Effect of solution heat treatment and hot isostatic pressing on the microstructure and mechanical properties of Hastelloy X manufactured by electron beam powder bed fusion

doi:10.1016/j.jmst.2021.04.059

Abstract

Abstract:

Prior to the application of AM components for critical applications, it is necessary to have a better understanding of the effect of different post-fabrication treatments on the microstructure and mechanical properties of such parts. In this study, efforts were made to achieve an in-depth understanding of the effect of post-fabrication Solution Heat Treatment (SHT) and Hot Isostatic Pressing (HIP) on the microstructure and mechanical properties of Hastelloy X parts built by electron beam powder bed fusion (PBF-EB) process. The effects of SHT and HIP on porosity, microstructure, texture and mechanical properties have been investigated and compared with that of as-built PBF-EB Hastelloy X. Post-fabrication HIP treatment led to a significant reduction in the porosity content, whereas no notable difference in porosity was observed between SHT and as-built parts. There was no evidence of any recrystallization occurring following the post-fabrication treatments as elongated columnar grain structures observed within as-built part were found to be maintained even after SHT and HIP process alongside the strong 〈100〉 crystallographic texture. Emphasis was laid upon understanding the influence of SHT and HIP on mechanical properties through stress-strain curves and work-hardening behaviour.

Key words: Additive manufacturing, Electron beam powder bed fusion, Nickel-based superalloy, Heat treatment, Hot isostatic pressing

AmalShaji Karapuzha, Darren Fraser, Yuman Zhu, Xinhua Wu, Aijun Huang. Effect of solution heat treatment and hot isostatic pressing on the microstructure and mechanical properties of Hastelloy X manufactured by electron beam powder bed fusion[J]. J. Mater. Sci. Technol., 2022, 98: 99-117.

Figures/Tables 22

Table 1 Chemical composition of the pre-alloyed Hastelloy X powder used in the present study obtained by ICP-OES analysis (wt.%).

Ni	Cr	Fe	Mo	Co	Si	W	Al	C	Mn
Bal.	21.0	18.6	9.2	1.6	0.47	0.74	0.2	< 0.01	< 0.01

Fig. 1. (a) SEM micrograph of pre-alloyed Hastelloy X powder, (b) schematic of scanning strategy used in the present study, (c) layout of horizontal and vertical build specimens on the build plate and (d) representative tensile specimens extracted from the as-built and post-treated blocks and its dimensions.

Fig. 2. (a) Relative density of as-built and post-treated PBF-EB Hastelloy X specimens obtained from µ-CT and OM image analysis, 3D visualization of defect distribution in (b) as-built, (c) SHT and (d) HIP PBF-EB Hastelloy X specimens and representative OM micrographs showing porosity in (e) as-built, (f) SHT and (g) HIP PBF-EB Hastelloy X specimens along the transverse plane.

Fig. 3. Etched OM micrographs of as-built PBF-EB Hastelloy X specimens sectioned along (a) transverse and (b) vertical plane. The scan tracks and melt pools are highlighted by yellow and red dashed lines, respectively. The solid black line corresponds to grain boundaries.

Fig. 4. Representative SEM micrographs of as-built PBF-EB Hastelloy X specimens showing grain structure (a) perpendicular to build direction, (b) parallel to build direction, (c) dendritic microstructure and (d) segregation of precipitates at grain boundaries.

Fig. 5. (a) SEM-BSE image and corresponding EDXS maps showing the presence of Mo-rich carbides along grain boundaries of as-built PBF-EB Hastelloy X, (b) EDXS line scan results obtained across the precipitate marked in (a), (c) EDXS spectrum and spot analysis results (in wt.%) of the γ-matrix (Spot 1) and carbide precipitate (Spot 2) shown in (a).

Fig. 6. (a) Etched optical micrograph showing the dissolution of melt pool boundaries after SHT, (b) high magnification SEM image showing the dissolution of dendritic microstructure after SHT, (c) no significant precipitates in SHT PBF-EB Hastelloy X, (d) segregation of precipitates at grain boundaries in HIPed PBF-EB Hastelloy X specimen.

Fig. 7. (a) EDXS map results showing the presence of Mo-rich carbide precipitates in the grain boundaries of HIP PBF-EB Hastelloy X, (b) EDXS line scan results obtained across the precipitate marked in (a), EDXS spectrum and spot analysis results (in wt.%) of the (c) γ-matrix (Spot 1) and (d) carbide precipitate (Spot 2) shown in (a).

Fig. 8. EBSD IPF maps showing grain morphology of as-built and post-treated PBF-EB Hastelloy X specimens along (a-c) transverse plane and (d-f) vertical plane. The corresponding {100}, {110} and {111} pole figure maps are shown below the IPF maps.

Table 2 Grain size characteristics of as-built and post-treated PBF-EB Hastelloy X specimens.

Sample	Number of grains	Mean Diameter (µm)	Mean Aspect Ratio	Min Aspect Ratio	Max Aspect Ratio
As-built-Horizontal	3727	28.9 ± 2.7	1.9 ± 0.7	1.0	7.2
As-built-Vertical	734	82.0 ± 65.4	4.5 ± 0.8	1.0	31.8
SHT-Horizontal	2490	35.7 ± 3.2	2.0 ± 0.9	1.0	12.8
SHT-Vertical	398	92.9 ± 76.7	5.4 ± 4.5	1.0	31.4
HIP-Horizontal	1796	42.9 ± 10.1	2.2 ± 1.1	1.0	12.3
HIP-Vertical	288	129.9 ± 101.5	4.7 ± 4.1	1.0	25.0

Fig. 9. Room temperature mechanical properties of PBF-EB Hastelloy X as a function of build orientations and post-treatment: (a) representative engineering stress-strain curves, (b) yield strength, (c) ultimate tensile stress, (d) elongation to failure, (e) Vickers microhardness. The dashed line corresponds to the room temperature tensile properties of as-cast Hastelloy X obtained from Ref. [48].

Fig. 10. Fracture surfaces of horizontal build room temperature PBF-EB Hastelloy X tensile specimens loaded perpendicular to build direction: (a) as-built, (b) SHT, (c) HIP condition. The high magnification SEM micrographs for corresponding post-fabrication treatments are shown in the inset. Few of the micro-pores are highlighted using red arrows.

Fig. 11. Fracture surfaces of vertically build room temperature PBF-EB Hastelloy X tensile specimens loaded parallel to build direction: (a) as-built, (b) SHT, (c) HIP condition. The high magnification SEM micrographs for corresponding conditions are shown in the inset. Few of the micro-pores are highlighted using red arrows.

Fig. 12. Grain structure of PBF-EB Hastelloy X as a function of post-fabrication treatments along transverse and vertical plane: (a, b), (e, f) and (i, j) grain size distribution; (c, d), (g, h) and (k, l) aspect ratio distribution.

Fig. 13. IAMA maps showing recrystallized, substructured and deformed grains in PBF-EB Hastelloy X as a function of post-fabrication thermal treatments along the transverse and vertical planes. The corresponding volume fraction of each type of grains is shown below the IAMA maps.

Fig. 14. (a) True tensile stress-strain curves, (b) instantaneous work hardening rate (θ) curves, (c) log σ vs log ε curves indicating work hardening exponents (n) for as-built, SHT and HIPed PBF-EB Hastelloy X specimens along horizontal and vertical directions. The inset figure in (b) shows the different stages of work hardening within PBF-EB Hastelloy X specimens.

Table 3 Parameters of Hollomon relation derived from tensile tests.

Specimen	K₁ (MPa)	n₁	K₂ (MPa)	n₂
As-built-Horizontal	705 ± 15	0.12 ± 0.005	1301 ± 11	0.33 ± 0.006
As-built-Vertical	594 ± 27	0.12 ± 0.006	1226 ± 54	0.39 ± 0.019
SHT-Horizontal	581 ± 31	0.12 ± 0.003	1523 ± 31	0.47 ± 0.022
SHT-Vertical	582 ± 10	0.12 ± 0.002	1239 ± 10	0.41 ± 0.006
HIP-Horizontal	554 ± 10	0.12 ± 0.003	1526 ± 36	0.48 ± 0.013
HIP-Vertical	546 ± 9	0.12 ± 0.004	1273 ± 34	0.42 ± 0.014

Table 4 Values of ki (MPa At. Fraction-0.5) for determining solid solution strengthening.

Cr	Fe	Mo	Co	Si	W	Al	Mn
337	153	1015	39.4	275	977	225	448

Fig. 15. Hall-Petch plot of the grain size dependence of yield stress in PBF-EB Hastelloy X.

Table 5 Estimated contribution of grain boundary strengthening towards the yield strength of as-built, SHT and HIPed PBF-EB Hastelloy X.

Loading Direction	As-built	SHT	HIP
Parallel to Transverse Plane	106 ± 23 MPa	95 ± 21 MPa	87 ± 19 MPa
Parallel to Vertical Plane	63 ± 14 MPa	59 ± 13 MPa	50 ± 11 MPa

Fig. 16. Taylor factor maps of as-built, SHT and HIPed PBF-EB Hastelloy X specimens.

Table 6 Estimated contribution of dislocation strengthening towards the yield strength of as-built, SHT and HIPed PBF-EB Hastelloy X.

Loading Direction	As-built	SHT	HIP
Parallel to Transverse Plane	197 ± 45 MPa	121 ± 23 MPa	129 ± 27 MPa
Parallel to Vertical Plane	140 ± 32 MPa	84 ± 16 MPa	95 ± 20 MPa

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