A 316 austenitic stainless-steel alloy, with modified alloy composition, manufactured by laser powder bed fusion (L-PBF) has been investigated. The modification of the alloy composition included addition of niobium (Nb), tungsten (W) and copper (Cu), together with a reduction in the amount of molybdenum (Mo) and an increased amount of carbon (C). To find suitable process parameters, a parameter study by varying laser power, hatch distance and scan speed was performed, centered on typical parameters used for normal 316 L. As-built material from a selected parameter configuration was then subjected to different stress relief annealing heat treatments and ageing heat treatments. The effectiveness of the stress annealing was ranked using a deformation-based method. Microstructural characterization, hardness and room temperature tensile testing were done to evaluate the effect of stress relief and aging heat treatments.

It was found that a higher volumetric energy was needed to build dense material, about ∼50 % higher compared to the volumetric energy input for normal 316 L. A subsequent aging heat treatment at 725 °C for 3 h increased the strength and hardness of the material. A reinforcement of the cellular microstructure by precipitation of carbides in between the cells is believed to be the main reason for this. To completely alleviate the residual stresses it was necessary to carry out a stress relief annealing process at 950 °C, which resulted in a removal of the cellular structure and a lower strength material.

In this work, the effectiveness of residual stress relief annealing on a laser powder bed fusion (L-PBF) manufactured austenitic stainless steel, alloy 21-6-9 was investigated. Residual stress levels were gauged using geometrical distortion and relaxation testing results. In the investigated temperature interval (600–850 °C), shape stability was reached after subjecting the as-built material to an annealing temperature of 850 °C for 1 h. Microstructural characterization and tensile testing were also performed for each annealing temperature to evaluate the alloy's thermal stability and the resulting tensile properties. In the as-built state, a yield strength (YS) of 640 MPa, ultimate tensile strength (UTS) of 810 MPa and 4D elongation of 47% were measured. Annealing at 850 °C for 1 h had little measurable effect on ductility (48% 4D elongation) while still having a softening effect (UTS = 775 MPa, YS = 540 MPa). From the microstructural characterization, cell-like features were observed sporadically in the annealed condition and appeared stable up until 800 °C after which gradual dissolution began, with the last remnants disappearing after subjecting the material to 900 °C for 1 h.

Additive manufacturing (AM) processes may introduce large residual stresses in the as-built part, in particular the laser powder bed fusion process (L-PBF). The residual stress state is an inherent consequence of the heterogeneous heating and subsequent cooling during the process. L-PBF has become renowned for its “free complexity” and rapid prototyping capabilities. However, it is vital to ensure shape stability after the component is removed from the build plate, which can be problematic due to the residual stress inducing nature of this manufacturing process. Residual stresses can be analyzed via many different characterization routes (e.g. X-ray and neutron diffraction, hole drilling, etc.), both quantitatively and qualitatively. From an industrial perspective, most of these techniques are either prohibitively expensive, complex or too slow to be implementable during the early prototyping stages of AM manufacturing.

In this work a deformation based method employing a specific geometry, a so called “keyhole”-geometry, has been investigated to qualitatively evaluate the effect of different stress relief annealing routes with respect to macroscopic part deformation, mechanical properties and microstructure. Previous published work has focused on structures with open geometry, commonly referred to as bridge-like structures where the deformation required for analysis occurs during removal from the build plate. The proposed keyhole-geometry can be removed from the build plate without releasing the residual stresses required for subsequent measurement, which enables bulk manufacturing on single build plates, prior to removal and stress relief annealing. 

Two L-PBF manufactured austenitic stainless steel alloys were studied, 316L and 21-6-9. Tensile specimen blanks were manufactured and the subsequent heat treatments were carried out in pairs of keyhole and tensile blank. Both a contact (micrometer measurement), and a non-contact (optical profilometry) method were employed to measure the residual stress induced deformation in the keyholes. The annealing heat treatment matrix was iteratively expanded with input from the deformation analysis to find the lowest temperature at which approximately zero deformation remained after opening the structure via wire electrical discharge machining. The lowest allowable annealing temperature was sought after to minimize strength loss. 

After stress relief annealing at 900 ℃ for 1 hour, the 316L keyhole-geometry was considered shape stable. The lateral micrometer measurement yielded a length change of 1 µm, and a radius of 140 m (over the 22 mm top surface) was assigned from curve fitting the top surface height profiles. The complementary microstructural characterization revealed that this temperature corresponded to where the last remains of the cellular sub-grain structures disappears. Tensile testing showed that the specimen subjected to the 900 ℃ heat treatment had a marked reduction in yield stress (YS) compared to that of the as-built: 540 MPa → 402 MPa, whereas ultimate tensile strength (UTS) only reduced slightly: 595 MPa → 570 MPa. The ductility (4D elongation) was found to be ~13 % higher for the specimen heat treated at 900 ℃ than that of the as-built specimen, 76% and 67% respectively. 

For alloy 21-6-9 the residual stress induced deformation minimum (zero measurable deformation) was found after stress relief heat treatment at 850 ℃ for 1 hour. Slight changes in the microstructure were observable through light optical microscopy when comparing the different heat treatment temperatures. The characteristic sub-grain features associated with alloy 316L were not verified for alloy 21-6-9. Similar to the results for 316L, UTS was slightly lower for the tensile specimen subjected to the heat treatment temperature required for shape stability (850 ℃) compared to the as-built specimen: 810 MPa → 775 MPa. The measured ductility (4D elongation) was found to be approximately equal for the as-built (47%), and heat treated (48%) specimen. As-built material exhibited a YS of 640 MPa while the heat treated specimen had a YS of 540 MPa. For alloy 21-6-9, the lateral micrometer deformation measurements were compared with stress relaxation testing performed at 600 ℃, 700℃ and 800 ℃. Stress relaxation results were in good agreement with the results from the lateral deformation measurements. 

The study showed that for both steel alloys, the keyhole method could be successfully employed to rapidly find a suitable stress relief heat treatment route when shape stability is vital.

The additive manufacturing method laser powder bed fusion (L-PBF) is known to introduce large residual stresses in the built component. Optimization of process parameters and subsequent heat treatment is crucial to relieve these residual stresses. However, many of the available tools used to analyze these residual stresses are either prohibitively expensive, or too time consuming for initial prototyping stages.

A qualitative method for rapid evaluation of the effectiveness of stress relief heat treatment of L-PBF manufactured 316L has been tested. Residual stress induced distortion has been measured with contact and non-contact methods to study the effect of different stress relief heat treatment temperatures (600 – 950 °C, fixed holding time: 1 h). Over the examined temperature interval, at which deformation was measured, distinct differences were observable at each temperature with both methods. Based on the distortion, shape stability was considered reached after subjecting the test geometry to a heat treatment temperature of 900 °C for 1 hour. Complementary mechanical testing and microstructural characterization were carried out to provide a more general understanding of the implications of each heat treatment temperature. Microstructural characterization revealed that complete dissolution of the cellular sub-grain features occurred at the same temperature as where the minimum magnitude of distortion was obtained.

Alloy 21-6-9 is an austenitic stainless steel with high strength, thermal stability at high temperatures, and retained toughness at cryogenic temperatures. This type of steel has been used for aerospace applications for decades, using traditional manufacturing processes. However, limited research has been conducted on this alloy manufactured using laser powder-bed fusion (LPBF). Therefore, in this work, a design of experiment (DOE) was performed to obtain optimized process parameters with regard to low porosity. Once the optimized parameters were established, horizontal and vertical blanks were built to investigate the mechanical properties and potential anisotropic behavior. As this alloy is exposed to elevated temperatures in industrial applications, the effect of elevated temperatures (room temperature and 750 °C) on the tensile properties was investigated. In this work, it was shown that alloy 21-6-9 could be built successfully using LPBF, with good properties and a density of 99.7%, having an ultimate tensile strength of 825 MPa, with an elongation of 41%, and without any significant anisotropic behavior.