Analyzing the Interplay of Sintering Conditions on Microstructure and Hardness in Indirect Additive Manufacturing of 17-4PH Stainless Steel

doi:10.1007/s40195-024-01745-6

Abstract

Abstract:

Indirect additive manufacturing (AM) methods have recently attracted attention from researchers thanks to their great potential for cheap, straightforward, and small-scale production of metallic components. Atomic diffusion additive manufacturing (ADAM), a variant of indirect AM methods, is a layer-wise indirect AM process recently developed based on fused deposition modeling and metal injection molding. However, there is still limited knowledge of the process conditions and material properties fabricated through this process, where sintering plays a crucial role in the final consolidation of parts. Therefore, this research, for the first time, systematically investigates the impact of various sintering conditions on the shrinkage, relative density, microstructure, and hardness of the 17-4PH ADAM samples. For this reason, as-washed samples were sintered under different time-temperature combinations. The sample density was evaluated using Archimedes, computed tomography, and image analysis methods. The outcomes revealed that sintering variables significantly impacted the density of brown 17-4PH Stainless Steel samples. The results indicated more than 99% relative densities, higher than the value reported by Markforged Inc. (~96%). Based on parallel porosities observed in the computed tomography results, it can be suggested that by modifying the infill pattern during printing, it would be possible to increase the final relative density. The microhardness of the sintered samples in this study was higher than that of the standard sample provided by Markforged Inc. Sintering at 1330 °C for 4 h increased the density of the printed sample without compromising its mechanical properties. According to X-ray diffraction analysis, the standard sample provided by Markforged Inc. and “1330 °C—4 h” one had similar stable phases, although copper-rich intermetallics were more abundant in the microstructure of reference samples. This study is expected to facilitate the adoption of indirect metal AM methods by different sectors, thanks to the high achievable relative densities reported here.

Key words: Indirect additive manufacturing, Atomic diffusion additive manufacturing, 17-4PH stainless steel, Computed tomography, Sintering

Erika Lannunziata, Mohammad Hossein Mosallanejad, Manuela Galati, Gabriele Piscopo, Abdollah Saboori. Analyzing the Interplay of Sintering Conditions on Microstructure and Hardness in Indirect Additive Manufacturing of 17-4PH Stainless Steel[J]. Acta Metallurgica Sinica (English Letters), 2024, 37(9): 1611-1620.

Figures/Tables 14

Table 1 Chemical composition of the 17-4PH filament used in this work [28]

Cr	Ni	Cu	Si	Mn	Nb	C	P	S	Fe
15-17.5%	3-5%	3-5%	1% max	1% max	0.15-0.45%	0.07% max	0.04% max	0.03% max	Bal.

Fig. 1 Time-temperature map for 17-4PH alloy used in this work for the sintering cycle selection [35]

Fig. 2 CT scan results for the 17-4PH sample sintered by Markforged

Fig. 3 3D scan result of the 17-4PH sample showing the external surfaces

Fig. 4 OM images depicting the porosities on a XY, c XZ planes for sample 1280 °C—1 h. The CT scan results show the porosities on b XY [top surface] d XZ plane for sample 1330 °C—4 h, with the onset image illustrating the analyzed portion

Table 2 Open, close, total, and relative densities of the 17-4PH samples after various sintering conditions

Sample	Open porosity (%)	Closed porosity (%)	Total porosity (%)	Relative density (%)
Standard	0.01	4.04	4.0	96.0±0.10
1280 °C—1 h	0.21	3.55	3.8	96.2±0.59
1280 °C—2 h	0.72	2.29	3.0	97.0±0.02
1280 °C—4 h	0.11	2.54	2.6	97.4±0.18
1330 °C—1 h	0.13	2.38	2.5	97.5±0.09
1330 °C—2 h	0.09	2.40	2.5	97.5±0.48
1330 °C—4 h	0.12	2.37	2.5	97.5±0.48

Fig. 5 Relative density of the sintered 17-4PH samples obtained by the image processing method

Fig. 6 Relative density of the sintered 17-4PH samples obtained by the CT scan analysis

Table 3 Weight loss, dimensional and volumetric shrinkage of the 17-4PH samples after sintering

Sample	Weight loss (%)	Shrinkage (%)
Sample	Weight loss (%)	l	w	h	Volume
1280 °C—1 h	3.00	14.87	14.83	16.52	39.74
1280 °C—2 h	2.87	15.07	15.23	15.76	39.35
1280 °C—4 h	2.87	15.17	15.32	16.31	39.88
1330 °C—1 h	2.91	14.99	15.22	16.25	39.63
1330 °C—2 h	2.91	14.72	15.27	15.73	39.10
1330 °C—4 h	2.90	14.84	15.26	16.20	39.53

Table 4 Hardness values of the 17-4PH samples after various sintering conditions

Hardness (HB)
Sample	XY	ZX
Standard	282±10	294±6
1280 °C—1 h	287±5	298±8
1280 °C—2 h	290±26	285±16
1280 °C—4 h	300±6	312±6
1330 °C—1 h	296±6	306±8
1330 °C—2 h	296±6	291±5
1330 °C—4 h	299±3	289±7

Fig. 7 XRD pattern of the sintered 17-4PH samples with inset magnifying the (111) γ and (110) α indexes

Fig. 8 SEM images of the 17-4PH sample sintered with a standard sintering cycle on XY, b XZ, sintered at c 1280 °C for 1 h, d 4 h, at e 1330 °C for 1 h, f 4 h in XZ

Fig. 9 EDS analysis of the 17-4PH sample sintered at 1330 °C for 1 h

Fig. 10 EDS analysis of the 17-4PH samples sintered at 1330 °C for 1 h

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