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At least 73 records · Page 4

Pitting Corrosion in 316L Stainless Steel Fabricated by Laser Powder Bed Fusion Additive Manufacturing: A Review and Perspective

Abstract 316L stainless steel (316L SS) is a flagship material for structural applications in corrosive environments, having been extensively studied for decades for its favorable balance between mechanical and corrosion properties. More recently, 316L SS has also proven to have excellent printability when parts are produced with additive manufacturing techniques, notably laser powder bed fusion (LPBF). Because of the harsh thermo-mechanical cycles experienced during rapid solidification and cooling, LPBF processing tends to generate unique microstructures. Strong heterogeneities can be found inside grains, including trapped elements, nano-inclusions, and a high density of dislocations that form the so-called cellular structure. Interestingly, LPBF 316L SS not only exhibits better mechanical properties than its conventionally processed counterpart, but it also usually offers much higher resistance to pitting in chloride solutions. Unfortunately, the complexity of the LPBF microstructures, in addition to process-induced defects, such as porosity and surface roughness, have slowed progress toward linking specific microstructural features to corrosion susceptibility and complicated the development of calibrated simulations of pitting phenomena. The first part of this article is dedicated to an in-depth review of the microstructures found in LPBF 316L SS and their potential effects on the corrosion properties, with an emphasis on pitting resistance. The second part offers a perspective of some relevant modeling techniques available to simulate the corrosion of LPBF 316L SS, including current challenges that should be overcome.

Voisin, T. (ORCID:0000000287462659)↗

Additive manufacturing of a metastable high entropy alloy: Metastability engineered microstructural control via process variable driven elemental segregation

Compositional paradigm shift in high entropy alloys (HEAs) provided new opportunities for microstructural engineering, whereas process control during laser powder bed fusion (LPBF) additive manufacturing (AM) enable fine microstructure tailoring. Metastability engineering in transformation induced plasticity (TRIP) HEAs by addition of minor alloying elements is an attractive strategy for fine microstructural tuning. This study explored in detail the microstructural evolution during LPBF AM of a metastable Fe 40 Mn 20 Co 20 Cr 15 Si 5 (at.%) dual phase HEA (CS-HEA). LPBF processing window for CS-HEA was established based on quantitative analysis and experiments. Based on melt pool overlap lack of fusion pores were observed at lower energy densities (J) of $\textit{J}$ ≤ 31.25 J/mm 3 and key-hole formation by melt pool destabilization in case of $\textit{J}$ ≥ 75 J/mm 3 . The microstructure of CS-HEA consists of metastable FCC-γ and HCP-ε phases; LPBF process parameters governed the final phase fraction in the alloy which has been correlated to metastability alteration of the high temperature γ phase. Final microstructural engineering was devised by LPBF process control which enabled cooling rate manipulation to guide Mn and Si segregation at the cell boundaries, thereby controlling the matrix metastability and final phase fraction. Additionally, high resolution transmission electron microscopy (TEM) revealed disparity in stacking fault morphology in CS-HEA with LPBF process variable alterations associated with local variations in chemical composition and stacking fault energy. Further, the phase evolution with process parameters also affected the nanomechanical behavior of the alloy.

36 MATERIALS SCIENCE↗

Pulsed Thermal Tomography Nondestructive Examination of Additively Manufactured Reactor Materials (Second Annual Progress Report)

Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of nuclear reactor parts. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process, which can introduce internal material flaws, such as pores and anisotropy. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures due to exposure to high temperature, radiation and corrosive environment in a nuclear reactor. Thermal tomography (TT) provides a capability for non-destructive evaluation of sub-surface defects in arbitrary size structures. Thermal tomography is a computational method for heat diffusion-based imaging of solids, which provides 3D visualization of data from flash thermography measurements. We investigate thermal tomography imaging and nondestructive evaluation of stainless steel and nickel super alloy metallic structures produced with laser powder bed fusion (LPBF) additive manufacturing (AM) process. Metallic structures produced with LPBF contain defects, and there are limited capabilities to evaluate these structures non-destructively. Thermal tomography reconstruction of 3D apparent spatial effusivity provides information about AM structure geometry and internal material flaws. We study performance of thermal tomography in imaging of metallic structures through COMSOL computer simulations of transient heat transfer, and through reconstruction of data obtained from experimental measurements. Reconstruction of internal defects is investigated using a stainless steel 316L specimen with flat bottom hole (FBH) indentations, and Inconel 718 plate produced with laser powder bed fusion (LPBF) method, which contains imprinted hemispherical shape low density regions containing non-sintered metallic powder. The FBH’s have the same sizes as the imprinted defects in the LPBF specimens, but offer better imaging contrast. Thermal tomography reconstructions provide visualizations of internal defects, and allow for estimation of their sizes and locations. Detection sensitivity of TT is limited by noises. We investigate separation of signal from noise in thermography images using several machine learning (ML) methods, including new spatio-temporal blind source separation (STBSS) and spatio-temporal sparse dictionary learning (STSDL) methods. Performance of the ML methods is benchmarked using thermography data obtained from imaging stainless steel 316L and Inconel 718 specimens produced LPBF method with imprinted calibrated porosity defects. The ML methods are ranked by F-score and execution runtime. Finally, we investigate TT of AM stainless steel 316L specimen with imprinted internal porosity defects using relatively low-cost, small form factor infrared (IR) camera based on uncooled micro bolometer detector. Sparse coding related K-means singular value decomposition (SVD) machine learning, image processing algorithms are developed to improve quality of TT images through removal of Additive white Gaussian noise without blurring the images. Following initial qualification of an AM component for deployment in a nuclear reactor, a compact TT can also be used for in-service nondestructive evaluation (NDE). With capability to perform in-service NDE of the AM component lifecycle, TT data can be used for development of a component digital twin.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

In-situ and ex-situ characterization of irradiated AM materials

This study investigates the irradiation performance of laser powder bed fusion (LPBF) 316L and 316H stainless steels (SS), and their wrought counterparts. While LPBF 316L has been more studied, LPBF 316H is relatively new, with little prior data on its irradiation behavior. The research involved fabricating, preparing, irradiating, and characterizing six materials: LPBF 316L (two variants), LPBF 316H (two variants), and wrought 316L and 316H. LPBF materials were subjected to various heat treatments, including solution annealing and stress relief, and were irradiated using in-situ and ex-situ ion techniques at temperatures of 300°C and 600°C, with doses ranging from 0.2 dpa to 25 dpa. Under ex-situ irradiation with 4 MeV Ni 2+ ions at 600°C, the dislocation cell structures in LPBF316L-1 and LPBF316H-1 gradually evolved into a uniform dislocation network. At a low irradiation dose (0.2 dpa), the cell structures were still partially visible. At 2 dpa, a uniform dislocation network formed, though remnants of the original cell structure were still discernible as contrast domains. At 5 dpa and 10 dpa, even the contrast domains vanished. For irradiation at 300°C, the cell structure was still clearly visible at 0.2 dpa for LPBF316L-1. For LPBF316H-1, the dislocation cell structure was less apparent at the same dose but was still recognizable. With further increase in dose at 300°C, the dislocation cell walls were completely replaced by irradiation-induced defects and no longer visible. Void formation was observed for irradiation at 600°C. At 2 dpa, no evident voids were observed in either LPBF316L-1 or LPBF316H-1.

36 MATERIALS SCIENCE↗

Influence of Spatter on Porosity, Microstructure, and Corrosion of Additively Manufactured Stainless Steel Printed Using Different Island Size

Specimens of 316 L stainless steel were printed using laser powder bed fusion (LPBF), a popular metal additive manufacturing (AM) technique, with varying island sizes. Not many researchers have considered the impact of spatter while optimizing LPBF printing parameters. In this research, the influence of spatter was considered while also investigating the effect of varied island size on the microstructure, surface roughness, microhardness, and corrosion resistance of LPBF-316 L. No correlation was observed between surface roughness or microhardness and minor variations in island size. However, a correlation was drawn between varied island sizes and porosity in LPBF-316 L. The specimens associated with larger island sizes showed significantly enhanced corrosion resistance due to fewer manufacturing defects and reduced porosity, attributed to the minimal influence of the spatter. Based on analysis, the LPBF parameters were revised, which lead to superior corrosion resistance of LPBF-316 L, attributed to high density and reduced porosity.

36 MATERIALS SCIENCE↗

In-Situ Characterization of Pore Formation Dynamics in Pulsed Wave Laser Powder Bed Fusion

Laser powder bed fusion (LPBF) is an additive manufacturing technology with the capability of printing complex metal parts directly from digital models. Between two available emission modes employed in LPBF printing systems, pulsed wave (PW) emission provides more control over the heat input compared to continuous wave (CW) emission, which is highly beneficial for printing parts with intricate features. However, parts printed with pulsed wave LPBF (PW-LPBF) commonly contain pores, which degrade their mechanical properties. In this study, we reveal pore formation mechanisms during PW-LPBF in real time by using an in-situ high-speed synchrotron x-ray imaging technique. We found that vapor depression collapse proceeds when the laser irradiation stops within one pulse, resulting in occasional pore formation during PW-LPBF. We also revealed that the melt ejection and rapid melt pool solidification during pulsed-wave laser melting resulted in cavity formation and subsequent formation of a pore pattern in the melted track. The pore formation dynamics revealed here may provide guidance on developing pore elimination approaches.

36 MATERIALS SCIENCE↗

Thermal stability of additively manufactured austenitic 304L ODS alloy

Thermal stability and high-temperature mechanical properties of a 304L austenitic oxide dispersion strengthened (ODS) alloy manufactured via laser powder bed fusion (LPBF) are examined in this work. Additively manufactured 304L ODS alloy samples were aged at temperatures of 1000, 1100, and 1200 °C for 100 h in an argon atmosphere. Microstructure characterization of LPBF 304L ODS alloy before and after the thermal stability experiments revealed that despite the annihilation of dislocations, induced cellular substructure by the LPBF process was partially retained in the ODS alloy even after aging at 1200 °C. The size of Y-Si-O nanoparticles after aging at 1200 °C increased from 25 to 50 nm. EBSD analysis revealed that nanoparticles retained the microstructure of LPBF 304L ODS and hindered recrystallization and further grain growth. At 600 °C and 800 °C, the yield stress of the 290 and 145 MPa were measured, respectively, which are substantially higher than 113 MPa, and 68 MPa for 304L at the same temperatures. Furthermore, the creep properties of LPBF 304L ODS alloy were evaluated at a temperature of 700 °C under three applied stresses of 70, 85, and 100 MPa yielding a stress exponent (n) of ~7.7; the minimum creep rate at 100 MPa was found to be about two orders of magnitude lower than found in the literature for wrought 304L stainless steel.

36 MATERIALS SCIENCE↗

Developing ductile and isotropic Ti alloy with tailored composition for laser powder bed fusion

Laser powder bed fusion (LPBF) is an advanced technology to create metallic components with complex geometry. Ti-6Al-4V (Ti64) is one of the most frequently used materials for LPBF. The intrinsic high cooling rates and ultra-high directional thermal gradient of melt, however, lead to a hierarchical structure composed of fine martensitic alpha' within columnar prior-beta grains in LPBF Ti64. This microstructure results in poor ductility and strong mechanical anisotropy in as-built Ti64 components, which largely limit their applications. Here, we report that the above shortcomings can be overcome by tailoring the alloy composition. Specifically, by reducing the aluminum content from 6 wt% to 4 wt%, the resultant LPBF Ti-4Al-4V (Ti44) alloy exhibits substantially improved ductility and mechanical isotropy. These improvements are attributed to grain refinement during solidification and the activation of multiple slip modes and twinning in the as-built material during deformation. This work offers a simple strategy to design new titanium alloys for LPBF with significantly improved ductility and isotropy.

36 MATERIALS SCIENCE↗

Exploring laser-material interactions of zirconium carbide under additive manufacturing conditions

Zirconium carbide (ZrC) is an ultra-high temperature ceramic with a melting temperature above 3000°C and a broad range of high temperature applications. Given the high melting and sintering temperatures of pure ZrC, producing near-net shape and fully dense parts remains challenging with conventional techniques. In this study, we investigate the fundamental laser-material interactions of ZrC under laser powder bed fusion (LPBF) additive manufacturing (AM) conditions. Normalized enthalpy, a scaling law term that is used in welding and AM literature for detailing laser-material interactions in metallic alloys, was calculated to determine the predictive capabilities of melt pool features in ZrC. Further, the melt pool quality of laser irradiated ZrC was used to compare LPBF relevant laser parameter combinations of laser power, scan speed, and beam diameter. Laser build parameters that resulted in desirable melt pool morphologies were applied to the fabrication of ZrC coupons using LPBF AM. A custom LPBF system was used to determine hatch spacing and layer height parameters that resulted in a fabricated sample with a density of 85% as measured by Archimedes and a Vicker's microhardness of 20.9 ± 1.9 GPa. This investigation reveals the laser-material interactions of ZrC under AM relevant conditions and is the first step towards LPBF fabrication of ZrC parts.

36 MATERIALS SCIENCE↗

Characterization of in-situ and ex-situ ion-irradiated additively manufactured 316L and 316H stainless steels

Additively manufactured (AM) 316 stainless steel (SS) differs from its wrought counterpart in its unique dislocation cell structure and the presence of segregation and oxide particles at the cell walls. This work investigated the evolution of the microstructure in laser powder bed fusion (LPBF) 316L and 316H SS under in-situ 1 MeV Kr ion irradiation at 600 °C to 5 dpa, and ex-situ 4 MeV Ni ion irradiation at 300 °C and 600 °C from 0.2 dpa to 10 dpa, with a dose rate for all experiments of 10 -3 dpa/s. The results reveal that the dislocation cell structure results in heterogeneous formation of dislocation loops and voids, particularly at 600 °C, where loops tend to form within the cell interiors while voids form at the cell boundaries. LPBF 316H has a reduced level of swelling compared to LPBF 316L due to prolonged incubation. Energy Dispersive X-ray Spectroscopy (EDS) mapping indicates Ni and Si segregation at void surfaces due to radiation-induced segregation. At 300 °C, where voids are absent, the distribution of dislocation loops and stacking fault tetrahedra appears to be uniform. Dislocation cell structures mostly disappeared by 2 dpa for all conditions in this work. M 23 C 6 carbides were observed in LPBF 316H at 600 °C as early as 0.2 dpa, but not in LPBF 316L. Nanoindentation was performed to obtain the hardness of irradiated materials. In conclusion, this work illustrated the influence of additive manufacturing processes on microstructure evolution under irradiation, revealing the differences as well as the similarities as compared with wrought 316 SS, and the AM-related phenomenon that can potentially occur under neutron irradiation in nuclear reactors.

36 - MATERIALS SCIENCE↗

Solidification and crystallographic texture modeling of laser powder bed fusion Ti-6Al-4V using finite difference-monte carlo method

Laser powder bed fusion (LPBF) additive manufacturing makes near-net-shaped parts with reduced material cost and time, rising as a promising technology to fabricate Ti-6Al-4V, a widely used titanium alloy in aerospace and medical industries. However, LPBF Ti-6Al-4V parts produced with 67° rotation between layers, a scan strategy commonly used to reduce microstructure and property inhomogeneity, have varying grain morphologies and weak crystallographic textures that change depending on processing parameters. Here, this study predicts LPBF Ti-6Al-4V solidification at three energy levels using a finite difference-Monte Carlo method and validates the simulations with large-area electron backscatter diffraction (EBSD) scans. The developed model accurately shows that a <001> texture forms at low energy and a <111> texture occurs at higher energies parallel to the build direction but with a lower strength than the textures observed from EBSD. A validated and well-established method of combining spatial correlation and general spherical harmonics representation of texture is developed to calculate a difference score between simulations and experiments. The quantitative comparison enables effective fine-tuning of nucleation density (N 0 ) input, which shows a nonlinear relationship with increasing energy level. Future improvements in texture prediction code and a more comprehensive study of N 0 with different energy levels will further advance the optimization of LPBF Ti-6Al-4V components. These developments contribute a novel understanding of crystallographic texture formation in LPBF Ti-6Al-4V, the development of robust model validation and calibration pipeline methodologies, and provide a platform for mechanical property prediction and process parameter optimization.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Critical role of slags in pitting corrosion of additively manufactured stainless steel in simulated seawater

Abstract Pitting corrosion in seawater is one of the most difficult forms of corrosion to identify and control. A workhorse material for marine applications, 316L stainless steel (316L SS) is known to balance resistance to pitting with good mechanical properties. The advent of additive manufacturing (AM), particularly laser powder bed fusion (LPBF), has prompted numerous microstructural and mechanical investigations of LPBF 316L SS; however, the origins of pitting corrosion on as-built surfaces is unknown, despite their utmost importance for certification of LPBF 316L SS prior to fielding. Here, we show that Mn-rich silicate slags are responsible for pitting of the as-built LPBF material in sodium chloride due to their introduction of deleterious defects such as cracks or surface oxide heterogeneities. In addition, we explain how slags are formed in the liquid metal and deposited at the as-built surfaces using high-fidelity melt pool simulations. Our work uncovers how LPBF changes surface oxides due to rapid solidification and high-temperature oxidation, leading to fundamentally different pitting corrosion mechanisms.

36 MATERIALS SCIENCE↗

Cost of Using Laser Powder Bed Fusion to Fabricate a Molten Salt-to-Supercritial Carbon Dioxide Heat Exchanger for Concentrating Solar Power

Advances in manufacturing technologies and materials are crucial to the commercial deployment of energy technologies. We present the case of concentrating solar power (CSP) with molten salt (MS) thermal storage, where low-cost, high-efficiency heat exchangers (HXs) are needed to achieve cost competitiveness. Here, the materials required to tolerate the extreme operating conditions in CSP systems make it difficult or infeasible to produce them using conventional manufacturing processes. Although it is technically possible to produce HXs with adequate performance using additive manufacturing, specifically laser powder bed fusion (LPBF), here we assess whether doing so is cost-effective. We describe a process-based cost model (PBCM) to estimate the cost of fabricating a MS-to-supercritical carbon dioxide HX using LPBF. The PBCM is designed to identify modifications to designs, process choices, and manufacturing innovations that have the greatest effect on manufacturing cost. Our PBCM identified HX design and LPBF process modifications that reduced projected HX cost from $\$750$ per kilo-Watt thermal (kW-th) ($\$8$ /cm 3 ) to $\$350$ /kW-th ($\$6/$ cm 3 ) using currently available LPBF technology, and down to $\$220$ /kW-th ($\$4$ /cm 3 ) with improvements in LPBF technology that are likely to be achieved in the near term. The PBCM also informed a redesign of the HX design that reduced projected costs to $\$140$ –160/kW-th ($\$3$ /cm 3 ).

36 MATERIALS SCIENCE↗

Embedding Sensors in 3D Printed Metal Structures

The Transformational Challenge Reactor (TCR) program is leveraging recent advances in modeling and simulation, materials, and additive manufacturing (AM) technologies to design a modern nuclear reactor. Some of the main TCR technologies include in situ monitoring and the integration of sensors during the manufacturing of quality-significant nuclear reactor components. This report describes the general procedure and process optimization for embedding sensors within generic stainless steel 316 (SS316) components using laser powder bed fusion (LPBF). A more detailed, quality-significant test plan and supporting procedures are available upon request (ORNL/TM-2021/2127). LPBF involves the use of a scanning laser to selectively melt regions of a powder bed, additively building a part layer by layer. This report describes the LPBF processing technique and discusses the effects of LPBF processing parameters on the success of the sensor embedding process. Experiments used machined cavities in the form of channels in an SS316 base for the sensors to lay in while material is additively built over the top, thereby embedding them in an SS316 matrix. A preliminary investigation involved using empty SS316 sheaths as surrogates to explore the effects of various LPBF processing parameters and the dimensional requirements of the machined channels. Microstructural investigations showed that a smaller channel width/depth combination closer to the sensor’s diameter was best for the embedding process. After the desired parameters were selected, Type-K thermocouples were embedded and evaluated post-embedding using nondestructive thermal testing, as well as destructive sectioning and microscopy. Post-build characterization showed that the thermocouples were well-bonded to the SS316 matrix and were fully functional after embedding. During thermal testing to temperatures up to 500 °C, the embedded thermocouples read consistently with one another and deviated only slightly from the readings of a nonembedded thermocouple located within the furnace. This slight discrepancy was most likely due to differences in the thermal time constants for a nonembedded thermocouple vs. a thermocouple embedded in a solid SS316 block. The results presented in this report will serve as the foundation for future work that will focus on embedding sensors in relevant TCR reactor components and eventually testing those components under neutron irradiation.

36 MATERIALS SCIENCE↗

Analysis of Defects in Metal Additive Manufacturing with Augmented Data Generation

Laser powder bed fusion (LPBF) is a method of additive manufacturing (AM) that selectively melts and fuses together microscopic metallic powder. LPBF offers the benefit of producing custom structures out of high strength metals that can be difficult to fabricate with conventional methods. The challenge of LPBF is that 3D printed structures often have internal pores due to process flaws. Pulsed thermal tomography (PTT) is a method for reconstructing the depth profile of materials, allowing the visualization internal voids in solids. In prior work, we developed a convolutional neural network (CNN) which, having been trained on simulated 2D PTT images of subsurface elliptical defects, was able to classify the semi-major radii, semi-minor radii, and angular orientation of the best-fit ellipses in previously unseen PTT images. The unseen PTT images contained subsurface irregular defect shapes imported from scanning electron microscopy (SEM) images of metallic LPBF-printed specimens. Training the CNN on irregular defect shapes instead of on elliptical shapes would make the resulting classifications more descriptive of actual defect shapes. However, this requires a much higher volume of SEM images of material defects, which are difficult to obtain because of random occurrence of defects in LPBF. To address this challenge, we developed a generative adversarial network (GAN) to augment the existing dataset of SEM defect images. The GAN model is demonstrated to create novel yet realistic defect shapes that can be used as input for simulated PTT images to train CNN.

36 MATERIALS SCIENCE↗

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing with a specific focus on laser powder bed fusion (LPBF). As an initial case study, the program has selected 316H stainless steel (SS) as an initial material around which to develop a code case development strategy. This strategy involves two parallel approaches: (1) an equivalency approach whereby round-robin testing across multiple collaborating laboratories demonstrates repeatability in processing and direct comparisons with conventional wrought 316H material and (2) a revolutionary approach to code qualification combining in situ data collection and high-fidelity modeling to capture, predict, and bound the performance of LPBF 316HSS components. As part of this campaign, this work package has initiated an extensive process optimization campaign across three laboratories, each printing variations of LPBF 316HSS using three different LPBF units (Concept Laser, EOS, and Renishaw). In FY23, ORNL has focused on unique experimental designs spanning wide ranges in energy inputs and turning knobs such as scan speed, laser power, hatch spacing, layer thickness, spot size, scan rotation, and more. On the Concept Laser M2, 72 different combinations of processing variables were investigated with duplicate samples and different powder compositions. In total, 252 samples were printed with combined in situ sensing data. A parallel design of experiments was conducted on the Renishaw AM400 with an additional 390 printed specimens for analysis. All 642 miniature specimens, each with unique features included in each print to capture geometry-related heterogeneity, were subjected to high-throughput x-ray computed tomography (XCT) analysis to enable the downselection of specific processing parameters of interest. Then, using electrical discharge machining (EDM), miniature tensile specimens were extracted for mechanical testing and microscopy investigations. From the analysis performed in FY23, it was found that powder composition drastically affects the resulting microstructure and mechanical performance of 316SS. Specifically, changing from 316L to 316HSS powder results in a wide range of grain sizes with varying degrees of preferred grain orientation, which increases as a function of energy density. It was also found that due to stored heat in thin fin–type features, large microstructural differences can be seen within one part printed with one set of processing parameters. These variations in microstructure features, including grain size, the nanoscale dislocation structure, and grain texture, will all affect the irradiation performance and high-temperature mechanical performance of LPBF 316HSS parts. Two sets of concept laser processing parameters, spanning both refined and columnar grain structures, were scaled to print larger 316H builds for campaign testing (high-temperature creep and irradiation). In addition, at least two optimized processing parameter sets were identified for the Renishaw AM400 for round-robin testing in FY24 with Argonne National Laboratory. Future work includes printing samples using identical parameters identified by partner institutions, providing material for corrosion and high-temperature mechanical testing, and continuing evaluations of heterogeneity in larger printed parts.

36 MATERIALS SCIENCE↗

Data-Driven Optimization of the Processing Window for 316H Components Fabricated Using Laser Powder Bed Fusion

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing with a specific focus on laser powder bed fusion (LPBF). As an initial case study, the program has selected 316H stainless steel (SS) as an initial material around which to develop a code case development strategy. This strategy involves two parallel approaches: (1) an equivalency approach whereby round-robin testing across multiple collaborating laboratories demonstrates repeatability in processing and direct comparisons with conventional wrought 316H material and (2) a revolutionary approach to code qualification combining in situ data collection and high-fidelity modeling to capture, predict, and bound the performance of LPBF 316HSS components. As part of this campaign, this work package has initiated an extensive process optimization campaign across three laboratories, each printing variations of LPBF 316HSS using three different LPBF units (Concept Laser, EOS, and Renishaw). In FY23, ORNL has focused on unique experimental designs spanning wide ranges in energy inputs and turning knobs such as scan speed, laser power, hatch spacing, layer thickness, spot size, scan rotation, and more. On the Concept Laser M2, 72 different combinations of processing variables were investigated with duplicate samples and different powder compositions. In total, 252 samples were printed with combined in situ sensing data. A parallel design of experiments was conducted on the Renishaw AM400 with an additional 390 printed specimens for analysis. All 642 miniature specimens, each with unique features included in each print to capture geometry-related heterogeneity, were subjected to high-throughput x-ray computed tomography (XCT) analysis to enable the downselection of specific processing parameters of interest. Then, using electrical discharge machining (EDM), miniature tensile specimens were extracted for mechanical testing and microscopy investigations. From the analysis performed in FY23, it was found that powder composition drastically affects the resulting microstructure and mechanical performance of 316SS. Specifically, changing from 316L to 316HSS powder results in a wide range of grain sizes with varying degrees of preferred grain orientation, which increases as a function of energy density. It was also found that due to stored heat in thin fin–type features, large microstructural differences can be seen within one part printed with one set of processing parameters. These variations in microstructure features, including grain size, the nanoscale dislocation structure, and grain texture, will all affect the irradiation performance and high-temperature mechanical performance of LPBF 316HSS parts. Two sets of concept laser processing parameters, spanning both refined and columnar grain structures, were scaled to print larger 316H builds for campaign testing (high-temperature creep and irradiation). In addition, at least two optimized processing parameter sets were identified for the Renishaw AM400 for round-robin testing in FY24 with Argonne National Laboratory. Future work includes printing samples using identical parameters identified by partner institutions, providing material for corrosion and high-temperature mechanical testing, and continuing evaluations of heterogeneity in larger printed parts.

36 MATERIALS SCIENCE↗

Manufacturability and performance response of developed Ni-based alloys for reactor environments

Under the Advanced Materials and Manufacturing Technologies program, two Ni-based alloys fabricated by laser powder bed fusion (LPBF) at Oak Ridge National Laboratory and by laser powder directed energy deposition (LP-DED) at Idaho National Laboratory have been evaluated: γ′-strengthened Haynes 282 and solution-strengthened Inconel 625. Printing defects were observed in the LPBF 282 alloy fabricated using a Renishaw AM250 machine, likely due to particle spattering during printing. For both the LPBF and LP-DED 282 alloys, annealing at 1,180°C for 1 h resulted in partial recrystallization and a bimodal grain distribution, and subsequent aging for 4 h at 800°C led to the formation of a high density of nano-size γ′-strengthening precipitates. Creep testing performed at 750°C revealed lower creep life and ductility for the LPBF and LP-DED 282 compared with wrought 282. X-ray computed tomography combined with optical and scanning electron microscopy microstructural characterization revealed crack formation in the LPBF 282 alloy during creep testing, initiated either from printing defects or from creep cavitation at grain boundaries. Creep cavitation and cracking at grain boundaries were also observed for the LP-DED 282 alloy, and optimization of the printing strategies and postheat treatments will be needed to fabricate high-performance 282 components for high-temperature nuclear applications.

36 MATERIALS SCIENCE↗