Rapid <i>in situ</i> alloying of CoCrFeMnNi high-entropy alloy from elemental feedstock toward high-throughput synthesis via laser powder bed fusion

doi:10.1007/s11465-022-0727-x

Front. Mech. Eng.

2023, Vol. 18

Issue (1) : 11 https://doi.org/10.1007/s11465-022-0727-x

RESEARCH ARTICLE

Rapid in situ alloying of CoCrFeMnNi high-entropy alloy from elemental feedstock toward high-throughput synthesis via laser powder bed fusion

Bowen WANG^1,^2,³, Bingheng LU^1,^2,³(

), Lijuan ZHANG^2,³(

), Jianxun ZHANG^3,⁴, Bobo LI^1,^2,³, Qianyu JI^1,^2,³, Peng LUO^2,⁵, Qian LIU^1,^2,³

¹. School of Mechanical Engineering, Xi’an Jiaotong University, Xi’an 710049, China
². State Key Laboratory of Manufacturing Systems Engineering, Xi’an Jiaotong University, Xi’an 710049, China
³. National Innovation Institute of Additive Manufacturing, Xi’an 710300, China
⁴. State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049, China
⁵. Institute of Materials, China Academy of Engineering Physics, Mianyang 621908, China

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Abstract

High-entropy alloys (HEAs) are considered alternatives to traditional structural materials because of their superior mechanical, physical, and chemical properties. However, alloy composition combinations are too numerous to explore. Finding a rapid synthesis method to accelerate the development of HEA bulks is imperative. Existing in situ synthesis methods based on additive manufacturing are insufficient for efficiently controlling the uniformity and accuracy of components. In this work, laser powder bed fusion (L-PBF) is adopted for the in situ synthesis of equiatomic CoCrFeMnNi HEA from elemental powder mixtures. High composition accuracy is achieved in parallel with ensuring internal density. The L-PBF-based process parameters are optimized; and two different methods, namely, a multi-melting process and homogenization heat treatment, are adopted to address the problem of incompletely melted Cr particles in the single-melted samples. X-ray diffraction indicates that HEA microstructure can be obtained from elemental powders via L-PBF. In the triple-melted samples, a strong crystallographic texture can be observed through electron backscatter diffraction, with a maximum polar density of 9.92 and a high ultimate tensile strength (UTS) of (735.3 ± 14.1) MPa. The homogenization heat-treated samples appear more like coarse equiaxed grains, with a UTS of (650.8 ± 16.1) MPa and an elongation of (40.2% ± 1.3%). Cellular substructures are also observed in the triple-melted samples, but not in the homogenization heat-treated samples. The differences in mechanical properties primarily originate from the changes in strengthening mechanism. The even and flat fractographic morphologies of the homogenization heat-treated samples represent a more uniform internal microstructure that is different from the complex morphologies of the triple-melted samples. Relative to the multi-melted samples, the homogenization heat-treated samples exhibit better processability, with a smaller composition deviation, i.e., ≤ 0.32 at.%. The two methods presented in this study are expected to have considerable potential for developing HEAs with high composition accuracy and composition flexibility.

Keywords laser powder bed fusion (L-PBF) in situ alloying high-entropy alloys heat treatment rapid synthesis

Corresponding Author(s): Bingheng LU,Lijuan ZHANG

Just Accepted Date: 30 August 2022 Issue Date: 10 January 2023

Cite this article:

Bowen WANG,Bingheng LU,Lijuan ZHANG, et al. Rapid in situ alloying of CoCrFeMnNi high-entropy alloy from elemental feedstock toward high-throughput synthesis via laser powder bed fusion[J]. Front. Mech. Eng., 2023, 18(1): 11.

URL:

https://academic.hep.com.cn/fme/EN/10.1007/s11465-022-0727-x
https://academic.hep.com.cn/fme/EN/Y2023/V18/I1/11

Fig.1 Secondary electron micrographs of the different morphologies of the used powders.

Tab.1 Particle size distributions of the Co, Cr, Fe, Mn, and Ni elemental powders and the blended powder

Fig.2 (a) Morphologies of the prepared elemental powder mixtures, (b) energy-dispersive X-ray spectroscopy mapping, and (c) forming strategy.

Tab.2 Inductively coupled plasma analysis results of the raw materials used in this study and the chemical composition of the in situ-synthesized CoCrFeMnNi HEA samples via different L-PBF sequences

Tab.3 Process parameters used in this study

Fig.3 Longitudinal section optical micrographs of as-built single-melted samples at VEDs of (a) 80 J/mm³, (b) 89 J/mm³, (c) 101 J/mm³, (d) 116 J/mm³, (e) 136 J/mm³, and (f) 165 J/mm³.

Fig.4 Longitudinal section optical micrographs of in situ-alloyed CoCrFeMnNi HEA with different numbers of melting steps: (a) single melting, (b) double melting, (c) triple melting, and (d) quadruple melting.

Fig.5 Scanning electron microscopy and energy-dispersive X-ray spectroscopy mapping of the in situ-synthesized CoCrFeMnNi high-entropy alloy from elemental powders through different processes: (a) single-melted samples (laser power: 280 W, scanning speed: 670 mm/s, hatch space: 90 μm, layer thickness: 40 μm, and VED: 116 J/mm³), (b) triple-melted samples, and (c) single-melted + homogenization heat-treated samples.

Fig.6 XRD patterns of the initial elemental powder mixture, single-melted samples, triple-melted samples, and homogenization heat-treated samples, with peak (111) enlarged.

Fig.7 3D crystallographic orientation demonstration and the corresponding pole figures and inverse pole figures of the (a) single-melted samples, (b) triple-melted samples, and (c) homogenization heat-treated samples (applied to single-melted samples).

Fig.8 Engineering tensile stress–strain curves of the triple-melted samples and homogenization heat-treated samples.

Samples	$σ 0$ /MPa	$σ GB$ /MPa	$σ dis$ /MPa	$σ y$ /MPa	Estimated YS/MPa	Deviation/%
Triple-melted samples	147	91.6	347.3	585.9	610.2	4.0
Homogenized samples	147	82.4	95.6	325.0	293.8	10.6

Tab.4 All strengthening components and estimated YS

Fig.9 Transmission electron microscopy bright field images of (a) triple-melted samples with cellular substructures and (b) homogenization heat-treated samples (applied to single-melted samples) without cellular substructures.

Samples	$σ y$ /MPa	UTS/MPa	$ε f$ /%	Reference
Triple-melting samples	610.2 ± 15.8	735.3 ± 14.1	14.4 ± 0.9	Present work
Homogenized samples	293.8 ± 8.1	650.8 ± 16.1	40.2 ± 1.3	Present work
L-PBF samples from pre-alloyed powders	582.9 ± 10.8	679.8 ± 12.9	23.8 ± 1.4	[16]
L-PBF samples from pre-alloyed powders	519.0	601.0	35.0	[26]
LMD samples from pre-alloyed powders	346.0	566.0	26.0	[50]
Electron beam welding samples	320.0	617.0	27.0	[51]
Gas W arc welding samples	297.0	530.0	15.0	[51]

Tab.5 Tensile properties of triple-melted samples, homogenization heat-treated samples, and samples produced using other processes

Fig.10 (a) Tensile fracture surface of the triple-melted samples and (b) homogenization heat-treated samples.

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