on samples with a limited set of parameters (e.g., power–scan speed) and do not allow for the guidance and development of unknown process windows for macro-defect-free samples. In addition, process optimization remains a time-consuming problem, with the traditional ‘trial and error’ method demanding considerable time and economic costs. The development of a simple and efficient method to predict the processing window for alloys without internal macro-defects is a key issue. In recent years, machine learning techniques have increasingly been used in the field of additive manufacturing and materials development [[34], [35], [36], [37]]. Aoyagi et al. [38] recently proposed a novel and efficient method based on a support vector machine (SVM) to optimize the two-dimensional process parameters (current and scan speed) and obtain PBF-EB-processed CoCr alloys without internal macro-defects. The method is one of the potential approaches toward effective optimization of more than two process parameters and makes it possible for the machine learning techniques to accelerate the development of alloys without internal macro-defects.

Herein, we focus on the elimination of internal macro-defects, such as pores, lack of fusion, etc., caused by raw powders and printing parameters. The Ti–6Al–4V powders produced by three different methods were compared, and the powder with the best sphericity, flowability, and minimal porosity was selected as the feedstock for subsequent printing. The relationship between the surface roughness and internal macro-defects in the Ti–6Al–4V components was also investigated. The combination of SVM and surface roughness indices (Sdr) predicted a wider four-dimensional processing window for obtaining Ti–6Al–4V alloys without internal macro-defects. Finally, we investigated the tensile properties of Ti–6Al–4V alloys at room temperature with different printing parameters, as well as the corresponding microstructures and fracture types.

Section snippets

Starting materials

Three types of Ti–6Al–4V alloy powders, produced by GA, PA, and PREP, were compared. The particle size distribution of the powders was determined using a laser particle size analyzer (LS230, Beckman Coulter, USA), and the flowability was measured using a Hall flowmeter (JIS-Z2502, Tsutsui Scientific Instruments Co., Ltd., Japan), according to the ASTM B213 standard. The powder morphology and internal macro-defects were determined using scanning electron microscopy (SEM, JEOL JCM-6000) and X-ray 

Comparison of the characteristics of GA, PA, and PREP Ti–6Al–4V powders

The particle size distributions (PSDs) and flowability of the three types of Ti–6Al–4V alloy powders produced by GA, PA, and PREP are shown in Fig. 2. Although the average particle sizes are similar (89.4 μm for GA, 82.5 μm for PA, and 86.1μm for PREP), the particle size range is different for the three types of powder (6.2–174.8 μm for GA, 27.3–139.2 μm for PA, and 39.4–133.9 μm for PREP). The flowability of the GA, PA, and PREP powders was 30.25 ± 0.98, 26.54 ± 0.37, and 25.03 ± 0.22 (s/50

Conclusions

The characteristics of the three types of Ti–6Al–4V alloy powders produced via GA, PA, and PREP were compared. The PREP powder with the best sphericity, flowability, and low porosity was found to be the most favorable powder for subsequent printing of Ti–6Al–4V alloys without internal macro-defects. The quantitative criterion of Sdr <0.015 for even surfaces was also found to be applicable to Ti–6Al–4V alloys. The process maps of Ti–6Al–4V alloys include two regions, high beam current/scan speed 

Uncited references

[55]; [56]; [57]; [58]; [59]; [60]; [61]; [62]; [63]; [64]; [65].

CRediT authorship contribution statement

Yunwei Gui: Writing – original draft, Visualization, Validation, Investigation. Kenta Aoyagi: Writing – review & editing, Supervision, Resources, Methodology, Funding acquisition, Conceptualization. Akihiko Chiba: Supervision, Funding acquisition.

Declaration of competing interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgments

This study was based on the results obtained from project JPNP19007, commissioned by the New Energy and Industrial Technology Development Organization (NEDO). This work was also supported by JSPS KAKENHI (Proposal No. 21K03801) and the Inter-University Cooperative Research Program (Proposal nos. 18G0418, 19G0411, and 20G0418) of the Cooperative Research and Development Center for Advanced Materials, Institute for Materials Research, Tohoku University. It was also supported by the Council for

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Fig. 1. (a) Dimensions of the casting with runners (unit: mm), (b) a melt flow simulation using Flow-3D software together with Reilly's model[44], predicted that a large amount of bifilms (denoted by the black particles) would be contained in the final casting. (c) A solidification simulation using Pro-cast software showed that no shrinkage defect was contained in the final casting.

AZ91 합금 주물 내 연행 결함에 대한 캐리어 가스의 영향

TianLiabJ.M.T.DaviesaXiangzhenZhuc
aUniversity of Birmingham, Birmingham B15 2TT, United Kingdom
bGrainger and Worrall Ltd, Bridgnorth WV15 5HP, United Kingdom
cBrunel Centre for Advanced Solidification Technology, Brunel University London, Kingston Ln, London, Uxbridge UB8 3PH, United Kingdom

Abstract

An entrainment defect (also known as a double oxide film defect or bifilm) acts a void containing an entrapped gas when submerged into a light-alloy melt, thus reducing the quality and reproducibility of the final castings. Previous publications, carried out with Al-alloy castings, reported that this trapped gas could be subsequently consumed by the reaction with the surrounding melt, thus reducing the void volume and negative effect of entrainment defects. Compared with Al-alloys, the entrapped gas within Mg-alloy might be more efficiently consumed due to the relatively high reactivity of magnesium. However, research into the entrainment defects within Mg alloys has been significantly limited. In the present work, AZ91 alloy castings were produced under different carrier gas atmospheres (i.e., SF6/CO2, SF6/air). The evolution processes of the entrainment defects contained in AZ91 alloy were suggested according to the microstructure inspections and thermodynamic calculations. The defects formed in the different atmospheres have a similar sandwich-like structure, but their oxide films contained different combinations of compounds. The use of carrier gases, which were associated with different entrained-gas consumption rates, affected the reproducibility of AZ91 castings.

연행 결함(이중 산화막 결함 또는 이중막이라고도 함)은 경합금 용융물에 잠길 때 갇힌 가스를 포함하는 공극으로 작용하여 최종 주물의 품질과 재현성을 저하시킵니다. Al-합금 주물을 사용하여 수행된 이전 간행물에서는 이 갇힌 가스가 주변 용융물과의 반응에 의해 후속적으로 소모되어 공극 부피와 연행 결함의 부정적인 영향을 줄일 수 있다고 보고했습니다. Al-합금에 비해 마그네슘의 상대적으로 높은 반응성으로 인해 Mg-합금 내에 포집된 가스가 더 효율적으로 소모될 수 있습니다. 그러나 Mg 합금 내 연행 결함에 대한 연구는 상당히 제한적이었습니다. 현재 작업에서 AZ91 합금 주물은 다양한 캐리어 가스 분위기(즉, SF6/CO2, SF6/공기)에서 생산되었습니다. AZ91 합금에 포함된 연행 결함의 진화 과정은 미세 조직 검사 및 열역학 계산에 따라 제안되었습니다. 서로 다른 분위기에서 형성된 결함은 유사한 샌드위치 구조를 갖지만 산화막에는 서로 다른 화합물 조합이 포함되어 있습니다. 다른 동반 가스 소비율과 관련된 운반 가스의 사용은 AZ91 주물의 재현성에 영향을 미쳤습니다.

Keywords

Magnesium alloy, Casting, Oxide film, Bifilm, Entrainment defect, Reproducibility

1. Introduction

As the lightest structural metal available on Earth, magnesium became one of the most attractive light metals over the last few decades. The magnesium industry has consequently experienced a rapid development in the last 20 years [1,2], indicating a large growth in demand for Mg alloys all over the world. Nowadays, the use of Mg alloys can be found in the fields of automobiles, aerospace, electronics and etc.[3,4]. It has been predicted that the global consumption of Mg metals will further increase in the future, especially in the automotive industry, as the energy efficiency requirement of both traditional and electric vehicles further push manufactures lightweight their design [3,5,6].

The sustained growth in demand for Mg alloys motivated a wide interest in the improvement of the quality and mechanical properties of Mg-alloy castings. During a Mg-alloy casting process, surface turbulence of the melt can lead to the entrapment of a doubled-over surface film containing a small quantity of the surrounding atmosphere, thus forming an entrainment defect (also known as a double oxide film defect or bifilm) [7][8][9][10]. The random size, quantity, orientation, and placement of entrainment defects are widely accepted to be significant factors linked to the variation of casting properties [7]. In addition, Peng et al. [11] found that entrained oxides films in AZ91 alloy melt acted as filters to Al8Mn5 particles, trapping them as they settle. Mackie et al. [12] further suggested that entrained oxide films can act to trawl the intermetallic particles, causing them to cluster and form extremely large defects. The clustering of intermetallic compounds made the entrainment defects more detrimental for the casting properties.

Most of the previous studies regarding entrainment defects were carried out on Al-alloys [7,[13][14][15][16][17][18], and a few potential methods have been suggested for diminishing their negative effect on the quality of Al-alloy castings. Nyahumwa et al.,[16] shows that the void volume within entrainment defects could be reduced by a hot isostatic pressing (HIP) process. Campbell [7] suggested the entrained gas within the defects could be consumed due to reaction with the surrounding melt, which was further verified by Raiszedeh and Griffiths [19].The effect of the entrained gas consumption on the mechanical properties of Al-alloy castings has been investigated by [8,9], suggesting that the consumption of the entrained gas promoted the improvement of the casting reproducibility.

Compared with the investigation concerning the defects within Al-alloys, research into the entrainment defects within Mg-alloys has been significantly limited. The existence of entrainment defects has been demonstrated in Mg-alloy castings [20,21], but their behaviour, evolution, as well as entrained gas consumption are still not clear.

In a Mg-alloy casting process, the melt is usually protected by a cover gas to avoid magnesium ignition. The cavities of sand or investment moulds are accordingly required to be flushed with the cover gas prior to the melt pouring [22]. Therefore, the entrained gas within Mg-alloy castings should contain the cover gas used in the casting process, rather than air only, which may complicate the structure and evolution of the corresponding entrainment defects.

SF6 is a typical cover gas widely used for Mg-alloy casting processes [23][24][25]. Although this cover gas has been restricted to use in European Mg-alloy foundries, a commercial report has pointed out that this cover is still popular in global Mg-alloy industry, especially in the countries which dominated the global Mg-alloy production, such as China, Brazil, India, etc. [26]. In addition, a survey in academic publications also showed that this cover gas was widely used in recent Mg-alloy studies [27]. The protective mechanism of SF6 cover gas (i.e., the reaction between liquid Mg-alloy and SF6 cover gas) has been investigated by several previous researchers, but the formation process of the surface oxide film is still not clearly understood, and even some published results are conflicting with each other. In early 1970s, Fruehling [28] found that the surface film formed under SF6 was MgO mainly with traces of fluorides, and suggested that SF6 was absorbed in the Mg-alloy surface film. Couling [29] further noticed that the absorbed SF6 reacted with the Mg-alloy melt to form MgF2. In last 20 years, different structures of the Mg-alloy surface films have been reported, as detailed below.(1)

Single-layered film. Cashion [30,31] used X-ray Photoelectron Spectroscopy (XPS) and Auger Spectroscopy (AES) to identify the surface film as MgO and MgF2. He also found that composition of the film was constant throughout the thickness and the whole experimental holding time. The film observed by Cashion had a single-layered structure created from a holding time from 10 min to 100 min.(2)

Double-layered film. Aarstad et. al [32] reported a doubled-layered surface oxide film in 2003. They observed several well-distributed MgF2 particles attached to the preliminary MgO film and grew until they covered 25–50% of the total surface area. The inward diffusion of F through the outer MgO film was the driving force for the evolution process. This double-layered structure was also supported by Xiong’s group [25,33] and Shih et al. [34].(3)

Triple-layered film. The triple-layered film and its evolution process were reported in 2002 by Pettersen [35]. Pettersen found that the initial surface film was a MgO phase and then gradually evolved to the stable MgF2 phase by the inward diffusion of F. In the final stage, the film has a triple-layered structure with a thin O-rich interlayer between the thick top and bottom MgF2 layers.(4)

Oxide film consisted of discrete particles. Wang et al [36] stirred the Mg-alloy surface film into the melt under a SF6 cover gas, and then inspect the entrained surface film after the solidification. They found that the entrained surface films were not continues as the protective surface films reported by other researchers but composed of discrete particles. The young oxide film was composed of MgO nano-sized oxide particles, while the old oxide films consist of coarse particles (about 1  µm in average size) on one side that contained fluorides and nitrides.

The oxide films of a Mg-alloy melt surface or an entrained gas are both formed due to the reaction between liquid Mg-alloy and the cover gas, thus the above-mentioned research regarding the Mg-alloy surface film gives valuable insights into the evolution of entrainment defects. The protective mechanism of SF6 cover gas (i.e., formation of a Mg-alloy surface film) therefore indicated a potential complicated evolution process of the corresponding entrainment defects.

However, it should be noted that the formation of a surface film on a Mg-alloy melt is in a different situation to the consumption of an entrained gas that is submerged into the melt. For example, a sufficient amount of cover gas was supported during the surface film formation in the studies previously mentioned, which suppressed the depletion of the cover gas. In contrast, the amount of entrained gas within a Mg-alloy melt is finite, and the entrained gas may become fully depleted. Mirak [37] introduced 3.5%SF6/air bubbles into a pure Mg-alloy melt solidifying in a specially designed permanent mould. It was found that the gas bubbles were entirely consumed, and the corresponding oxide film was a mixture of MgO and MgF2. However, the nucleation sites (such as the MgF2 spots observed by Aarstad [32] and Xiong [25,33]) were not observed. Mirak also speculated that the MgF2 formed prior to MgO in the oxide film based on the composition analysis, which was opposite to the surface film formation process reported in previous literatures (i.e., MgO formed prior to MgF2). Mirak’s work indicated that the oxide-film formation of an entrained gas may be quite different from that of surface films, but he did not reveal the structure and evolution of the oxide films.

In addition, the use of carrier gas in the cover gases also influenced the reaction between the cover gas and the liquid Mg-alloy. SF6/air required a higher content of SF6 than did a SF6/CO2 carrier gas [38], to avoid the ignition of molten magnesium, revealing different gas-consumption rates. Liang et.al [39] suggested that carbon was formed in the surface film when CO2 was used as a carrier gas, which was different from the films formed in SF6/air. An investigation into Mg combustion [40] reported a detection of Mg2C3 in the Mg-alloy sample after burning in CO2, which not only supported Liang’s results, but also indicated a potential formation of Mg carbides in double oxide film defects.

The work reported here is an investigation into the behaviour and evolution of entrainment defects formed in AZ91 Mg-alloy castings, protected by different cover gases (i.e., SF6/air and SF6/CO2). These carrier gases have different protectability for liquid Mg alloy, which may be therefore associated with different consumption rates and evolution processes of the corresponding entrained gases. The effect of the entrained-gas consumption on the reproducibility of AZ91 castings was also studied.

2. Experiment

2.1. Melting and casting

Three kilograms AZ91 alloy was melted in a mild steel crucible at 700 ± 5 °C. The composition of the AZ91 alloy has been shown in Table 1. Prior to heating, all oxide scale on the ingot surface was removed by machining. The cover gases used were 0.5%SF6/air or 0.5%SF6/CO2 (vol.%) at a flow rate of 6 L/min for different castings. The melt was degassed by argon with a flow rate of 0.3 L/min for 15 min [41,42], and then poured into sand moulds. Prior to pouring, the sand mould cavity was flushed with the cover gas for 20 min [22]. The residual melt (around 1 kg) was solidified in the crucible.

Table 1. Composition (wt.%) of the AZ91 alloy used in this study.

AlZnMnSiFeNiMg
9.40.610.150.020.0050.0017Residual

Fig. 1(a) shows the dimensions of the casting with runners. A top-filling system was deliberately used to generate entrainment defects in the final castings. Green and Campbell [7,43] suggested that a top-filling system caused more entrainment events (i.e., bifilms) during a casting process, compared with a bottom-filling system. A melt flow simulation (Flow-3D software) of this mould, using Reilly’s model [44] regarding the entrainment events, also predicted that a large amount of bifilms would be contained in the final casting (denoted by the black particles in Fig. 1b).

Fig. 1. (a) Dimensions of the casting with runners (unit: mm), (b) a melt flow simulation using Flow-3D software together with Reilly's model[44], predicted that a large amount of bifilms (denoted by the black particles) would be contained in the final casting. (c) A solidification simulation using Pro-cast software showed that no shrinkage defect was contained in the final casting.

Shrinkage defects also affect the mechanical properties and reproducibility of castings. Since this study focused on the effect of bifilms on the casting quality, the mould has been deliberately designed to avoid generating shrinkage defects. A solidification simulation using ProCAST software showed that no shrinkage defect would be contained in the final casting, as shown in Fig. 1c. The casting soundness has also been confirmed using a real time X-ray prior to the test bar machining.

The sand moulds were made from resin-bonded silica sand, containing 1wt. % PEPSET 5230 resin and 1wt. % PEPSET 5112 catalyst. The sand also contained 2 wt.% Na2SiF6 to act as an inhibitor [45]. The pouring temperature was 700 ± 5 °C. After the solidification, a section of the runner bars was sent to the Sci-Lab Analytical Ltd for a H-content analysis (LECO analysis), and all the H-content measurements were carried out on the 5th day after the casting process. Each of the castings was machined into 40 test bars for a tensile strength test, using a Zwick 1484 tensile test machine with a clip extensometer. The fracture surfaces of the broken test bars were examined using Scanning Electron Microscope (SEM, Philips JEOL7000) with an accelerating voltage of 5–15 kV. The fractured test bars, residual Mg-alloy solidified in the crucible, and the casting runners were then sectioned, polished and also inspected using the same SEM. The cross-section of the oxide film found on the test-bar fracture surface was exposed by the Focused Ion Beam milling technique (FIB), using a CFEI Quanta 3D FEG FIB-SEM. The oxide film required to be analysed was coated with a platinum layer. Then, a gallium ion beam, accelerated to 30 kV, milled the material substrate surrounding the platinum coated area to expose the cross section of the oxide film. EDS analysis of the oxide film’s cross section was carried out using the FIB equipment at accelerating voltage of 30 kV.

2.2. Oxidation cell

As previously mentioned, several past researchers investigated the protective film formed on a Mg-alloy melt surface [38,39,[46][47][48][49][50][51][52]. During these experiments, the amount of cover gas used was sufficient, thus suppressing the depletion of fluorides in the cover gas. The experiment described in this section used a sealed oxidation cell, which limited the supply of cover gas, to study the evolution of the oxide films of entrainment defects. The cover gas contained in the oxidation cell was regarded as large-size “entrained bubble”.

As shown in Fig. 2, the main body of the oxidation cell was a closed-end mild steel tube which had an inner length of 400 mm, and an inner diameter of 32 mm. A water-cooled copper tube was wrapped around the upper section of the cell. When the tube was heated, the cooling system created a temperature difference between the upper and lower sections, causing the interior gas to convect within the tube. The temperature was monitored by a type-K thermocouple located at the top of the crucible. Nie et al. [53] suggested that the SF6 cover gas would react with the steel wall of the holding furnace when they investigated the surface film of a Mg-alloy melt. To avoid this reaction, the interior surface of the steel oxidation cell (shown in Fig. 2) and the upper half section of the thermocouple were coated with boron nitride (the Mg-alloy was not in contact with boron nitride).

Fig. 2. Schematic of the oxidation cell used to study the evolution of the oxide films of the entrainment defects (unit mm).

During the experiment, a block of solid AZ91 alloy was placed in a magnesia crucible located at the bottom of the oxidation cell. The cell was heated to 100 °C in an electric resistance furnace under a gas flow rate of 1 L/min. The cell was held at this temperature for 20 min, to replace the original trapped atmosphere (i.e. air). Then, the oxidation cell was further heated to 700 °C, melting the AZ91 sample. The gas inlet and exit valves were then closed, creating a sealed environment for oxidation under a limited supply of cover gas. The oxidation cell was then held at 700 ± 10 °C for periods of time from 5 min to 30 min in 5-min intervals. At the end of each holding time, the cell was quenched in water. After cooling to room temperature, the oxidised sample was sectioned, polished, and subsequently examined by SEM.

3. Results

3.1. Structure and composition of the entrainment defects formed in SF6/air

The structure and composition of the entrainment defect formed in the AZ91 castings under a cover gas of 0.5%SF6/air was observed by SEM and EDS. The results indicate that there exist two types of entrainment defects which are sketched in Fig. 3: (1) Type A defect whose oxide film has a traditional single-layered structure and (2) Type B defect, whose oxide film has two layers. The details of these defects were introduced in the following. Here it should be noticed that, as the entrainment defects are also known as biofilms or double oxide film, the oxide films of Type B defect were referred to as “multi-layered oxide film” or “multi-layered structure” in the present work to avoid a confusing description such as “the double-layered oxide film of a double oxide film defect”.

Fig. 3. Schematic of the different types of entrainment defects found in AZ91 castings. (a) Type A defect with a single-layered oxide film and (b) Type B defect with two-layered oxide film.

Fig. 4(a-b) shows a Type A defect having a compact single-layered oxide film with about 0.4 µm thickness. Oxygen, fluorine, magnesium and aluminium were detected in this film (Fig. 4c). It is speculated that oxide film is the mixture of fluoride and oxide of magnesium and aluminium. The detection of fluorine revealed that an entrained cover gas was contained in the formation of this defect. That is to say that the pores shown in Fig. 4(a) were not shrinkage defects or hydrogen porosity, but entrainment defects. The detection of aluminium was different with Xiong and Wang’s previous study [47,48], which showed that no aluminium was contained in their surface film of an AZ91 melt protected by a SF6 cover gas. Sulphur could not be clearly recognized in the element map, but there was a S-peak in the corresponding ESD spectrum.

Fig. 4. (a) A Type A entrainment defect formed in SF6/air and having a single-layered oxide film, (b) the oxide film of this defect, (c) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area highlighted in (b).

Fig. 5(a-b) shows a Type B entrainment defect having a multi-layered oxide film. The compact outer layers of the oxide films were enriched with fluorine and oxygen (Fig. 5c), while their relatively porous inner layers were only enriched with oxygen (i.e., poor in fluorine) and partly grew together, thus forming a sandwich-like structure. Therefore, it is speculated that the outer layer is the mixture of fluoride and oxide, while the inner layer is mainly oxide. Sulphur could only be recognized in the EDX spectrum and could not be clearly identified in the element map, which might be due to the small S-content in the cover gas (i.e., 0.5% volume content of SF6 in the cover gas). In this oxide film, aluminium was contained in the outer layer of this oxide film but could not be clearly detected in the inner layer. Moreover, the distribution of Al seems to be uneven. It can be found that, in the right side of the defect, aluminium exists in the film but its concentration can not be identified to be higher than the matrix. However, there is a small area with much higher aluminium concentration in the left side of the defect. Such an uneven distribution of aluminium was also observed in other defects (shown in the following), and it is the result of the formation of some oxide particles in or under the film.

Fig. 5. (a) A Type B entrainment defect formed in SF6/air and having a multi-layered oxide film, (b) the oxide films of this defect have grown together, (c) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area shown in (b).

Figs. 4 and 5 show cross sectional observations of the entrainment defects formed in the AZ91 alloy sample cast under a cover gas of SF6/air. It is not sufficient to characterize the entrainment defects only by the figures observed from the two-dimensional section. To have a further understanding, the surface of the entrainment defects (i.e. the oxide film) was further studied by observing the fracture surface of the test bars.

Fig. 6(a) shows fracture surfaces of an AZ91 alloy tensile test bar produced in SF6/air. Symmetrical dark regions can be seen on both sides of the fracture surfaces. Fig. 6(b) shows boundaries between the dark and bright regions. The bright region consisted of jagged and broken features, while the surface of the dark region was relatively smooth and flat. In addition, the EDS results (Fig. 6c-d and Table 2) show that fluorine, oxygen, sulphur, and nitrogen were only detected in the dark regions, indicating that the dark regions were surface protective films entrained into the melt. Therefore, it could be suggested that the dark regions were an entrainment defect with consideration of their symmetrical nature. Similar defects on fracture surfaces of Al-alloy castings have been previously reported [7]Nitrides were only found in the oxide films on the test-bar fracture surfaces but never detected in the cross-sectional samples shown in Figs. 4 and 5. An underlying reason is that the nitrides contained in these samples may have hydrolysed during the sample polishing process [54].

Fig. 6. (a) A pair of the fracture surfaces of a AZ91 alloy tensile test bar produced under a cover gas of SF6/air. The dimension of the fracture surface is 5 mm × 6 mm, (b) a section of the boundary between the dark and bright regions shown in (a), (c-d) EDS spectrum of the (c) bright regions and (d) dark regions, (e) schematic of an entrainment defect contained in a test bar.

Table 2. EDS results (wt.%) corresponding to the regions shown in Fig. 6 (cover gas: SF6/air).

Empty CellCOMgFAlZnSN
Dark region in Fig. 6(b)3.481.3279.130.4713.630.570.080.73
Bright region in Fig. 6(b)3.5884.4811.250.68

In conjunction with the cross-sectional observation of the defects shown in Figs. 4 and 5, the structure of an entrainment defect contained in a tensile test bar was sketched as shown in Fig. 6(e). The defect contained an entrained gas enclosed by its oxide film, creating a void section inside the test bar. When the tensile force applied on the defect during the fracture process, the crack was initiated at the void section and propagated along the entrainment defect, since cracks would be propagated along the weakest path [55]. Therefore, when the test bar was finally fractured, the oxide films of entrainment defect appeared on both fracture surfaces of the test bar, as shown in Fig. 6(a).

3.2. Structure and composition of the entrainment defects formed in SF6/CO2

Similar to the entrainment defect formed in SF6/air, the defects formed under a cover gas of 0.5%SF6/CO2 also had two types of oxide films (i.e., single-layered and multi-layered types). Fig. 7(a) shows an example of the entrainment defects containing a multi-layered oxide film. A magnified observation to the defect (Fig. 7b) shows that the inner layers of the oxide films had grown together, presenting a sandwich-like structure, which was similar to the defects formed in an atmosphere of SF6/air (Fig. 5b). An EDS spectrum (Fig. 7c) revealed that the joint area (inner layer) of this sandwich-like structure mainly contained magnesium oxides. Peaks of fluorine, sulphur, and aluminium were recognized in this EDS spectrum, but their amount was relatively small. In contrast, the outer layers of the oxide films were compact and composed of a mixture of fluorides and oxides (Fig. 7d-e).

Fig. 7. (a) An example of entrainment defects formed in SF6/CO2 and having a multi-layered oxide film, (b) magnified observation of the defect, showing the inner layer of the oxide films has grown together, (c) EDS spectrum of the point denoted in (b), (d) outer layer of the oxide film, (e) SEM-EDS element maps (using Philips JEOL7000) corresponding to the area shown in (d).

Fig. 8(a) shows an entrainment defect on the fracture surfaces of an AZ91 alloy tensile test bar, which was produced in an atmosphere of 0.5%SF6/CO2. The corresponding EDS results (Table 3) showed that oxide film contained fluorides and oxides. Sulphur and nitrogen were not detected. Besides, a magnified observation (Fig. 8b) indicated spots on the oxide film surface. The diameter of the spots ranged from hundreds of nanometres to a few micron meters.

Fig. 8. (a) A pair of the fracture surfaces of a AZ91 alloy tensile test bar, produced in an atmosphere of SF6/CO2. The dimension of the fracture surface is 5 mm × 6 mm, (b) surface appearance of the oxide films on the fracture surfaces, showing spots on the film surface.

To further reveal the structure and composition of the oxide film clearly, the cross-section of the oxide film on a test-bar fracture surface was onsite exposed using the FIB technique (Fig. 9). As shown in Fig. 9a, a continuous oxide film was found between the platinum coating layer and the Mg-Al alloy substrate. Fig. 9 (b-c) shows a magnified observation to oxide films, indicating a multi-layered structure (denoted by the red box in Fig. 9c). The bottom layer was enriched with fluorine and oxygen and should be the mixture of fluoride and oxide, which was similar to the “outer layer” shown in Figs. 5 and 7, while the only-oxygen-enriched top layer was similar to the “inner layer” shown in Figs. 5 and 7.

Fig. 9. (a) A cross-sectional observation of the oxide film on the fracture surface of the AZ91 casting produced in SF6/CO2, exposed by FIB, (b) a magnified observation of area highlighted in (a), and (c) SEM-EDS elements map of the area shown in (b), obtained by CFEI Quanta 3D FEG FIB-SEM.

Except the continuous film, some individual particles were also observed in or below the continuous film, as shown in Fig. 9. An Al-enriched particle was detected in the left side of the oxide film shown in Fig. 9b and might be speculated to be spinel Mg2AlO4 because it also contains abundant magnesium and oxygen elements. The existing of such Mg2AlO4 particles is responsible for the high concentration of aluminium in small areas of the observed film and the uneven distribution of aluminium, as shown in Fig. 5(c). Here it should be emphasized that, although the other part of the bottom layer of the continuous oxide film contains less aluminium than this Al-enriched particle, the Fig. 9c indicated that the amount of aluminium in this bottom layer was still non-negligible, especially when comparing with the outer layer of the film. Below the right side of the oxide film shown in Fig. 9b, a particle was detected and speculated to be MgO because it is rich in Mg and O. According to Wang’s result [56], lots of discrete MgO particles can be formed on the surface of the Mg melt by the oxidation of Mg melt and Mg vapor. The MgO particles observed in our present work may be formed due to the same reasons. While, due to the differences in experimental conditions, less Mg melt can be vapored or react with O2, thus only a few of MgO particles formed in our work. An enrichment of carbon was also found in the film, revealing that CO2 was able to react with the melt, thus forming carbon or carbides. This carbon concentration was consistent with the relatively high carbon content of the oxide film shown in Table 3 (i.e., the dark region). In the area next to the oxide film.

Table 3. EDS results (wt.%) corresponding to the regions shown in Fig. 8 (cover gas: SF6/ CO2).

Empty CellCOMgFAlZnSN
Dark region in Fig. 8(a)7.253.6469.823.827.030.86
Bright region in Fig. 8(a)2.100.4482.8313.261.36

This cross-sectional observation of the oxide film on a test bar fracture surface (Fig. 9) further verified the schematic of the entrainment defect shown in Fig. 6(e). The entrainment defects formed in different atmospheres of SF6/CO2 and SF6/air had similar structures, but their compositions were different.

3.3. Evolution of the oxide films in the oxidation cell

The results in Section 3.1 and 3.2 have shown the structures and compositions of entrainment defects formed in AZ91 castings under cover gases of SF6/air and SF6/CO2. Different stages of the oxidation reaction may lead to the different structures and compositions of entrainment defects. Although Campbell has conjectured that an entrained gas may react with the surrounding melt, it is rarely reported that the reaction occurring between the Mg-alloy melt and entrapped cover gas. Previous researchers normally focus on the reaction between a Mg-alloy melt and the cover gas in an open environment [38,39,[46][47][48][49][50][51][52], which was different from the situation of a cover gas trapped into the melt. To further understand the formation of the entrainment defect in an AZ91 alloy, the evolution process of oxide films of the entrainment defect was further studied using an oxidation cell.

Fig. 10 (a and d) shows a surface film held for 5 min in the oxidation cell, protected by 0.5%SF6/air. There was only one single layer consisting of fluoride and oxide (MgF2 and MgO). In this surface film. Sulphur was detected in the EDS spectrum, but its amount was too small to be recognized in the element map. The structure and composition of this oxide film was similar to the single-layered films of entrainment defects shown in Fig. 4.

Fig. 10. Oxide films formed in the oxidation cell under a cover gas of 0.5%SF6/air and held at 700 °C for (a) 5 min; (b) 10 min; (c) 30 min, and (d-f) the SEM-EDS element maps (using Philips JEOL7000) corresponding to the oxide film shown in (a-c) respectively, (d) 5 min; (e) 10 min; (f) 30 min. The red points in (c and f) are the location references, denoting the boundary of the F-enriched layer in different element maps.

After a holding time of 10 min, a thin (O, S)-enriched top layer (around 700 nm) appeared upon the preliminary F-enriched film, forming a multi-layered structure, as shown in Fig. 10(b and e). The thickness of the (O, S)-enriched top layer increased with increased holding time. As shown in Fig. 10(c and f), the oxide film held for 30 min also had a multi-layered structure, but the thickness of its (O, S)-enriched top layer (around 2.5 µm) was higher than the that of the 10-min oxide film. The multi-layered oxide films shown in Fig. 10(b-c) presented a similar appearance to the films of the sandwich-like defect shown in Fig. 5.

The different structures of the oxide films shown in Fig. 10 indicated that fluorides in the cover gas would be preferentially consumed due to the reaction with the AZ91 alloy melt. After the depletion of fluorides, the residual cover gas reacted further with the liquid AZ91 alloy, forming the top (O, S)-enriched layer in the oxide film. Therefore, the different structures and compositions of entrainment defects shown in Figs. 4 and 5 may be due to an ongoing oxidation reaction between melt and entrapped cover gas.

This multi-layered structure has not been reported in previous publications concerning the protective surface film formed on a Mg-alloy melt [38,[46][47][48][49][50][51]. This may be due to the fact that previous researchers carried out their experiments with an un-limited amount of cover gas, creating a situation where the fluorides in the cover gas were not able to become depleted. Therefore, the oxide film of an entrainment defect had behaviour traits similar to the oxide films shown in Fig. 10, but different from the oxide films formed on the Mg-alloy melt surface reported in [38,[46][47][48][49][50][51].

Similar with the oxide films held in SF6/air, the oxide films formed in SF6/CO2 also had different structures with different holding times in the oxidation cell. Fig. 11(a) shows an oxide film, held on an AZ91 melt surface under a cover gas of 0.5%SF6/CO2 for 5 min. This film had a single-layered structure consisting of MgF2. The existence of MgO could not be confirmed in this film. After the holding time of 30 min, the film had a multi-layered structure; the inner layer was of a compact and uniform appearance and composed of MgF2, while the outer layer is the mixture of MgF2 and MgO. Sulphur was not detected in this film, which was different from the surface film formed in 0.5%SF6/air. Therefore, fluorides in the cover gas of 0.5%SF6/CO2 were also preferentially consumed at an early stage of the film growth process. Compared with the film formed in SF6/air, the MgO in film formed in SF6/CO2 appeared later and sulphide did not appear within 30 min. It may mean that the formation and evolution of film in SF6/air is faster than SF6/CO2. CO2 may have subsequently reacted with the melt to form MgO, while sulphur-containing compounds accumulated in the cover gas and reacted to form sulphide in very late stage (may after 30 min in oxidation cell).

Fig. 11. Oxide films formed in the oxidation cell under a cover gas of 0.5%SF6/CO2, and their SEM-EDS element maps (using Philips JEOL7000). They were held at 700 °C for (a) 5 min; (b) 30 min. The red points in (b) are the location references, denoting the boundary between the top and bottom layers in the oxide film.

4. Discussion

4.1. Evolution of entrainment defects formed in SF6/air

HSC software from Outokumpu HSC Chemistry for Windows (http://www.hsc-chemistry.net/) was used to carry out thermodynamic calculations needed to explore the reactions which might occur between the trapped gases and liquid AZ91 alloy. The solutions to the calculations suggest which products are most likely to form in the reaction process between a small amount of cover gas (i.e., the amount within a trapped bubble) and the AZ91-alloy melt.

In the trials, the pressure was set to 1 atm, and the temperature set to 700 °C. The amount of the cover gas was assumed to be 7 × 10−7 kg, with a volume of approximately 0.57 cm3 (3.14 × 10−8 kmol) for 0.5%SF6/air, and 0.35 cm3 (3.12 × 10−8 kmol) for 0.5%SF6/CO2. The amount of the AZ91 alloy melt in contact with the trapped gas was assumed to be sufficient to complete all reactions. The decomposition products of SF6 were SF5, SF4, SF3, SF2, F2, S(g), S2(g) and F(g) [57][58][59][60].

Fig. 12 shows the equilibrium diagram of the thermodynamic calculation of the reaction between the AZ91 alloy and 0.5%SF6/air. In the diagram, the reactants and products with less than 10−15 kmol have not been shown, as this was 5 orders of magnitude less than the amount of SF6 present (≈ 1.57 × 10−10 kmol) and therefore would not affect the observed process in a practical way.

Fig. 12. An equilibrium diagram for the reaction between 7e-7 kg 0.5%SF6/air and a sufficient amount of AZ91 alloy. The X axis is the amount of AZ91 alloy melt having reacted with the entrained gas, and the vertical Y-axis is the amount of the reactants and products.

This reaction process could be divided into 3 stages.

Stage 1: The formation of fluorides. the AZ91 melt preferentially reacted with SF6 and its decomposition products, producing MgF2, AlF3, and ZnF2. However, the amount of ZnF2 may have been too small to be detected practically (1.25 × 10−12 kmol of ZnF2 compared with 3 × 10−10 kmol of MgF2), which may be the reason why Zn was not detected in any the oxide films shown in Sections 3.13.3. Meanwhile, sulphur accumulated in the residual gas as SO2.

Stage 2: The formation of oxides. After the liquid AZ91 alloy had depleted all the available fluorides in the entrapped gas, the amount of AlF3 and ZnF2 quickly reduced due to a reaction with Mg. O2(g) and SO2 reacted with the AZ91 melt, forming MgO, Al2O3, MgAl2O4, ZnO, ZnSO4 and MgSO4. However, the amount of ZnO and ZnSO4 would have been too small to be found practically by EDS (e.g. 9.5 × 10−12 kmol of ZnO,1.38 × 10−14 kmol of ZnSO4, in contrast to 4.68 × 10−10 kmol of MgF2, when the amount of AZ91 on the X-axis is 2.5 × 10−9 kmol). In the experimental cases, the concentration of F in the cover gas is very low, whole the concentration f O is much higher. Therefore, the stage 1 and 2, i.e, the formation of fluoride and oxide may happen simultaneously at the beginning of the reaction, resulting in the formation of a singer-layered mixture of fluoride and oxide, as shown in Figs. 4 and 10(a). While an inner layer consisted of oxides but fluorides could form after the complete depletion of F element in the cover gas.

Stages 1- 2 theoretically verified the formation process of the multi-layered structure shown in Fig. 10.

The amount of MgAl2O4 and Al2O3 in the oxide film was of a sufficient amount to be detected, which was consistent with the oxide films shown in Fig. 4. However, the existence of aluminium could not be recognized in the oxide films grown in the oxidation cell, as shown in Fig. 10. This absence of Al may be due to the following reactions between the surface film and AZ91 alloy melt:(1)

Al2O3 + 3Mg + = 3MgO + 2Al, △G(700 °C) = -119.82 kJ/mol(2)

Mg + MgAl2O4 = MgO + Al, △G(700 °C) =-106.34 kJ/molwhich could not be simulated by the HSC software since the thermodynamic calculation was carried out under an assumption that the reactants were in full contact with each other. However, in a practical process, the AZ91 melt and the cover gas would not be able to be in contact with each other completely, due to the existence of the protective surface film.

Stage 3: The formation of Sulphide and nitride. After a holding time of 30 min, the gas-phase fluorides and oxides in the oxidation cell had become depleted, allowing the melt reaction with the residual gas, forming an additional sulphur-enriched layer upon the initial F-enriched or (F, O)-enriched surface film, thus resulting in the observed multi-layered structure shown in Fig. 10 (b and c). Besides, nitrogen reacted with the AZ91 melt until all reactions were completed. The oxide film shown in Fig. 6 may correspond to this reaction stage due to its nitride content. However, the results shows that the nitrides were not detected in the polished samples shown in Figs. 4 and 5, but only found on the test bar fracture surfaces. The nitrides may have hydrolysed during the sample preparation process, as follows [54]:(3)

Mg3N2 + 6H2O =3Mg(OH)2 + 2NH3↑(4)

AlN+ 3H2O =Al(OH)3 + NH3

In addition, Schmidt et al. [61] found that Mg3N2 and AlN could react to form ternary nitrides (Mg3AlnNn+2, n= 1, 2, 3…). HSC software did not contain the database of ternary nitrides, and it could not be added into the calculation. The oxide films in this stage may also contain ternary nitrides.

4.2. Evolution of entrainment defects formed in SF6/CO2

Fig. 13 shows the results of the thermodynamic calculation between AZ91 alloy and 0.5%SF6/CO2. This reaction processes can also be divided into three stages.

Fig. 13. An equilibrium diagram for the reaction between 7e-7 kg 0.5%SF6/CO2 and a sufficient amount of AZ91 alloy. The X axis denotes the amount of Mg alloy melt having reacted with the entrained gas, and the vertical Y-axis denotes the amounts of the reactants and products.

Stage 1: The formation of fluorides. SF6 and its decomposition products were consumed by the AZ91 melt, forming MgF2, AlF3, and ZnF2. As in the reaction of AZ91 in 0.5%SF6/air, the amount of ZnF2 was too small to be detected practically (1.51 × 10−13 kmol of ZnF2 compared with 2.67 × 10−10 kmol of MgF2). Sulphur accumulated in the residual trapped gas as S2(g) and a portion of the S2(g) reacted with CO2, to form SO2 and CO. The products in this reaction stage were consistent with the film shown in Fig. 11(a), which had a single layer structure that contained fluorides only.

Stage 2: The formation of oxides. AlF3 and ZnF2 reacted with the Mg in the AZ91 melt, forming MgF2, Al and Zn. The SO2 began to be consumed, producing oxides in the surface film and S2(g) in the cover gas. Meanwhile, the CO2 directly reacted with the AZ91 melt, forming CO, MgO, ZnO, and Al2O3. The oxide films shown in Figs. 9 and 11(b) may correspond to this reaction stage due to their oxygen-enriched layer and multi-layered structure.

The CO in the cover gas could further react with the AZ91 melt, producing C. This carbon may further react with Mg to form Mg carbides, when the temperature reduced (during solidification period) [62]. This may be the reason for the high carbon content in the oxide film shown in Figs. 89. Liang et al. [39] also reported carbon-detection in an AZ91 alloy surface film protected by SO2/CO2. The produced Al2O3 may be further combined with MgO, forming MgAl2O4 [63]. As discussed in Section 4.1, the alumina and spinel can react with Mg, causing an absence of aluminium in the surface films, as shown in Fig. 11.

Stage 3: The formation of Sulphide. the AZ91 melt began to consume S2(g) in the residual entrapped gas, forming ZnS and MgS. These reactions did not occur until the last stage of the reaction process, which could be the reason why the S-content in the defect shown Fig. 7(c) was small.

In summary, thermodynamic calculations indicate that the AZ91 melt will react with the cover gas to form fluorides firstly, then oxides and sulphides in the last. The oxide film in the different reaction stages would have different structures and compositions.

4.3. Effect of the carrier gases on consumption of the entrained gas and the reproducibility of AZ91 castings

The evolution processes of entrainment defects, formed in SF6/air and SF6/CO2, have been suggested in Sections 4.1 and 4.2. The theoretical calculations were verified with respect to the corresponding oxide films found in practical samples. The atmosphere within an entrainment defect could be efficiently consumed due to the reaction with liquid Mg-alloy, in a scenario dissimilar to the Al-alloy system (i.e., nitrogen in an entrained air bubble would not efficiently react with Al-alloy melt [64,65], however, nitrogen would be more readily consumed in liquid Mg alloys, commonly referred to as “nitrogen burning” [66]).

The reaction between the entrained gas and the surrounding liquid Mg-alloy converted the entrained gas into solid compounds (e.g. MgO) within the oxide film, thus reducing the void volume of the entrainment defect and hence probably causing a collapse of the defect (e.g., if an entrained gas of air was depleted by the surrounding liquid Mg-alloy, under an assumption that the melt temperature is 700 °C and the depth of liquid Mg-alloy is 10 cm, the total volume of the final solid products would be 0.044% of the initial volume taken by the entrapped air).

The relationship between the void volume reduction of entrainment defects and the corresponding casting properties has been widely studied in Al-alloy castings. Nyahumwa and Campbell [16] reported that the Hot Isostatic Pressing (HIP) process caused the entrainment defects in Al-alloy castings to collapse and their oxide surfaces forced into contact. The fatigue lives of their castings were improved after HIP. Nyahumwa and Campbell [16] also suggested a potential bonding of the double oxide films that were in contact with each other, but there was no direct evidence to support this. This binding phenomenon was further investigated by Aryafar et.al.[8], who re-melted two Al-alloy bars with oxide skins in a steel tube and then carried out a tensile strength test on the solidified sample. They found that the oxide skins of the Al-alloy bars strongly bonded with each other and became even stronger with an extension of the melt holding time, indicating a potential “healing” phenomenon due to the consumption of the entrained gas within the double oxide film structure. In addition, Raidszadeh and Griffiths [9,19] successfully reduced the negative effect of entrainment defects on the reproducibility of Al-alloy castings, by extending the melt holding time before solidification, which allowed the entrained gas to have a longer time to react with the surrounding melt.

With consideration of the previous work mentioned, the consumption of the entrained gas in Mg-alloy castings may diminish the negative effect of entrainment defects in the following two ways.

(1) Bonding phenomenon of the double oxide films. The sandwich-like structure shown in Fig. 5 and 7 indicated a potential bonding of the double oxide film structure. However, more evidence is required to quantify the increase in strength due to the bonding of the oxide films.

(2) Void volume reduction of entrainment defects. The positive effect of void-volume reduction on the quality of castings has been widely demonstrated by the HIP process [67]. As the evolution processes discussed in Section 4.14.2, the oxide films of entrainment defects can grow together due to an ongoing reaction between the entrained gas and surrounding AZ91 alloy melt. The volume of the final solid products was significant small compared with the entrained gas (i.e., 0.044% as previously mentioned).

Therefore, the consumption rate of the entrained gas (i.e., the growth rate of oxide films) may be a critical parameter for improving the quality of AZ91 alloy castings. The oxide film growth rate in the oxidization cell was accordingly further investigated.

Fig. 14 shows a comparison of the surface film growth rates in different cover gases (i.e., 0.5%SF6/air and 0.5%SF6/CO2). 15 random points on each sample were selected for film thickness measurements. The 95% confidence interval (95%CI) was computed under an assumption that the variation of the film thickness followed a Gaussian distribution. It can be seen that all the surface films formed in 0.5%SF6/air grew faster than those formed in 0.5%SF6/CO2. The different growth rates suggested that the entrained-gas consumption rate of 0.5%SF6/air was higher than that of 0.5%SF6/CO2, which was more beneficial for the consumption of the entrained gas.

Fig. 14. A comparison of the AZ91 alloy oxide film growth rates in 0.5%SF6/air and 0.5%SF6/CO2

It should be noted that, in the oxidation cell, the contact area of liquid AZ91 alloy and cover gas (i.e. the size of the crucible) was relatively small with consideration of the large volume of melt and gas. Consequently, the holding time for the oxide film growth within the oxidation cell was comparatively long (i.e., 5–30 min). However, the entrainment defects contained in a real casting are comparatively very small (i.e., a few microns size as shown in Figs. 36, and [7]), and the entrained gas is fully enclosed by the surrounding melt, creating a relatively large contact area. Hence the reaction time for cover gas and the AZ91 alloy melt may be comparatively short. In addition, the solidification time of real Mg-alloy sand castings can be a few minutes (e.g. Guo [68] reported that a Mg-alloy sand casting with 60 mm diameter required 4 min to be solidified). Therefore, it can be expected that an entrained gas trapped during an Mg-alloy melt pouring process will be readily consumed by the surrounding melt, especially for sand castings and large-size castings, where solidification times are long.

Therefore, the different cover gases (0.5%SF6/air and 0.5%SF6/CO2) associated with different consumption rates of the entrained gases may affect the reproducibility of the final castings. To verify this assumption, the AZ91 castings produced in 0.5%SF6/air and 0.5%SF6/CO2 were machined into test bars for mechanical evaluation. A Weibull analysis was carried out using both linear least square (LLS) method and non-linear least square (non-LLS) method [69].

Fig. 15(a-b) shows a traditional 2-p linearized Weibull plot of the UTS and elongation of the AZ91 alloy castings, obtained by the LLS method. The estimator used is P= (i-0.5)/N, which was suggested to cause the lowest bias among all the popular estimators [69,70]. The casting produced in SF6/air has an UTS Weibull moduli of 16.9, and an elongation Weibull moduli of 5.0. In contrast, the UTS and elongation Weibull modulus of the casting produced in SF6/CO2 are 7.7 and 2.7 respectively, suggesting that the reproducibility of the casting protected by SF6/CO2 were much lower than that produced in SF6/air.

Fig. 15. The Weibull modulus of AZ91 castings produced in different atmospheres, estimated by (a-b) the linear least square method, (c-d) the non-linear least square method, where SSR is the sum of residual squares.

In addition, the author’s previous publication [69] demonstrated a shortcoming of the linearized Weibull plots, which may cause a higher bias and incorrect R2 interruption of the Weibull estimation. A Non-LLS Weibull estimation was therefore carried out, as shown in Fig. 15 (c-d). The UTS Weibull modulus of the SF6/air casting was 20.8, while the casting produced under SF6/CO2 had a lower UTS Weibull modulus of 11.4, showing a clear difference in their reproducibility. In addition, the SF6/air elongation (El%) dataset also had a Weibull modulus (shape = 5.8) higher than the elongation dataset of SF6/CO2 (shape = 3.1). Therefore, both the LLS and Non-LLS estimations suggested that the SF6/air casting has a higher reproducibility than the SF6/CO2 casting. It supports the method that the use of air instead of CO2 contributes to a quicker consumption of the entrained gas, which may reduce the void volume within the defects. Therefore, the use of 0.5%SF6/air instead of 0.5%SF6/CO2 (which increased the consumption rate of the entrained gas) improved the reproducibility of the AZ91 castings.

However, it should be noted that not all the Mg-alloy foundries followed the casting process used in present work. The Mg-alloy melt in present work was degassed, thus reducing the effect of hydrogen on the consumption of the entrained gas (i.e., hydrogen could diffuse into the entrained gas, potentially suppressing the depletion of the entrained gas [7,71,72]). In contrast, in Mg-alloy foundries, the Mg-alloy melt is not normally degassed, since it was widely believed that there is not a ‘gas problem’ when casting magnesium and hence no significant change in tensile properties [73]. Although studies have shown the negative effect of hydrogen on the mechanical properties of Mg-alloy castings [41,42,73], a degassing process is still not very popular in Mg-alloy foundries.

Moreover, in present work, the sand mould cavity was flushed with the SF6 cover gas prior to pouring [22]. However, not all the Mg-alloy foundries flushed the mould cavity in this way. For example, the Stone Foundry Ltd (UK) used sulphur powder instead of the cover-gas flushing. The entrained gas within their castings may be SO2/air, rather than the protective gas.

Therefore, although the results in present work have shown that using air instead of CO2 improved the reproducibility of the final casting, it still requires further investigations to confirm the effect of carrier gases with respect to different industrial Mg-alloy casting processes.

7. Conclusion

Entrainment defects formed in an AZ91 alloy were observed. Their oxide films had two types of structure: single-layered and multi-layered. The multi-layered oxide film can grow together forming a sandwich-like structure in the final casting.2.

Both the experimental results and the theoretical thermodynamic calculations demonstrated that fluorides in the trapped gas were depleted prior to the consumption of sulphur. A three-stage evolution process of the double oxide film defects has been suggested. The oxide films contained different combinations of compounds, depending on the evolution stage. The defects formed in SF6/air had a similar structure to those formed in SF6/CO2, but the compositions of their oxide films were different. The oxide-film formation and evolution process of the entrainment defects were different from that of the Mg-alloy surface films previous reported (i.e., MgO formed prior to MgF2).3.

The growth rate of the oxide film was demonstrated to be greater under SF6/air than SF6/CO2, contributing to a quicker consumption of the damaging entrapped gas. The reproducibility of an AZ91 alloy casting improved when using SF6/air instead of SF6/CO2.

Acknowledgements

The authors acknowledge funding from the EPSRC LiME grant EP/H026177/1, and the help from Dr W.D. Griffiths and Mr. Adrian Carden (University of Birmingham). The casting work was carried out in University of Birmingham.

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Fig. 1 Multi-physics phenomena in the laser-material interaction zone

COMPARISON BETWEEN GREEN AND
INFRARED LASER IN LASER POWDER BED
FUSION OF PURE COPPER THROUGH HIGH
FIDELITY NUMERICAL MODELLING AT MESOSCALE

316-L 스테인리스강의 레이저 분말 베드 융합 중 콜드 스패터 형성의 충실도 높은 수치 모델링

W.E. ALPHONSO1*, M. BAYAT1 and J.H. HATTEL1
*Corresponding author
1Technical University of Denmark (DTU), 2800, Kgs, Lyngby, Denmark

ABSTRACT

L-PBF(Laser Powder Bed Fusion)는 금속 적층 제조(MAM) 기술로, 기존 제조 공정에 비해 부품 설계 자유도, 조립품 통합, 부품 맞춤화 및 낮은 툴링 비용과 같은 여러 이점을 산업에 제공합니다.

전기 코일 및 열 관리 장치는 일반적으로 높은 전기 및 열 전도성 특성으로 인해 순수 구리로 제조됩니다. 따라서 순동의 L-PBF가 가능하다면 기하학적으로 최적화된 방열판과 자유형 전자코일을 제작할 수 있습니다.

그러나 L-PBF로 조밀한 순동 부품을 생산하는 것은 적외선에 대한 낮은 광 흡수율과 높은 열전도율로 인해 어렵습니다. 기존의 L-PBF 시스템에서 조밀한 구리 부품을 생산하려면 적외선 레이저의 출력을 500W 이상으로 높이거나 구리의 광흡수율이 높은 녹색 레이저를 사용해야 합니다.

적외선 레이저 출력을 높이면 후면 반사로 인해 레이저 시스템의 광학 구성 요소가 손상되고 렌즈의 열 광학 현상으로 인해 공정이 불안정해질 수 있습니다. 이 작업에서 FVM(Finite Volume Method)에 기반한 다중 물리학 중간 규모 수치 모델은 Flow-3D에서 개발되어 용융 풀 역학과 궁극적으로 부품 품질을 제어하는 ​​물리적 현상 상호 작용을 조사합니다.

녹색 레이저 열원과 적외선 레이저 열원은 기판 위의 순수 구리 분말 베드에 단일 트랙 증착을 생성하기 위해 개별적으로 사용됩니다.

용융 풀 역학에 대한 레이저 열원의 유사하지 않은 광학 흡수 특성의 영향이 탐구됩니다. 수치 모델을 검증하기 위해 단일 트랙이 구리 분말 베드에 증착되고 시뮬레이션된 용융 풀 모양과 크기가 비교되는 실험이 수행되었습니다.

녹색 레이저는 광흡수율이 높아 전도 및 키홀 모드 용융이 가능하고 적외선 레이저는 흡수율이 낮아 키홀 모드 용융만 가능하다. 레이저 파장에 대한 용융 모드의 변화는 궁극적으로 기계적, 전기적 및 열적 특성에 영향을 미치는 열 구배 및 냉각 속도에 대한 결과를 가져옵니다.

Laser Powder Bed Fusion (L-PBF) is a Metal Additive Manufacturing (MAM) technology which offers several advantages to industries such as part design freedom, consolidation of assemblies, part customization and low tooling cost over conventional manufacturing processes. Electric coils and thermal management devices are generally manufactured from pure copper due to its high electrical and thermal conductivity properties. Therefore, if L-PBF of pure copper is feasible, geometrically optimized heat sinks and free-form electromagnetic coils can be manufactured. However, producing dense pure copper parts by L-PBF is difficult due to low optical absorptivity to infrared radiation and high thermal conductivity. To produce dense copper parts in a conventional L-PBF system either the power of the infrared laser must be increased above 500W, or a green laser should be used for which copper has a high optical absorptivity. Increasing the infrared laser power can damage the optical components of the laser systems due to back reflections and create instabilities in the process due to thermal-optical phenomenon of the lenses. In this work, a multi-physics meso-scale numerical model based on Finite Volume Method (FVM) is developed in Flow-3D to investigate the physical phenomena interaction which governs the melt pool dynamics and ultimately the part quality. A green laser heat source and an infrared laser heat source are used individually to create single track deposition on pure copper powder bed above a substrate. The effect of the dissimilar optical absorptivity property of laser heat sources on the melt pool dynamics is explored. To validate the numerical model, experiments were conducted wherein single tracks are deposited on a copper powder bed and the simulated melt pool shape and size are compared. As the green laser has a high optical absorptivity, a conduction and keyhole mode melting is possible while for the infrared laser only keyhole mode melting is possible due to low absorptivity. The variation in melting modes with respect to the laser wavelength has an outcome on thermal gradient and cooling rates which ultimately affect the mechanical, electrical, and thermal properties.

Keywords

Pure Copper, Laser Powder Bed Fusion, Finite Volume Method, multi-physics

Fig. 1 Multi-physics phenomena in the laser-material interaction zone
Fig. 1 Multi-physics phenomena in the laser-material interaction zone
Fig. 2 Framework for single laser track simulation model including powder bed and substrate (a) computational domain with boundaries (b) discretization of the domain with uniform quad mesh.
Fig. 2 Framework for single laser track simulation model including powder bed and substrate (a) computational domain with boundaries (b) discretization of the domain with uniform quad mesh.
Fig. 3 2D melt pool contours from the numerical model compared to experiments [16] for (a) VED = 65 J/mm3 at 7 mm from the beginning of the single track (b) VED = 103 J/mm3 at 3 mm from the beginning of the single track (c) VED = 103 J/mm3 at 7 mm from the beginning of the single track. In the 2D contour, the non-melted region is indicated in blue, and the melted region is indicated by red and green when the VED is 65 J/mm3 and 103 J/mm3 respectively.
Fig. 3 2D melt pool contours from the numerical model compared to experiments [16] for (a) VED = 65 J/mm3 at 7 mm from the beginning of the single track (b) VED = 103 J/mm3 at 3 mm from the beginning of the single track (c) VED = 103 J/mm3 at 7 mm from the beginning of the single track. In the 2D contour, the non-melted region is indicated in blue, and the melted region is indicated by red and green when the VED is 65 J/mm3 and 103 J/mm3 respectively.
Fig. 4 3D temperature contour plots of during single track L-PBF process at time1.8 µs when (a) VED = 65 J/mm3 (b) VED = 103 J/mm3 along with 2D melt pool contours at 5 mm from the laser initial position. In the 2D contour, the non-melted region is indicated in blue, and the melted region is indicated by red and green when the VED is 65 J/mm3 and 103 J/mm3 respectively.
Fig. 4 3D temperature contour plots of during single track L-PBF process at time1.8 µs when (a) VED = 65 J/mm3 (b) VED = 103 J/mm3 along with 2D melt pool contours at 5 mm from the laser initial position. In the 2D contour, the non-melted region is indicated in blue, and the melted region is indicated by red and green when the VED is 65 J/mm3 and 103 J/mm3 respectively.

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Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.

플라즈마 회전 전극 공정 중 분말 형성에 대한 공정 매개변수 및 냉각 가스의 영향

Effects of process parameters and cooling gas on powder formation during the plasma rotating electrode process

Yujie Cuia Yufan Zhaoa1 Haruko Numatab Kenta Yamanakaa Huakang Biana Kenta Aoyagia AkihikoChibaa
aInstitute for Materials Research, Tohoku University, Sendai 980-8577, JapanbDepartment of Materials Processing, Graduate School of Engineering, Tohoku University, Sendai 980-8577, Japan

Highlights

•The limitation of increasing the rotational speed in decreasing powder size was clarified.

•Cooling and disturbance effects varied with the gas flowing rate.

•Inclined angle of the residual electrode end face affected powder formation.

•Additional cooling gas flowing could be applied to control powder size.

Abstract

The plasma rotating electrode process (PREP) is rapidly becoming an important powder fabrication method in additive manufacturing. However, the low production rate of fine PREP powder limits the development of PREP. Herein, we investigated different factors affecting powder formation during PREP by combining experimental methods and numerical simulations. The limitation of increasing the rotation electrode speed in decreasing powder size is attributed to the increased probability of adjacent droplets recombining and the decreased tendency of granulation. The effects of additional Ar/He gas flowing on the rotational electrode on powder formation is determined through the cooling effect, the disturbance effect, and the inclined effect of the residual electrode end face simultaneously. A smaller-sized powder was obtained in the He atmosphere owing to the larger inclined angle of the residual electrode end face compared to the Ar atmosphere. Our research highlights the route for the fabrication of smaller-sized powders using PREP.

플라즈마 회전 전극 공정(PREP)은 적층 제조 에서 중요한 분말 제조 방법으로 빠르게 자리잡고 있습니다. 그러나 미세한 PREP 분말의 낮은 생산율은 PREP의 개발을 제한합니다. 여기에서 우리는 실험 방법과 수치 시뮬레이션을 결합하여 PREP 동안 분말 형성에 영향을 미치는 다양한 요인을 조사했습니다. 분말 크기 감소에서 회전 전극 속도 증가의 한계는 인접한 액적 재결합 확률 증가 및 과립화 경향 감소에 기인합니다.. 회전 전극에 흐르는 추가 Ar/He 가스가 분말 형성에 미치는 영향은 냉각 효과, 외란 효과 및 잔류 전극 단면의 경사 효과를 통해 동시에 결정됩니다. He 분위기에서는 Ar 분위기에 비해 잔류 전극 단면의 경사각이 크기 때문에 더 작은 크기의 분말이 얻어졌다. 우리의 연구는 PREP를 사용하여 더 작은 크기의 분말을 제조하는 경로를 강조합니다.

Keywords

Plasma rotating electrode process

Ti-6Al-4 V alloy, Rotating speed, Numerical simulation, Gas flowing, Powder size

Introduction

With the development of additive manufacturing, there has been a significant increase in high-quality powder production demand [1,2]. The initial powder characteristics are closely related to the uniform powder spreading [3,4], packing density [5], and layer thickness observed during additive manufacturing [6], thus determining the mechanical properties of the additive manufactured parts [7,8]. Gas atomization (GA) [9–11], centrifugal atomization (CA) [12–15], and the plasma rotating electrode process (PREP) are three important powder fabrication methods.

Currently, GA is the dominant powder fabrication method used in additive manufacturing [16] for the fabrication of a wide range of alloys [11]. GA produces powders by impinging a liquid metal stream to droplets through a high-speed gas flow of nitrogen, argon, or helium. With relatively low energy consumption and a high fraction of fine powders, GA has become the most popular powder manufacturing technology for AM.

The entrapped gas pores are generally formed in the powder after solidification during GA, in which the molten metal is impacted by a high-speed atomization gas jet. In addition, satellites are formed in GA powder when fine particles adhere to partially molten particles.

The gas pores of GA powder result in porosity generation in the additive manufactured parts, which in turn deteriorates its mechanical properties because pores can become crack initiation sites [17]. In CA, a molten metal stream is poured directly onto an atomizer disc spinning at a high rotational speed. A thin film is formed on the surface of the disc, which breaks into small droplets due to the centrifugal force. Metal powder is obtained when these droplets solidify.

Compared with GA powder, CA powder exhibits higher sphericity, lower impurity content, fewer satellites, and narrower particle size distribution [12]. However, very high speed is required to obtain fine powder by CA. In PREP, the molten metal, melted using the plasma arc, is ejected from the rotating rod through centrifugal force. Compared with GA powder, PREP-produced powders also have higher sphericity and fewer pores and satellites [18].

For instance, PREP-fabricated Ti6Al-4 V alloy powder with a powder size below 150 μm exhibits lower porosity than gas-atomized powder [19], which decreases the porosity of additive manufactured parts. Furthermore, the process window during electron beam melting was broadened using PREP powder compared to GA powder in Inconel 718 alloy [20] owing to the higher sphericity of the PREP powder.

In summary, PREP powder exhibits many advantages and is highly recommended for powder-based additive manufacturing and direct energy deposition-type additive manufacturing. However, the low production rate of fine PREP powder limits the widespread application of PREP powder in additive manufacturing.

Although increasing the rotating speed is an effective method to decrease the powder size [21,22], the reduction in powder size becomes smaller with the increased rotating speed [23]. The occurrence of limiting effects has not been fully clarified yet.

Moreover, the powder size can be decreased by increasing the rotating electrode diameter [24]. However, these methods are quite demanding for the PREP equipment. For instance, it is costly to revise the PREP equipment to meet the demand of further increasing the rotating speed or electrode diameter.

Accordingly, more feasible methods should be developed to further decrease the PREP powder size. Another factor that influences powder formation is the melting rate [25]. It has been reported that increasing the melting rate decreases the powder size of Inconel 718 alloy [26].

In contrast, the powder size of SUS316 alloy was decreased by decreasing the plasma current within certain ranges. This was ascribed to the formation of larger-sized droplets from fluid strips with increased thickness and spatial density at higher plasma currents [27]. The powder size of NiTi alloy also decreases at lower melting rates [28]. Consequently, altering the melting rate, varied with the plasma current, is expected to regulate the PREP powder size.

Furthermore, gas flowing has a significant influence on powder formation [27,29–31]. On one hand, the disturbance effect of gas flowing promotes fluid granulation, which in turn contributes to the formation of smaller-sized powder [27]. On the other hand, the cooling effect of gas flowing facilitates the formation of large-sized powder due to increased viscosity and surface tension. However, there is a lack of systematic research on the effect of different gas flowing on powder formation during PREP.

Herein, the authors systematically studied the effects of rotating speed, electrode diameter, plasma current, and gas flowing on the formation of Ti-6Al-4 V alloy powder during PREP as additive manufactured Ti-6Al-4 V alloy exhibits great application potential [32]. Numerical simulations were conducted to explain why increasing the rotating speed is not effective in decreasing powder size when the rotation speed reaches a certain level. In addition, the different factors incited by the Ar/He gas flowing on powder formation were clarified.

Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.
Fig. 1. Schematic figure showing the PREP with additional gas flowing on the end face of electrode.

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Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

반고체 레오 다이 캐스팅 공정으로 제작된 알루미늄 합금 브래킷의 수치 시뮬레이션 및 생산 실험 검증을 기반으로 한 게이팅 시스템 설계

International Journal of Metalcasting volume 16, pages878–893 (2022)Cite this article

Abstract

In this study a gating system including sprue, runner and overflows for semi-solid rheocasting of aluminum alloy was designed by means of numerical simulations with a commercial software. The effects of pouring temperature, mold temperature and injection speed on the filling process performance of semi-solid die casting were studied. Based on orthogonal test analysis, the optimal die casting process parameters were selected, which were metal pouring temperature 590 °C, mold temperature 260 °C and injection velocity 0.5 m/s. Semi-solid slurry preparation process of Swirled Enthalpy Equilibration Device (SEED) was used for die casting production experiment. Aluminum alloy semi-solid bracket components were successfully produced with the key die casting process parameters selected, which was consistent with the simulation result. The design of semi-solid gating system was further verified by observing and analyzing the microstructure of different zones of the casting. The characteristic parameters, particle size and shape factor of microstructure of the produced semi-solid casting showed that the semi-solid aluminum alloy components are of good quality.

이 연구에서 알루미늄 합금의 반고체 레오캐스팅을 위한 스프루, 러너 및 오버플로를 포함하는 게이팅 시스템은 상용 소프트웨어를 사용한 수치 시뮬레이션을 통해 설계되었습니다. 주입 온도, 금형 온도 및 사출 속도가 반고체 다이캐스팅의 충전 공정 성능에 미치는 영향을 연구했습니다. 직교 테스트 분석을 기반으로 금속 주입 온도 590°C, 금형 온도 260°C 및 사출 속도 0.5m/s인 최적의 다이 캐스팅 공정 매개변수가 선택되었습니다. Swirled Enthalpy Equilibration Device(SEED)의 반고체 슬러리 제조 공정을 다이캐스팅 생산 실험에 사용하였다. 알루미늄 합금 반고체 브래킷 구성 요소는 시뮬레이션 결과와 일치하는 주요 다이 캐스팅 공정 매개변수를 선택하여 성공적으로 생산되었습니다. 반고체 게이팅 시스템의 설계는 주조의 다른 영역의 미세 구조를 관찰하고 분석하여 추가로 검증되었습니다. 생산된 반고체 주조물의 특성 매개변수, 입자 크기 및 미세 구조의 형상 계수는 반고체 알루미늄 합금 부품의 품질이 양호함을 보여주었습니다.

Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process
Gating System Design Based on Numerical Simulation and Production Experiment Verification of Aluminum Alloy Bracket Fabricated by Semi-solid Rheo-Die Casting Process

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Keywords

  • semi-solid rheo-die casting
  • gating system
  • process parameters
  • numerical simulation
  • microstructure
Figure 2. Schematic diagram for pilot-scale cooling-water circulation system (a) along with a real picture of the system (b).

Application of Computational Fluid Dynamics in Chlorine-Dynamics Modeling of In-Situ Chlorination Systems for Cooling Systems

Jongchan Yi 1, Jonghun Lee 1, Mohd Amiruddin Fikri 2,3, Byoung-In Sang 4 and Hyunook Kim 1,*

Abstract

염소화는 상대적인 효율성과 저렴한 비용으로 인해 발전소 냉각 시스템에서 생물학적 오염을 제어하는​​데 선호되는 방법입니다. 해안 지역에 발전소가 있는 경우 바닷물을 사용하여 현장에서 염소를 전기화학적으로 생성할 수 있습니다. 이를 현장 전기염소화라고 합니다. 이 접근 방식은 유해한 염소화 부산물이 적고 염소를 저장할 필요가 없다는 점을 포함하여 몇 가지 장점이 있습니다. 그럼에도 불구하고, 이 전기화학적 공정은 실제로는 아직 초기 단계에 있습니다. 이 연구에서는 파일럿 규모 냉각 시스템에서 염소 붕괴를 시뮬레이션하기 위해 병렬 1차 동역학을 적용했습니다. 붕괴가 취수관을 따라 발생하기 때문에 동역학은 전산유체역학(CFD) 코드에 통합되었으며, 이후에 파이프의 염소 거동을 시뮬레이션하는데 적용되었습니다. 실험과 시뮬레이션 데이터는 강한 난류가 형성되는 조건하에서도 파이프 벽을 따라 염소 농도가 점진적인 것으로 나타났습니다. 염소가 중간보다 파이프 표면을 따라 훨씬 더 집중적으로 남아 있다는 사실은 전기 염소화를 기반으로 하는 시스템의 전체 염소 요구량을 감소시킬 수 있었습니다. 현장 전기 염소화 방식의 냉각 시스템은 직접 주입 방식에 필요한 염소 사용량의 1/3만 소비했습니다. 따라서 현장 전기염소화는 해안 지역의 발전소에서 바이오파울링 제어를 위한 비용 효율적이고 환경 친화적인 접근 방식으로 사용될 수 있다고 결론지었습니다.

Chlorination is the preferred method to control biofouling in a power plant cooling system due to its comparative effectiveness and low cost. If a power plant is located in a coastal area, chlorine can be electrochemically generated in-situ using seawater, which is called in-situ electrochlorination; this approach has several advantages including fewer harmful chlorination byproducts and no need for chlorine storage. Nonetheless, this electrochemical process is still in its infancy in practice. In this study, a parallel first-order kinetics was applied to simulate chlorine decay in a pilot-scale cooling system. Since the decay occurs along the water-intake pipe, the kinetics was incorporated into computational fluid dynamics (CFD) codes, which were subsequently applied to simulate chlorine behavior in the pipe. The experiment and the simulation data indicated that chlorine concentrations along the pipe wall were incremental, even under the condition where a strong turbulent flow was formed. The fact that chlorine remained much more concentrated along the pipe surface than in the middle allowed for the reduction of the overall chlorine demand of the system based on the electro-chlorination. The cooling system, with an in-situ electro-chlorination, consumed only 1/3 of the chlorine dose demanded by the direct injection method. Therefore, it was concluded that in-situ electro-chlorination could serve as a cost-effective and environmentally friendly approach for biofouling control at power plants on coastal areas.

Keywords

computational fluid dynamics; power plant; cooling system; electro-chlorination; insitu chlorination

Figure 1. Electrodes and batch experiment set-up. (a) Two cylindrical electrodes used in this study. (b) Batch experiment set-up for kinetic tests.
Figure 1. Electrodes and batch experiment set-up. (a) Two cylindrical electrodes used in this study. (b) Batch experiment set-up for kinetic tests.
Figure 2. Schematic diagram for pilot-scale cooling-water circulation system (a) along with a real picture of the system (b).
Figure 2. Schematic diagram for pilot-scale cooling-water circulation system (a) along with a real picture of the system (b).
Figure 3. Free chlorine decay curves in seawater with different TOC and initial chlorine concentration. Each line represents the predicted concentration of chlorine under a given condition. (a) Artificial seawater solution with 1 mg L−1 of TOC; (b) artificial seawater solution with 2 mg L−1 of TOC; (c) artificial seawater solution with 3 mg L−1 of TOC; (d) West Sea water (1.3 mg L−1 of TOC).
Figure 3. Free chlorine decay curves in seawater with different TOC and initial chlorine concentration. Each line represents the predicted concentration of chlorine under a given condition. (a) Artificial seawater solution with 1 mg L−1 of TOC; (b) artificial seawater solution with 2 mg L−1 of TOC; (c) artificial seawater solution with 3 mg L−1 of TOC; (d) West Sea water (1.3 mg L−1 of TOC).
Figure 4. Correlation between model and experimental data in the chlorine kinetics using seawater.
Figure 4. Correlation between model and experimental data in the chlorine kinetics using seawater.
Figure 5. Free chlorine concentrations in West Sea water under different current conditions in an insitu electro-chlorination system.
Figure 5. Free chlorine concentrations in West Sea water under different current conditions in an insitu electro-chlorination system.
Figure 6. Free chlorine distribution along the sampling ports under different flow rates. Each dot represents experimental data, and each point on the black line is the expected chlorine concentration obtained from computational fluid dynamics (CFD) simulation with a parallel first-order decay model. The red-dotted line is the desirable concentration at the given flow rate: (a) 600 L min−1 of flow rate, (b) 700 L min−1 of flow rate, (c) 800 L min−1 of flow rate, (d) 900 L min−1 of flow rate.
Figure 6. Free chlorine distribution along the sampling ports under different flow rates. Each dot represents experimental data, and each point on the black line is the expected chlorine concentration obtained from computational fluid dynamics (CFD) simulation with a parallel first-order decay model. The red-dotted line is the desirable concentration at the given flow rate: (a) 600 L min−1 of flow rate, (b) 700 L min−1 of flow rate, (c) 800 L min−1 of flow rate, (d) 900 L min−1 of flow rate.
Figure 7. Fluid contour images from CFD simulation of the electro-chlorination experiment. Inlet flow rate is 800 L min−1. Outlet pressure was set to 10.8 kPa. (a) Chlorine concentration; (b) expanded view of electrode side in image (a); (c) velocity magnitude; (d) pressure.
Figure 7. Fluid contour images from CFD simulation of the electro-chlorination experiment. Inlet flow rate is 800 L min−1. Outlet pressure was set to 10.8 kPa. (a) Chlorine concentration; (b) expanded view of electrode side in image (a); (c) velocity magnitude; (d) pressure.
Figure 8. Chlorine concentration contour in the simulation of full-scale in-situ electro-chlorination with different cathode positions. The pipe diameter is 2 m and the flow rate is 14 m3 s−1. The figure shows 10 m of the pipeline. (a) The simulation result when the cathode is placed on the surface of the pipe wall. (b) The simulation result when the cathode is placed on the inside of the pipe with 100 mm of distance from the pipe wall.
Figure 8. Chlorine concentration contour in the simulation of full-scale in-situ electro-chlorination with different cathode positions. The pipe diameter is 2 m and the flow rate is 14 m3 s−1. The figure shows 10 m of the pipeline. (a) The simulation result when the cathode is placed on the surface of the pipe wall. (b) The simulation result when the cathode is placed on the inside of the pipe with 100 mm of distance from the pipe wall.
Figure 9. Comparison of in-situ electro-chlorination and direct chlorine injection in full-scale applications. (a) Estimated chlorine concentrations along the pipe surface. (b) Relative chlorine demands.
Figure 9. Comparison of in-situ electro-chlorination and direct chlorine injection in full-scale applications. (a) Estimated chlorine concentrations along the pipe surface. (b) Relative chlorine demands.

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Fig. 1. A typical Boiling Water Reactor (BWR) and selected segment of study for simulation

Understanding dry-out mechanism in rod bundles of boiling water reactor

끓는 물 원자로 봉 다발의 건조 메커니즘 이해

Liril D.SilviaDinesh K.ChandrakercSumanaGhoshaArup KDasb
aDepartment of Chemical Engineering, Indian Institute of Technology, Roorkee, India
bDepartment of Mechanical Engineering, Indian Institute of Technology, Roorkee, India
cReactor Engineering Division, Bhabha Atomic Research Centre, Mumbai, India

Abstract

Present work reports numerical understanding of interfacial dynamics during co-flow of vapor and liquid phases of water inside a typical Boiling Water Reactor (BWR), consisting of a nuclear fuel rod bundle assembly of 7 pins in a circular array. Two representative spacings between rods in a circular array are used to carry out the simulation. In literature, flow boiling in a nuclear reactor is dealt with mechanistic models or averaged equations. Hence, in the present study using the Volume of Fluid (VOF) based multiphase model, a detailed numerical understanding of breaking and making in interfaces during flow boiling in BWR is targeted. Our work will portray near realistic vapor bubble and liquid flow dynamics in rod bundle scenario. Constant wall heat flux for fuel rod and uniform velocity of the liquid at the inlet patch is applied as a boundary condition. The saturation properties of water are taken at 30 bar pressure. Flow boiling stages involving bubble nucleation, growth, merging, local dry-out, rewetting with liquid patches, and complete dry-out are illustrated. The dry-out phenomenon with no liquid presence is numerically observed with phase fraction contours at various axial cut-sections. The quantification of the liquid phase fraction at different axial planes is plotted over time, emphasizing the progressive dry-out mechanism. A comparison of liquid-vapor distribution for inner and outer rods reveals that the inner rod’s dry-out occurs sooner than that of the outer rod. The heat transfer coefficient to identify the heat dissipation capacity of each case is also reported.

현재 작업은 원형 배열에 있는 7개의 핀으로 구성된 핵연료봉 다발 어셈블리로 구성된 일반적인 끓는 물 원자로(BWR) 내부의 물의 증기 및 액체상의 동시 흐름 동안 계면 역학에 대한 수치적 이해를 보고합니다.

원형 배열의 막대 사이에 두 개의 대표적인 간격이 시뮬레이션을 수행하는 데 사용됩니다. 문헌에서 원자로의 유동 비등은 기계론적 모델 또는 평균 방정식으로 처리됩니다.

따라서 VOF(Volume of Fluid) 기반 다상 모델을 사용하는 본 연구에서는 BWR에서 유동 비등 동안 계면의 파괴 및 생성에 대한 자세한 수치적 이해를 목표로 합니다.

우리의 작업은 막대 번들 시나리오에서 거의 사실적인 증기 기포 및 액체 흐름 역학을 묘사합니다. 연료봉에 대한 일정한 벽 열유속과 입구 패치에서 액체의 균일한 속도가 경계 조건으로 적용됩니다. 물의 포화 특성은 30bar 압력에서 취합니다.

기포 핵 생성, 성장, 병합, 국소 건조, 액체 패치로 재습윤 및 완전한 건조를 포함하는 유동 비등 단계가 설명됩니다. 액체가 존재하지 않는 건조 현상은 다양한 축 단면에서 위상 분율 윤곽으로 수치적으로 관찰됩니다.

다른 축 평면에서 액상 분율의 정량화는 점진적인 건조 메커니즘을 강조하면서 시간이 지남에 따라 표시됩니다. 내부 막대와 외부 막대의 액-증기 분포를 비교하면 내부 막대의 건조가 외부 막대보다 더 빨리 발생함을 알 수 있습니다. 각 경우의 방열 용량을 식별하기 위한 열 전달 계수도 보고됩니다.

Fig. 1. A typical Boiling Water Reactor (BWR) and selected segment of study for simulation
Fig. 1. A typical Boiling Water Reactor (BWR) and selected segment of study for simulation
Fig. 2. (a-c) dimensions and mesh configuration for G = 6 mm; (d-f) dimensions and mesh configuration for G = 0.6 mm
Fig. 2. (a-c) dimensions and mesh configuration for G = 6 mm; (d-f) dimensions and mesh configuration for G = 0.6 mm
Fig. 3. Simulating the effect of spacer (a) Spacer configuration around rod bundle (b) Mesh structure in spacer zone (c) Distribution of vapor bubbles in a rod bundle with spacer (d) Liquid phase fraction comparison for geometry with and without spacer (e,f,g) Wall temperature comparison for geometry with and without spacer; WS: With Spacer, WOS: Without Spacer; Temperature in the y-axis is in (f) and (g) is same as (e).
Fig. 3. Simulating the effect of spacer (a) Spacer configuration around rod bundle (b) Mesh structure in spacer zone (c) Distribution of vapor bubbles in a rod bundle with spacer (d) Liquid phase fraction comparison for geometry with and without spacer (e,f,g) Wall temperature comparison for geometry with and without spacer; WS: With Spacer, WOS: Without Spacer; Temperature in the y-axis is in (f) and (g) is same as (e).
Fig. 4. Validation of the present numerical model with crossflow boiling over a heated cylindrical rod [40]
Fig. 4. Validation of the present numerical model with crossflow boiling over a heated cylindrical rod [40]
Fig. 5. Grid-Independent study in terms of vapor volume in 1/4th of computational domain
Fig. 5. Grid-Independent study in terms of vapor volume in 1/4th of computational domain
Fig. 6. Interface contour for G = 6 mm; ul = 1.2 m/s; q˙ w = 396 kW/m2; they are showing nucleation, growth, merging, and pseudo-steady-state condition.
Fig. 6. Interface contour for G = 6 mm; ul = 1.2 m/s; q˙ w = 396 kW/m2; they are showing nucleation, growth, merging, and pseudo-steady-state condition.
Fig. 7. Interface contours for G = 0.6 mm; ul = 1.2 m/s; q˙ w = 396 kW/m2; It shows dry-out at pseudo-steady-state near the exit
Fig. 7. Interface contours for G = 0.6 mm; ul = 1.2 m/s; q˙ w = 396 kW/m2; It shows dry-out at pseudo-steady-state near the exit
Fig. 8. Vapor-liquid distribution across various distant cross-sections (Black color indicates liquid; Gray color indicates vapor); Magnification factor: 1 × (for a and b), 1.5 × (for c and d)
Fig. 8. Vapor-liquid distribution across various distant cross-sections (Black color indicates liquid; Gray color indicates vapor); Magnification factor: 1 × (for a and b), 1.5 × (for c and d)
Fig. 21. Two-phase flow mixture velocity (u¯z); for G = 6 mm, r = 5 means location at inner heated wall and r = 25 means location at outer adiabatic wall; for G = 0.66 mm, r = 5 means location at inner heated wall and r = 16.6 mm means location at outer adiabatic wall.
Fig. 21. Two-phase flow mixture velocity (u¯z); for G = 6 mm, r = 5 means location at inner heated wall and r = 25 means location at outer adiabatic wall; for G = 0.66 mm, r = 5 means location at inner heated wall and r = 16.6 mm means location at outer adiabatic wall.

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Figure 3 Simulation PTC pipes enhanced with copper foam and nanoparticles in FLOW-3D software.

다공성 미디어 및 나노유체에 의해 강화된 수집기로 태양광 CCHP 시스템의 최적화

Optimization of Solar CCHP Systems with Collector Enhanced by Porous Media and Nanofluid


Navid Tonekaboni,1Mahdi Feizbahr,2 Nima Tonekaboni,1Guang-Jun Jiang,3,4 and Hong-Xia Chen3,4

Abstract

태양열 집열기의 낮은 효율은 CCHP(Solar Combined Cooling, Heating, and Power) 사이클의 문제점 중 하나로 언급될 수 있습니다. 태양계를 개선하기 위해 나노유체와 다공성 매체가 태양열 집열기에 사용됩니다.

다공성 매질과 나노입자를 사용하는 장점 중 하나는 동일한 조건에서 더 많은 에너지를 흡수할 수 있다는 것입니다. 이 연구에서는 평균 일사량이 1b인 따뜻하고 건조한 지역의 600 m2 건물의 전기, 냉방 및 난방을 생성하기 위해 다공성 매질과 나노유체를 사용하여 태양열 냉난방 복합 발전(SCCHP) 시스템을 최적화했습니다.

본 논문에서는 침전물이 형성되지 않는 lb = 820 w/m2(이란) 정도까지 다공성 물질에서 나노유체의 최적량을 계산하였다. 이 연구에서 태양열 집열기는 구리 다공성 매체(95% 다공성)와 CuO 및 Al2O3 나노 유체로 향상되었습니다.

나노유체의 0.1%-0.6%가 작동 유체로 물에 추가되었습니다. 나노유체의 0.5%가 태양열 집열기 및 SCCHP 시스템에서 가장 높은 에너지 및 엑서지 효율 향상으로 이어지는 것으로 밝혀졌습니다.

본 연구에서 포물선형 집열기(PTC)의 최대 에너지 및 엑서지 효율은 각각 74.19% 및 32.6%입니다. 그림 1은 태양 CCHP의 주기를 정확하게 설명하기 위한 그래픽 초록으로 언급될 수 있습니다.

The low efficiency of solar collectors can be mentioned as one of the problems in solar combined cooling, heating, and power (CCHP) cycles. For improving solar systems, nanofluid and porous media are used in solar collectors. One of the advantages of using porous media and nanoparticles is to absorb more energy under the same conditions. In this research, a solar combined cooling, heating, and power (SCCHP) system has been optimized by porous media and nanofluid for generating electricity, cooling, and heating of a 600 m2 building in a warm and dry region with average solar radiation of Ib = 820 w/m2 in Iran. In this paper, the optimal amount of nanofluid in porous materials has been calculated to the extent that no sediment is formed. In this study, solar collectors were enhanced with copper porous media (95% porosity) and CuO and Al2O3 nanofluids. 0.1%–0.6% of the nanofluids were added to water as working fluids; it is found that 0.5% of the nanofluids lead to the highest energy and exergy efficiency enhancement in solar collectors and SCCHP systems. Maximum energy and exergy efficiency of parabolic thermal collector (PTC) riches in this study are 74.19% and 32.6%, respectively. Figure 1 can be mentioned as a graphical abstract for accurately describing the cycle of solar CCHP.

1. Introduction

Due to the increase in energy consumption, the use of clean energy is one of the important goals of human societies. In the last four decades, the use of cogeneration cycles has increased significantly due to high efficiency. Among clean energy, the use of solar energy has become more popular due to its greater availability [1]. Low efficiency of energy production, transmission, and distribution system makes a new system to generate simultaneously electricity, heating, and cooling as an essential solution to be widely used. The low efficiency of the electricity generation, transmission, and distribution system makes the CCHP system a basic solution to eliminate waste of energy. CCHP system consists of a prime mover (PM), a power generator, a heat recovery system (produce extra heating/cooling/power), and thermal energy storage (TES) [2]. Solar combined cooling, heating, and power (SCCHP) has been started three decades ago. SCCHP is a system that receives its propulsive force from solar energy; in this cycle, solar collectors play the role of propulsive for generating power in this system [3].

Increasing the rate of energy consumption in the whole world because of the low efficiency of energy production, transmission, and distribution system causes a new cogeneration system to generate electricity, heating, and cooling energy as an essential solution to be widely used. Building energy utilization fundamentally includes power required for lighting, home electrical appliances, warming and cooling of building inside, and boiling water. Domestic usage contributes to an average of 35% of the world’s total energy consumption [4].

Due to the availability of solar energy in all areas, solar collectors can be used to obtain the propulsive power required for the CCHP cycle. Solar energy is the main source of energy in renewable applications. For selecting a suitable area to use solar collectors, annual sunshine hours, the number of sunny days, minus temperature and frosty days, and the windy status of the region are essentially considered [5]. Iran, with an average of more than 300 sunny days, is one of the suitable countries to use solar energy. Due to the fact that most of the solar radiation is in the southern regions of Iran, also the concentration of cities is low in these areas, and transmission lines are far apart, one of the best options is to use CCHP cycles based on solar collectors [6]. One of the major problems of solar collectors is their low efficiency [7]. Low efficiency increases the area of collectors, which increases the initial cost of solar systems and of course increases the initial payback period. To increase the efficiency of solar collectors and improve their performance, porous materials and nanofluids are used to increase their workability.

There are two ways to increase the efficiency of solar collectors and mechanical and fluid improvement. In the first method, using porous materials or helical filaments inside the collector pipes causes turbulence of the flow and increases heat transfer. In the second method, using nanofluids or salt and other materials increases the heat transfer of water. The use of porous materials has grown up immensely over the past twenty years. Porous materials, especially copper porous foam, are widely used in solar collectors. Due to the high contact surface area, porous media are appropriate candidates for solar collectors [8]. A number of researchers investigated Solar System performance in accordance with energy and exergy analyses. Zhai et al. [9] reviewed the performance of a small solar-powered system in which the energy efficiency was 44.7% and the electrical efficiency was 16.9%.

Abbasi et al. [10] proposed an innovative multiobjective optimization to optimize the design of a cogeneration system. Results showed the CCHP system based on an internal diesel combustion engine was the applicable alternative at all regions with different climates. The diesel engine can supply the electrical requirement of 31.0% and heating demand of 3.8% for building.

Jiang et al. [11] combined the experiment and simulation together to analyze the performance of a cogeneration system. Moreover, some research focused on CCHP systems using solar energy. It integrated sustainable and renewable technologies in the CCHP, like PV, Stirling engine, and parabolic trough collector (PTC) [21215].

Wang et al. [16] optimized a cogeneration solar cooling system with a Rankine cycle and ejector to reach the maximum total system efficiency of 55.9%. Jing et al. analyzed a big-scale building with the SCCHP system and auxiliary heaters to produced electrical, cooling, and heating power. The maximum energy efficiency reported in their work is 46.6% [17]. Various optimization methods have been used to improve the cogeneration system, minimum system size, and performance, such as genetic algorithm [1819].

Hirasawa et al. [20] investigated the effect of using porous media to reduce thermal waste in solar systems. They used the high-porosity metal foam on top of the flat plate solar collector and observed that thermal waste decreased by 7% due to natural heat transfer. Many researchers study the efficiency improvement of the solar collector by changing the collector’s shapes or working fluids. However, the most effective method is the use of nanofluids in the solar collector as working fluid [21]. In the experimental study done by Jouybari et al. [22], the efficiency enhancement up to 8.1% was achieved by adding nanofluid in a flat plate collector. In this research, by adding porous materials to the solar collector, collector efficiency increased up to 92% in a low flow regime. Subramani et al. [23] analyzed the thermal performance of the parabolic solar collector with Al2O3 nanofluid. They conducted their experiments with Reynolds number range 2401 to 7202 and mass flow rate 0.0083 to 0.05 kg/s. The maximum efficiency improvement in this experiment was 56% at 0.05 kg/s mass flow rate.

Shojaeizadeh et al. [24] investigated the analysis of the second law of thermodynamic on the flat plate solar collector using Al2O3/water nanofluid. Their research showed that energy efficiency rose up to 1.9% and the exergy efficiency increased by a maximum of 0.72% compared to pure water. Tiwari et al. [25] researched on the thermal performance of solar flat plate collectors for working fluid water with different nanofluids. The result showed that using 1.5% (optimum) particle volume fraction of Al2O3 nanofluid as an absorbing medium causes the thermal efficiency to enhance up to 31.64%.

The effect of porous media and nanofluids on solar collectors has already been investigated in the literature but the SCCHP system with a collector embedded by both porous media and nanofluid for enhancing the ratio of nanoparticle in nanofluid for preventing sedimentation was not discussed. In this research, the amount of energy and exergy of the solar CCHP cycles with parabolic solar collectors in both base and improved modes with a porous material (copper foam with 95% porosity) and nanofluid with different ratios of nanoparticles was calculated. In the first step, it is planned to design a CCHP system based on the required load, and, in the next step, it will analyze the energy and exergy of the system in a basic and optimize mode. In the optimize mode, enhanced solar collectors with porous material and nanofluid in different ratios (0.1%–0.7%) were used to optimize the ratio of nanofluids to prevent sedimentation.

2. Cycle Description

CCHP is one of the methods to enhance energy efficiency and reduce energy loss and costs. The SCCHP system used a solar collector as a prime mover of the cogeneration system and assisted the boiler to generate vapor for the turbine. Hot water flows from the expander to the absorption chiller in summer or to the radiator or fan coil in winter. Finally, before the hot water wants to flow back to the storage tank, it flows inside a heat exchanger for generating domestic hot water [26].

For designing of solar cogeneration system and its analysis, it is necessary to calculate the electrical, heating (heating load is the load required for the production of warm water and space heating), and cooling load required for the case study considered in a residential building with an area of 600 m2 in the warm region of Iran (Zahedan). In Table 1, the average of the required loads is shown for the different months of a year (average of electrical, heating, and cooling load calculated with CARRIER software).Table 1 The average amount of electric charges, heating load, and cooling load used in the different months of the year in the city of Zahedan for a residential building with 600 m2.

According to Table 1, the maximum magnitude of heating, cooling, and electrical loads is used to calculate the cogeneration system. The maximum electric load is 96 kW, the maximum amount of heating load is 62 kW, and the maximum cooling load is 118 kW. Since the calculated loads are average, all loads increased up to 10% for the confidence coefficient. With the obtained values, the solar collector area and other cogeneration system components are calculated. The cogeneration cycle is capable of producing 105 kW electric power, 140 kW cooling capacity, and 100 kW heating power.

2.1. System Analysis Equations

An analysis is done by considering the following assumptions:(1)The system operates under steady-state conditions(2)The system is designed for the warm region of Iran (Zahedan) with average solar radiation Ib = 820 w/m2(3)The pressure drops in heat exchangers, separators, storage tanks, and pipes are ignored(4)The pressure drop is negligible in all processes and no expectable chemical reactions occurred in the processes(5)Potential, kinetic, and chemical exergy are not considered due to their insignificance(6)Pumps have been discontinued due to insignificance throughout the process(7)All components are assumed adiabatic

Schematic shape of the cogeneration cycle is shown in Figure 1 and all data are given in Table 2.

Figure 1 Schematic shape of the cogeneration cycle.Table 2 Temperature and humidity of different points of system.

Based on the first law of thermodynamic, energy analysis is based on the following steps.

First of all, the estimated solar radiation energy on collector has been calculated:where α is the heat transfer enhancement coefficient based on porous materials added to the collector’s pipes. The coefficient α is increased by the porosity percentage, the type of porous material (in this case, copper with a porosity percentage of 95), and the flow of fluid to the collector equation.

Collector efficiency is going to be calculated by the following equation [9]:

Total energy received by the collector is given by [9]

Also, the auxiliary boiler heat load is [2]

Energy consumed from vapor to expander is calculated by [2]

The power output form by the screw expander [9]:

The efficiency of the expander is 80% in this case [11].

In this step, cooling and heating loads were calculated and then, the required heating load to reach sanitary hot water will be calculated as follows:

First step: calculating the cooling load with the following equation [9]:

Second step: calculating heating loads [9]:

Then, calculating the required loud for sanitary hot water will be [9]

According to the above-mentioned equations, efficiency is [9]

In the third step, calculated exergy analysis as follows.

First, the received exergy collector from the sun is calculated [9]:

In the previous equation, f is the constant of air dilution.

The received exergy from the collector is [9]

In the case of using natural gas in an auxiliary heater, the gas exergy is calculated from the following equation [12]:

Delivering exergy from vapor to expander is calculated with the following equation [9]:

In the fourth step, the exergy in cooling and heating is calculated by the following equation:

Cooling exergy in summer is calculated [9]:

Heating exergy in winter is calculated [9]:

In the last step based on thermodynamic second law, exergy efficiency has been calculated from the following equation and the above-mentioned calculated loads [9]:

3. Porous Media

The porous medium that filled the test section is copper foam with a porosity of 95%. The foams are determined in Figure 2 and also detailed thermophysical parameters and dimensions are shown in Table 3.

Figure 2 Copper foam with a porosity of 95%.Table 3 Thermophysical parameters and dimensions of copper foam.

In solar collectors, copper porous materials are suitable for use at low temperatures and have an easier and faster manufacturing process than ceramic porous materials. Due to the high coefficient conductivity of copper, the use of copper metallic foam to increase heat transfer is certainly more efficient in solar collectors.

Porous media and nanofluid in solar collector’s pipes were simulated in FLOW-3D software using the finite-difference method [27]. Nanoparticles Al2O3 and CUO are mostly used in solar collector enhancement. In this research, different concentrations of nanofluid are added to the parabolic solar collectors with porous materials (copper foam with porosity of 95%) to achieve maximum heat transfer in the porous materials before sedimentation. After analyzing PTC pipes with the nanofluid flow in FLOW-3D software, for energy and exergy efficiency analysis, Carrier software results were used as EES software input. Simulation PTC with porous media inside collector pipe and nanofluids sedimentation is shown in Figure 3.

Figure 3 Simulation PTC pipes enhanced with copper foam and nanoparticles in FLOW-3D software.

3.1. Nano Fluid

In this research, copper and silver nanofluids (Al2O3, CuO) have been added with percentages of 0.1%–0.7% as the working fluids. The nanoparticle properties are given in Table 4. Also, system constant parameters are presented in Table 4, which are available as default input in the EES software.Table 4 Properties of the nanoparticles [9].

System constant parameters for input in the software are shown in Table 5.Table 5 System constant parameters.

The thermal properties of the nanofluid can be obtained from equations (18)–(21). The basic fluid properties are indicated by the index (bf) and the properties of the nanoparticle silver with the index (np).

The density of the mixture is shown in the following equation [28]:where ρ is density and ϕ is the nanoparticles volume fraction.

The specific heat capacity is calculated from the following equation [29]:

The thermal conductivity of the nanofluid is calculated from the following equation [29]:

The parameter β is the ratio of the nanolayer thickness to the original particle radius and, usually, this parameter is taken equal to 0.1 for the calculated thermal conductivity of the nanofluids.

The mixture viscosity is calculated as follows [30]:

In all equations, instead of water properties, working fluids with nanofluid are used. All of the above equations and parameters are entered in the EES software for calculating the energy and exergy of solar collectors and the SCCHP cycle. All calculation repeats for both nanofluids with different concentrations of nanofluid in the solar collector’s pipe.

4. Results and Discussion

In the present study, relations were written according to Wang et al. [16] and the system analysis was performed to ensure the correctness of the code. The energy and exergy charts are plotted based on the main values of the paper and are shown in Figures 4 and 5. The error rate in this simulation is 1.07%.

Figure 4 Verification charts of energy analysis results.

Figure 5 Verification charts of exergy analysis results.

We may also investigate the application of machine learning paradigms [3141] and various hybrid, advanced optimization approaches that are enhanced in terms of exploration and intensification [4255], and intelligent model studies [5661] as well, for example, methods such as particle swarm optimizer (PSO) [6062], differential search (DS) [63], ant colony optimizer (ACO) [616465], Harris hawks optimizer (HHO) [66], grey wolf optimizer (GWO) [5367], differential evolution (DE) [6869], and other fusion and boosted systems [4146485054557071].

At the first step, the collector is modified with porous copper foam material. 14 cases have been considered for the analysis of the SCCHP system (Table 6). It should be noted that the adding of porous media causes an additional pressure drop inside the collector [922263072]. All fourteen cases use copper foam with a porosity of 95 percent. To simulate the effect of porous materials and nanofluids, the first solar PTC pipes have been simulated in the FLOW-3D software and then porous media (copper foam with porosity of 95%) and fluid flow with nanoparticles (AL2O3 and CUO) are generated in the software. After analyzing PTC pipes in FLOW-3D software, for analyzing energy and exergy efficiency, software outputs were used as EES software input for optimization ratio of sedimentation and calculating energy and exergy analyses.Table 6 Collectors with different percentages of nanofluids and porous media.

In this research, an enhanced solar collector with both porous media and Nanofluid is investigated. In the present study, 0.1–0.5% CuO and Al2O3 concentration were added to the collector fully filled by porous media to achieve maximum energy and exergy efficiencies of solar CCHP systems. All steps of the investigation are shown in Table 6.

Energy and exergy analyses of parabolic solar collectors and SCCHP systems are shown in Figures 6 and 7.

Figure 6 Energy and exergy efficiencies of the PTC with porous media and nanofluid.

Figure 7 Energy and exergy efficiency of the SCCHP.

Results show that the highest energy and exergy efficiencies are 74.19% and 32.6%, respectively, that is achieved in Step 12 (parabolic collectors with filled porous media and 0.5% Al2O3). In the second step, the maximum energy efficiency of SCCHP systems with fourteen steps of simulation are shown in Figure 7.

In the second step, where 0.1, −0.6% of the nanofluids were added, it is found that 0.5% leads to the highest energy and exergy efficiency enhancement in solar collectors and SCCHP systems. Using concentrations more than 0.5% leads to sediment in the solar collector’s pipe and a decrease of porosity in the pipe [73]. According to Figure 7, maximum energy and exergy efficiencies of SCCHP are achieved in Step 12. In this step energy efficiency is 54.49% and exergy efficiency is 18.29%. In steps 13 and 14, with increasing concentration of CUO and Al2O3 nanofluid solution in porous materials, decreasing of energy and exergy efficiency of PTC and SCCHP system at the same time happened. This decrease in efficiency is due to the formation of sediment in the porous material. Calculations and simulations have shown that porous materials more than 0.5% nanofluids inside the collector pipe cause sediment and disturb the porosity of porous materials and pressure drop and reduce the coefficient of performance of the cogeneration system. Most experience showed that CUO and AL2O3 nanofluids with less than 0.6% percent solution are used in the investigation on the solar collectors at low temperatures and discharges [74]. One of the important points of this research is that the best ratio of nanofluids in the solar collector with a low temperature is 0.5% (AL2O3 and CUO); with this replacement, the cost of solar collectors and SCCHP cycle is reduced.

5. Conclusion and Future Directions

In the present study, ways for increasing the efficiency of solar collectors in order to enhance the efficiency of the SCCHP cycle are examined. The research is aimed at adding both porous materials and nanofluids for estimating the best ratio of nanofluid for enhanced solar collector and protecting sedimentation in porous media. By adding porous materials (copper foam with porosity of 95%) and 0.5% nanofluids together, high efficiency in solar parabolic collectors can be achieved. The novelty in this research is the addition of both nanofluids and porous materials and calculating the best ratio for preventing sedimentation and pressure drop in solar collector’s pipe. In this study, it was observed that, by adding 0.5% of AL2O3 nanofluid in working fluids, the energy efficiency of PTC rises to 74.19% and exergy efficiency is grown up to 32.6%. In SCCHP cycle, energy efficiency is 54.49% and exergy efficiency is 18.29%.

In this research, parabolic solar collectors fully filled by porous media (copper foam with a porosity of 95) are investigated. In the next step, parabolic solar collectors in the SCCHP cycle were simultaneously filled by porous media and different percentages of Al2O3 and CuO nanofluid. At this step, values of 0.1% to 0.6% of each nanofluid were added to the working fluid, and the efficiency of the energy and exergy of the collectors and the SCCHP cycle were determined. In this case, nanofluid and the porous media were used together in the solar collector and maximum efficiency achieved. 0.5% of both nanofluids were used to achieve the biggest efficiency enhancement.

In the present study, as expected, the highest efficiency is for the parabolic solar collector fully filled by porous material (copper foam with a porosity of 95%) and 0.5% Al2O3. Results of the present study are as follows:(1)The average enhancement of collectors’ efficiency using porous media and nanofluids is 28%.(2)Solutions with 0.1 to 0.5% of nanofluids (CuO and Al2O3) are used to prevent collectors from sediment occurrence in porous media.(3)Collector of solar cogeneration cycles that is enhanced by both porous media and nanofluid has higher efficiency, and the stability of output temperature is more as well.(4)By using 0.6% of the nanofluids in the enhanced parabolic solar collectors with copper porous materials, sedimentation occurs and makes a high-pressure drop in the solar collector’s pipe which causes decrease in energy efficiency.(5)Average enhancement of SCCHP cycle efficiency is enhanced by both porous media and nanofluid 13%.

Nomenclature

:Solar radiation
a:Heat transfer augmentation coefficient
A:Solar collector area
Bf:Basic fluid
:Specific heat capacity of the nanofluid
F:Constant of air dilution
:Thermal conductivity of the nanofluid
:Thermal conductivity of the basic fluid
:Viscosity of the nanofluid
:Viscosity of the basic fluid
:Collector efficiency
:Collector energy receives
:Auxiliary boiler heat
:Expander energy
:Gas energy
:Screw expander work
:Cooling load, in kilowatts
:Heating load, in kilowatts
:Solar radiation energy on collector, in Joule
:Sanitary hot water load
Np:Nanoparticle
:Energy efficiency
:Heat exchanger efficiency
:Sun exergy
:Collector exergy
:Natural gas exergy
:Expander exergy
:Cooling exergy
:Heating exergy
:Exergy efficiency
:Steam mass flow rate
:Hot water mass flow rate
:Specific heat capacity of water
:Power output form by the screw expander
Tam:Average ambient temperature
:Density of the mixture.

Greek symbols

ρ:Density
ϕ:Nanoparticles volume fraction
β:Ratio of the nanolayer thickness.

Abbreviations

CCHP:Combined cooling, heating, and power
EES:Engineering equation solver.

Data Availability

For this study, data were generated by CARRIER software for the average electrical, heating, and cooling load of a residential building with 600 m2 in the city of Zahedan, Iran.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

Acknowledgments

This work was partially supported by the National Natural Science Foundation of China under Contract no. 71761030 and Natural Science Foundation of Inner Mongolia under Contract no. 2019LH07003.

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Energy and exergy analysis of an enhanced solar CCHP system with a collector embedded by porous media and nano fluid

Energy and exergy analysis of an enhanced solar CCHP system with a collector embedded by porous media and nano fluid

Year 2021, Volume 7, Issue 6, 1489 – 1505, 02.09.2021

N. TONEKABONI  H. SALARIAN  M. Eshagh NIMVARI  J. KHALEGHINIA https://doi.org/10.18186/thermal.990897

Abstract

The low efficiency of Collectors that absorb energy can be mentioned as one of the drawbacks in solar cogeneration cycles. In the present study, solar systems have been improved by adding porous media and Nanofluid to collectors. One advantage of using porous media and nanomaterials is to absorb more energy while the surface area is reduced. In this study, first, solar collectors are enhanced using 90% porosity copper in solar combined cooling, heating and power systems (SCCHP). Second, different percentages of CuO and Al2O3 nano-fluids are added to a flat plate and parabolic collectors to enhance thermal properties. Simulations are performed in different modes (simple parabolic collectors, simple flat plate collectors, improved flat plate collectors, parabolic collectors with porous media, and flat plate and parabolic collectors with different density of CuO and Al2O3 nanofluids). A case study is investigated for warm and dry regions with mean solar radiation Ib = 820 w / m2 in Iran. The maximum energy and exergy efficiencies are 60.12% and 18.84%, respectively, that is related to enhanced parabolic solar collectors with porous media and nanofluids. Adding porous media and nano-fluids increases an average 14.4% collector energy efficiency and 8.08% collector exergy efficiency.

Keywords

Exergy analysisSolar cogeneration systemPorous mediaNanofluid

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Details

Primary LanguageEnglish
SubjectsEngineering
Journal SectionArticles
AuthorsN. TONEKABONI  This is me
Islamic Azad University Nour Branch
0000-0002-1563-4407
IranH. SALARIAN  This is me (Primary Author)
Islamic Azad University Nour Branch
0000-0002-2161-0276
IranM. Eshagh NIMVARI  This is me
Amol University of Special Modern Technologies
0000-0002-7401-315X
IranJ. KHALEGHINIA  This is me
Islamic Azad University Nour Branch
0000-0001-5357-193X
Iran
Publication DateSeptember 2, 2021
Application DateDecember 28, 2020
Acceptance DateMay 9, 2020
Published in IssueYear 2021, Volume 7, Issue 6
Fig. 1. Schematic of (a) geometry of the simulation model, (b) A-A cross-section presenting the locations of point probes for recording temperature history (unit: µm).

Laser powder bed fusion of 17-4 PH stainless steel: a comparative study on the effect of heat treatment on the microstructure evolution and mechanical properties

17-4 PH 스테인리스강의 레이저 분말 베드 융합: 열처리가 미세조직의 진화 및 기계적 특성에 미치는 영향에 대한 비교 연구

panelS.Saboonia, A.Chaboka, S.Fenga,e, H.Blaauwb, T.C.Pijperb,c, H.J.Yangd, Y.T.Peia
aDepartment of Advanced Production Engineering, Engineering and Technology Institute Groningen, University of Groningen, Nijenborgh 4, 9747 AG, Groningen, The Netherlands
bPhilips Personal Care, Oliemolenstraat 5, 9203 ZN, Drachten, The Netherlands
cInnovation Cluster Drachten, Nipkowlaan 5, 9207 JA, Drachten, The Netherlands
dShi-changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016, P. R. China
eSchool of Mechanical Engineering, University of Science and Technology Beijing, Beijing, 100083, P.R. China

Abstract

17-4 PH (precipitation hardening) stainless steel is commonly used for the fabrication of complicated molds with conformal cooling channels using laser powder bed fusion process (L-PBF). However, their microstructure in the as-printed condition varies notably with the chemical composition of the feedstock powder, resulting in different age-hardening behavior. In the present investigation, 17-4 PH stainless steel components were fabricated by L-PBF from two different feedstock powders, and subsequently subjected to different combinations of post-process heat treatments. It was observed that the microstructure in as-printed conditions could be almost fully martensitic or ferritic, depending on the ratio of Creq/Nieq of the feedstock powder. Aging treatment at 480 °C improved the yield and ultimate tensile strengths of the as-printed components. However, specimens with martensitic structures exhibited accelerated age-hardening response compared with the ferritic specimens due to the higher lattice distortion and dislocation accumulation, resulting in the “dislocation pipe diffusion mechanism”. It was also found that the martensitic structures were highly susceptible to the formation of reverted austenite during direct aging treatment, where 19.5% of austenite phase appeared in the microstructure after 15 h of direct aging. Higher fractions of reverted austenite activates the transformation induced plasticity and improves the ductility of heat treated specimens. The results of the present study can be used to tailor the microstructure of the L-PBF printed 17-4 PH stainless steel by post-process heat treatments to achieve a good combination of mechanical properties.

17-4 PH(석출 경화) 스테인리스강은 레이저 분말 베드 융합 공정(L-PBF)을 사용하여 등각 냉각 채널이 있는 복잡한 금형 제작에 일반적으로 사용됩니다. 그러나 인쇄된 상태의 미세 구조는 공급원료 분말의 화학적 조성에 따라 크게 달라지므로 시효 경화 거동이 다릅니다.

현재 조사에서 17-4 PH 스테인리스강 구성요소는 L-PBF에 의해 두 가지 다른 공급원료 분말로 제조되었으며, 이후에 다양한 조합의 후처리 열처리를 거쳤습니다. 인쇄된 상태의 미세구조는 공급원료 분말의 Creq/Nieq 비율에 따라 거의 완전히 마르텐사이트 또는 페라이트인 것으로 관찰되었습니다.

480 °C에서 노화 처리는 인쇄된 구성 요소의 수율과 극한 인장 강도를 개선했습니다. 그러나 마텐자이트 구조의 시편은 격자 변형 및 전위 축적이 높아 페라이트 시편에 비해 시효 경화 반응이 가속화되어 “전위 파이프 확산 메커니즘”이 발생합니다.

또한 마르텐사이트 구조는 직접 시효 처리 중에 복귀된 오스테나이트의 형성에 매우 민감한 것으로 밝혀졌으며, 여기서 15시간의 직접 시효 후 미세 조직에 19.5%의 오스테나이트 상이 나타났습니다.

복귀된 오스테나이트의 비율이 높을수록 변형 유도 가소성이 활성화되고 열처리된 시편의 연성이 향상됩니다. 본 연구의 결과는 기계적 특성의 우수한 조합을 달성하기 위해 후처리 열처리를 통해 L-PBF로 인쇄된 17-4 PH 스테인리스강의 미세 구조를 조정하는 데 사용할 수 있습니다.

Keywords

Laser powder bed fusion17-4 PH stainless steelPost-process heat treatmentAge hardeningReverted austenite

Fig. 1. Schematic of (a) geometry of the simulation model, (b) A-A cross-section presenting the locations of point probes for recording temperature history (unit: µm).
Fig. 1. Schematic of (a) geometry of the simulation model, (b) A-A cross-section presenting the locations of point probes for recording temperature history (unit: µm).
Fig. 2. Optical (a, b) and TEM (c) micrographs of the wrought 17-4 PH stainless steel.
Fig. 2. Optical (a, b) and TEM (c) micrographs of the wrought 17-4 PH stainless steel.
Fig. 3. EBSD micrographs of the as-printed 17-4 PH steel fabricated with “powder A” (a, b) and “powder B” (c, d) on two different cross sections: (a, c) perpendicular to the building direction, and (b, d) parallel to the building direction.
Fig. 3. EBSD micrographs of the as-printed 17-4 PH steel fabricated with “powder A” (a, b) and “powder B” (c, d) on two different cross sections: (a, c) perpendicular to the building direction, and (b, d) parallel to the building direction.
Fig. 4. Microstructure of the as-printed 17-4 PH stainless steel fabricated with “powder A” (a) and “powder B” (b).
Fig. 4. Microstructure of the as-printed 17-4 PH stainless steel fabricated with “powder A” (a) and “powder B” (b).
Fig. 5. Simulated temperature history of the probes located at the cross section of the L-PBF 17-4 PH steel sample.
Fig. 5. Simulated temperature history of the probes located at the cross section of the L-PBF 17-4 PH steel sample.
Fig. 6. Dependency of the volume fraction of delta ferrite in the final microstructure of L-PBF printed 17-4 PH steel as a function of Creq/Nieq.
Fig. 6. Dependency of the volume fraction of delta ferrite in the final microstructure of L-PBF printed 17-4 PH steel as a function of Creq/Nieq.
Fig. 7. IQ + IPF (left column), parent austenite grain maps (middle column) and phase maps (right column, green color = martensite, red color = austenite) of the post-process heat treated 17-4 PH stainless steel: (a-c) direct aged, (d-f) HIP + aging, (g-i) SA + Aging, and (j-l) HIP + SA + aging (all sample were printed with “powder A”).
Fig. 7. IQ + IPF (left column), parent austenite grain maps (middle column) and phase maps (right column, green color = martensite, red color = austenite) of the post-process heat treated 17-4 PH stainless steel: (a-c) direct aged, (d-f) HIP + aging, (g-i) SA + Aging, and (j-l) HIP + SA + aging (all sample were printed with “powder A”).
Fig. 8. TEM micrographs of the post process heat treated 17-4 PH stainless steel: (a) direct aging and (b) HIP + aging (printed with “powder A”).
Fig. 8. TEM micrographs of the post process heat treated 17-4 PH stainless steel: (a) direct aging and (b) HIP + aging (printed with “powder A”).
Fig. 9. XRD patterns of the post-process heat treated 17-4 PH stainless steel printed with “powder A”.
Fig. 9. XRD patterns of the post-process heat treated 17-4 PH stainless steel printed with “powder A”.
Fig. 10. (a) Volume fraction of reverted austenite as a function of aging time for “direct aging” condition, (b) phase map (green color = martensite, red color = austenite) of the 15 h direct aged specimen printed with “powder A”.
Fig. 10. (a) Volume fraction of reverted austenite as a function of aging time for “direct aging” condition, (b) phase map (green color = martensite, red color = austenite) of the 15 h direct aged specimen printed with “powder A”.
Fig. 11. Microhardness variations of the “direct aged” specimens as a function of aging time at 480 °C.
Fig. 11. Microhardness variations of the “direct aged” specimens as a function of aging time at 480 °C.
Fig. 12. Kernel average misorientation graphs of the as-printed 17-4 PH steel with (a) martensitic structure (printed with “powder A”) and (b) ferritic structure (printed with “powder b”).
Fig. 12. Kernel average misorientation graphs of the as-printed 17-4 PH steel with (a) martensitic structure (printed with “powder A”) and (b) ferritic structure (printed with “powder b”).
Fig. 13. Typical stress-strain curves (a) along with the yield and ultimate tensile strengths (b) and elongation (c) of the as-printed and post-process heat treated 17-4 PH stainless steel (all sample are fabricated with “powder A”).
Fig. 13. Typical stress-strain curves (a) along with the yield and ultimate tensile strengths (b) and elongation (c) of the as-printed and post-process heat treated 17-4 PH stainless steel (all sample are fabricated with “powder A”).
Fig. 14. (a) IQ + IPF and (b) phase map (green color = martensite, red color = austenite) of the “direct aged” specimen after tensile test at a location nearby the rupture point (tension direction from left to right).
Fig. 14. (a) IQ + IPF and (b) phase map (green color = martensite, red color = austenite) of the “direct aged” specimen after tensile test at a location nearby the rupture point (tension direction from left to right).

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