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Brazing characteristics, microstructure, and wettability of laser powder bed fusion additive manufactured GRCop-84 compared to CuCrZr and OFC, and brazing to titanium-zirconium-molybdenum alloy limiters

Laser Powder Bed Fusion (L-PBF) of Glenn Research Copper 84 (GRCop-84), a Cr 2 Nb (8 at. % Cr, 4 at. % Nb) precipitation hardened alloy, produces a fully dense, high conductivity alloy with a yield strength of 500 MPa and ultimate tensile strength (UTS) of 740 MPa with 20% elongation; superior to other competing copper alloys. Braze wetting characteristics of GRCop-84 with Ag-Cu-X, and Au-Cu brazes were similar to CuCrZr, but less than oxygen free copper. No difference in wetting was observed between infill and surface contour areas in L-PBF GRCop-84. Wet sanding to 240 grit (R a =0.24 µm) was considered the optimal surface condition. Silver diffusing through GRCop-84 depleted Cr 2 Nb precipitates from the copper grain and deposited agglomerations of coarsened precipitates within silver-rich regions of intergranular diffusion once a density threshold was reached. Microstructure modification was minimized with 50Au-50Cu braze implying that silver caused precipitate coarsening and agglomeration, and not high temperature exposure. Coarsened precipitates were observed on the surface within braze pools implying a contribution to braze wetting. Palcusil-25, Ticusil, CuSil-ABA, and 50Au-50Cu brazes were suitable for brazing to unplated Titanium-Zirconium-Molybdenum (TZM), while sulfamate nickel plating to allows wetting with CuSil or other non-active brazes. Additionally, vacuum brazing techniques were developed to join a 1 mm thick layer of TZM to the front of additive manufactured GRCop-84 waveguides considering the brazing characteristics of both GRCop-84, TZM, and internal stress from the difference in coefficient in thermal expansion.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Predictive Tools for Customizing Heat Treatment of Additively Manufactured Aerospace Components

Laser-bed powder fusion (LBPF) additive manufacturing is increasingly being used to produce components of complex geometries using the Ni-base superalloy Inconel 718. The composition and the microstructure of the alloy are currently well optimized for wrought components made using conventional manufacturing processes such as rolling, forging, extrusion, etc. The attractive mechanical properties of the alloy result from the underlying austenitic matrix with fine equiaxed grains, and a high density and uniform distribution of the precipitation hardening phase, γ". Heat treatment steps such as homogenization, solutioning and aging are well documented for the wrought alloy. However, when the same wrought alloy compositions are used for the additive manufacturing (AM) processes, the asprocessed microstructure is significantly different, because of the different thermal history associated with LBPF, including rapid solidification and multiple temperature excursions that lead to multiple re-melting and reheating in the solid state. Rapid solidification introduces potential non-equilibrium effects at the moving solid-liquid interfaces that impact the extent of solute segregation, as well as the morphology of the dendritic grains that form. In order to recover the target mechanical properties, AM components have to undergo post-process heat treatments. However, such heat treatments have to be custom designed for the AM process and the component geometry because of the expected vast differences in the microstructure at various locations of a component with complex geometry. The homogenization and precipitation steps should be optimized for the component so that target mechanical properties can be obtained throughout the part. The objective of this research is to utilize High Performance Computing in phase field simulations of microstructure evolution during post-processing of AM components. The physics-based modeling will be beneficial in reducing the experimental effort required for heat treatment process selection, optimization, and certification, thus leading to a significant reduction in energy consumption for AM and post-processing heat treatment. The optimization study will help identify heat treatments steps that are critical for development of a final desired microstructure with the minimum energy input. This combined with shortening of the production cycle (time-to-market) by reducing the number of failed parts (property targets), and reduction in the number of iterations for process optimization, will enable 30-40% savings in the energy costs. Phase field simulations of the degree of homogenization and the effect of local matrix composition on the nucleation and growth of competing precipitating phases were performed using the Microstructure Evolution Using Massively Parallel Phase Field Simulations code developed in-house at the Oak Ridge National Laboratory. The simulations were able to successfully capture the kinetics of nucleation and growth, and morphologies of various precipitating phases as a function of local matrix compositions and composition gradients characteristic of local microstructures arising from location-dependent variations in the thermal conditions. Future work will involve extending the simulations to a length scale consisting of multiple dendrites, so that the effect of homogenization on the coarsening of the dendrites can be simulated and used as an additional input to the optimization of the heat treatment process.

36 MATERIALS SCIENCE↗

Mechanical Behavior of Neutron Irradiated Refractory Multi-Principal Element Alloys Processed via Spark Plasma Sintering

The search for advanced materials capable of withstanding the extreme conditions of Generation IV reactors is a critical area in materials science research. These reactors operate under severe environments, including high temperatures, corrosion, stress, and irradiation damage. Consequently, there is a need for innovative alloy systems to ensure the reliability and longevity of proposed Generation IV reactor components. Refractory multi-principal-element alloys (RMPEA) have emerged as a promising candidate due to their exceptional properties. These alloys, characterized by their composition of multiple principal elements in near-equiatomic ratios, exhibit superior resistance to irradiation damage, reduced void swelling, enhanced microstructural stability, and minimal irradiation-induced hardening. While initial studies on RMPEAs have shown promising results, most research has been limited to thin films, nanocrystalline microstructures, and ion irradiation, which do not accurately represent the behavior of bulk materials. To address this gap, our research focused on the neutron irradiation of bulk RMPEAs. We aim to conduct comprehensive post-irradiation examinations (PIE) of RMPEAs irradiated at the Advanced Test Reactor at Idaho National Laboratory. The RMPEAs were synthesized using spark plasma sintering (SPS) with mechanically alloyed metallurgical powder. The RMPEA specimens are a MoNbTi alloy system with additions of -Zr, and -ZrV. Furthermore, PIE consisted of mechanical testing and advanced materials characterization. The mechanical testing consisted of sub-sized tensile testing, micro- and nano- indentation. Microstructural characterization included scanning electron microscopy and transmission electron microscopy. Mechanical testing coupled with advanced microscopy techniques provides insight into phase morphology and its effects on the mechanical properties of the RMPEA specimens. The results indicate that both pristine and irradiated RMPEA specimens exhibited brittle behavior during tensile testing, which can be attributed to their heterogeneous microstructure. The SPS manufacturing process did not include any post treatment, which resulted in a heterogeneous microstructure. Energy-dispersive X-ray spectroscopy revealed the presence of intermetallic such as laves phases within the microstructure. Specifically, Ti-rich precipitates were observed in the MoNbTi specimen, while Mo-rich precipitates were found in the MoNbTiZrV specimen. Nano-hardness testing of pristine samples showed that the laves phases exhibited higher hardness values compared to the matrix phase, suggesting that precipitate hardening is likely the dominant hardening mechanism in these specimens. The results from this work will be used to build a finite element model to predict mechanical behavior of future MPEA compositions. Thus, enabling for a streamlined approach to developing novel MPEAs for the nuclear industry.

36 - MATERIALS SCIENCE↗

Structural integrity of additively manufactured stainless steel with cold sprayed barrier coating under combined cyclic loading

Integration of metal additive manufacturing (AM) and cold spray (CS) technologies provide an unprecedented opportunity to manufacture coated material systems with complex geometrical features. The application of these material systems in functionally critical components requires adequate structural integrity, particularly in the presence of cyclic loading. This article researches the multiaxial fatigue (axial-torsional cyclic loading) behavior of a coated material system consisting of 15Cr-5Ni precipitation-hardening stainless steel (15-5 PH SS) substrate additively manufactured by direct metal laser sintering with a layer of chromium carbide nickel (CrC-Ni) barrier coating deposited by CS. The influence of AM and CS-induced residual stresses on fatigue performance of test specimens was thoroughly studied. Additionally, the effect of surface roughness and processes induced defects were considered to explain the crack growth mechanism. Stresses assessed by synchrotron X-ray diffraction indicated a substantial accumulation of residual stresses, particularly in the outer surface of the as-fabricated 155 PH SS specimens. The state of residual stress was changed notably following the deposition of CrC-Ni coating in the axial, hoop, and radial directions of the fatigue test specimen. Also, CS deposition of CrC-Ni coating caused significant improvement in the surface quality of the additively manufactured components. Fatigue test results indicated, CS deposition of CrC-Ni substantially enhances the fatigue life of the AM-produced 15-5 PH SS substrate in all loading conditions, particularly in the high cycle fatigue regime. The improvement in the fatigue life of the specimens with coating was associated with a reduction in equivalent residual stress at the substrate surface and improvement in the specimens' surface condition (i.e., reduced surface roughness). The fractographic analysis of the specimen indicated the cracks tend to initiate in the surface of both as-fabricated and cold-sprayed specimens. However, the mechanism of crack growth changed notably following the deposition of CrC-Ni coating. The cracks tended to propagate in the planes parallel or with a small deviation from the build layers of the AM-produced specimens. On the other hand, deposition of CrC-Ni coating increased the deviation of crack growth plane from the build layers of the substrate.

36 MATERIALS SCIENCE↗

Peak microhardness recovery via T6 heat treatment with extremely soft annealed Al7075 feedstock in additive friction stir deposition

With standard T6 heat treatments, precipitate-hardened alloys such as Al7075 and Al6061 fabricated using Additive Friction Stir Deposition (AFSD) method restore to noticeablely different peak mechanical properties. Previous research observed similar results but did not provide a viable solution. This study proposes a new processing strategy, namely enhanced plastic deformation by subjecting the Al7075 feedstock to annealed softening treatments. Specifically, by annealing the standard T651-Al7075 feedstock and deposition substrate (179 HV), their Microhardness were first degraded to its lowest state (80 HV), which is called a Soft-to-Soft system. For the Soft-to-Soft system subjected to AFSD, after undergoing appropriate T6 heat treatment, the microhardness of the AFSD 7075 alloy was restored to its peak value (183.1 ± 1.8 HV). The results indicate that this softening strategy can effectively reduce the non-strengthening phase in the AFSD matrix, thereby increasing the strengthening phase (η′ phase). This addresses the issue of traditional AFSD-prepared aluminum alloys being unable to achieve peak performance through T6 heat treatment.

36 MATERIALS SCIENCE↗

Unearthing principal strengthening factors tuning the additive manufactured 15-5 PH stainless steel

Additive manufactured (AM) materials exhibit enhanced performance, while post-processing is essential to reinforce its properties. Controlling the tunable factors and the underlying strengthening mechanisms during the post-processing are a key to answering the calls from the industry and end users. We identified the principal strengthening factors that contribute to AM stainless steel under heat-treatment and weighed their importance. The as-built sample exhibited a unique microstructure with a heterogeneous grain size distribution, a small amount of retained austenite, high dislocation density, and dispersed oxide particles. The strengthening primarily by dislocation forest and additionally by heterogeneous grain size contributed to the as-built sample. Although aging slightly decreased dislocation strengthening, superior aging enhancement was achieved by Cu-precipitates. The solid-solutionizing not only increased the effective grain size but also reduced the dislocation density by eliminating the heterogeneous microstructure, which deteriorated the precipitation hardenability. Our findings shed light on the performance optimization of AM metals.

36 MATERIALS SCIENCE↗

Microstructure-based prediction of thermal aging strength reduction factors for grade 91 ferritic-martensitic steel

This study aimed to develop a microstructure-based mechanistic approach to address the long-term thermal aging effect on yield stress and ultimate tensile strength and to provide a physical basis for developing thermal aging factors for G91 for a design life of 60 years. Several heats of G91 steel were examined. Controlled aging experiments were conducted on two heats at temperatures of 550, 600, and 650 °C for times up to ~64,000 h. Specimens were also taken from archived creep-tested specimens of G91 and from a tube removed from the Kingston coal-fired power plant to obtain data that cover a wide range of temperatures and for aging times up to 155,000 h. Thermal aging caused significant subgrain recovery, coarsening of M 23 C 6 carbides at subgrain boundaries and MX carbonitrides within subgrains. The intermetallic Laves phase forms during aging and grows rapidly. The growth rate of the subgrain width and MX mean size during thermal aging were described by kinetic models. Thermal aging results in the reductions in the yield stress and the ultimate tensile strength of G91. The effects of thermal aging on the reductions in yield stress and ultimate tensile strength were well described by the microstructure-strength model that considers three superimposed strengthening mechanisms, namely, sub-boundary strengthening, MX precipitation hardening, and Mo solid solution strengthening. Furthermore, the model was independently validated by the ASME Code values and is being used by the ASME to develop the aging-induced strength reduction factors for G91 steel for a design life of 60 years.

36 MATERIALS SCIENCE↗

Crack mitigation and wear performance of high-strength steel coatings deposited by high-speed laser cladding

This article investigates the fabrication of defect-free Rockit® 606, a high‑carbon, vanadium- and chromium-enriched precipitation-hardening martensitic steel coating, using high-speed laser cladding (HSLC). Compared to conventional laser cladding, HSLC offers higher deposition efficiency, improved coating quality, minimal thermal distortion, and a reduced heat-affected zone. Various HSLC parameters—including laser power, travel speed, powder feed rate, and overlap distance—were optimized to achieve superior coating properties. Microstructural analysis revealed solidification cracks in coatings deposited on carburized steel, regardless of processing parameters. However, preheating the substrate to 250 °C effectively eliminated cracking by reducing thermal gradients. The coatings exhibited a columnar dendritic microstructure, with coarser dendrites near the substrate and finer dendrites towards the surface. Hardness measurements confirmed that all coatings significantly exceeded the industry-specified threshold of 60 HRC, with preheating having minimal effect on overall hardness distribution. Reciprocating sliding wear tests demonstrated a substantial improvement in wear resistance for the defect-free HSLC coatings compared to baseline carburized steel. These findings underscore the potential of HSLC for producing high-performance, wear-resistant coatings suitable for industrial applications.

36 MATERIALS SCIENCE↗

Dynamic response of 17-4 stainless steel as a function of manufacturing method and heat treatment

We present a series of plate-impact experiments on 17-4 stainless steel to study the effect of manufacturing method and heat treatment on the Hugoniot elastic limit (HEL), Hugoniot, phase transformation stress, and spallation strength. Two traditional manufacturing methods were considered, wrought processing and casting, as well as two additive manufacturing methods, laser powder-bed fusion (LPBF) and wire-fed electron beam (EBAM). For both LPBF and EBAM 17-4 stainless steel variants, two billets were printed, enabling the application of two unique heat treatments. The HEL stress depended heavily on the thermal history, with the HEL increasing after the formation of Cu-rich precipitates via heat treatment. The Hugoniot response both below and above the phase transition was unaffected by the manufacturing method or heat treatment. The phase transition stress depended heavily on the thermal history, with its variation being attributed to the presence of various microstructural features. This is supported by a marked increase in the phase transition stress after precipitation hardening. These results suggest that the notion of the phase transition stress being dictated by bulk composition is an oversimplification and the stress fields generated by the meso-scale structure are a dominant force. The spallation strength was lower in the cast material compared to all other 17-4 stainless steel variants due to the presence of brittle δ-ferrite inclusions. Additionally, a drop in the tensile strain-rate was observed in the spallation response above the phase transition stress, which was hypothesized to stem from the kinetics of the reversion to the low-pressure phase during spall.

Compressive stress↗

Chemical and Chemical-Mechanical Polishing of Surface Roughness on L-PBF/GRCop-42 Cu-Cr-Nb Additive Manufactured 10-GHz RF Structures

Laser-based powder bed fusion (L-PBF) allows additive manufacture (AM) of lower hybrid current drive (LHCD) radio-frequency (RF) launchers from Glenn Research Copper, a Cr 2 Nb precipitation-hardened alloy (GRCop-42) in configurations unachievable with conventional machining. Rough surfaces in AM components increase RF losses and lead to arcing in high-power vacuum RF applications. Chemical polishing, chemical-mechanical polishing, or a combination of both were utilized to planarize the internal surfaces of RF structures, resulting in surface roughness as low as R a = 0.2 µm. Refinement in polishing techniques now enables GRCop-42 alloys (4 at. % Cr, 2 at. % Nb) to achieve similar surface roughness to GRCop-84 (8 at. % Cr, 4 at. % Nb) and equivalent cavity losses to extruded oxygen-free copper waveguides at 10 GHz.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Effect of deposition rate on microstructure and mechanical properties of 17-4 PH stainless steel fabricated by laser engineered net shaping

Laser engineered net shaping (LENS) is an additive manufacturing technique for fabricating and repairing metallic components. However, the relationships between its process parameters and the resulting mechanical properties of alloys such as 17-4 precipitation-hardening (PH) stainless steel require further investigation to enable reliable application. This study examines the specific effect of LENS deposition rate on the microstructure and mechanical properties of 17-4 PH stainless steel. Specimens were fabricated at two different deposition rates (8.47 and 9.31 mm s−1), subjected to subsequent solution and H900 aging treatment, and then evaluated via tensile testing, hardness measurements, and microscopy. A higher deposition rate results in a finer grain structure but increased porosity, leading to greater ultimate tensile strength (∼1294 MPa) yet lower ductility (strain at failure ∼5.8%) compared to the slower deposition rate (∼1266 MPa, ∼9.0% strain). Hardness follows the same trend as tensile strength. Tensile fracture surfaces for both conditions exhibited a mixed mode of ductile dimples and brittle quasi-cleavage regions, with chromium/silicon oxide particles identified within dimples. Complementary finite element modeling indicates that small void fractions primarily reduce ductility by enhancing localized plasticity, with only a marginal decrease in tensile strength. These integrated experimental and numerical results elucidate the mechanical properties linked to deposition rate, providing insight into tailoring LENS processes to achieve desired properties of 17-4 PH stainless steel.

17-4 PH stainlesssteel↗

Materials for Advanced Ultra-Supercritical (A-USC) Steam Turbines --- A-USC Component Demonstration

The U.S. Advanced Ultra-Supercritical (A-USC) Consortium was formed in 2001 as a government/industry program, sponsored by the U.S. Department of Energy (DOE) and the Ohio Coal Development Office (OCDO) and cost shared by industrial and not-for-profit partners. The purpose of the consortium was to advance the state of the art for power generation by evaluating and developing materials that allow the use of advanced steam cycles in coal-based power plants. These advanced cycles, with steam temperatures up to 1400°F (760°C), can increase the efficiency of coal-fired boilers from an average of 35% (current U.S. fleet) to more than 45% higher heating value (HHV) (>49% lower heating value [LHV]). The increase in a plant’s efficiency is limited unless new materials able to withstand these higher operating temperatures and pressures are identified and approved for use. The A-USC Consortium identified these needed materials during earlier phases of the program. It developed the welding and joining techniques along with manufacturing processes for casting and wrought products made from these new high-nickel alloys. It subjected these materials to extensive laboratory and steam loop testing. It then obtained ASME code approval for their use in U.S. boiler systems. The program’s successes leave this last remaining activity (ComTest Phase 2) that the U.S. utility industry has recommended to be accomplished prior to commercialization. The focus of the activity is the evaluation and demonstration of commercial readiness for “full scale” components to be made from these nickel-based alloy materials and provided by a U.S. domestic supply chain that is new to working with these alloys. According to studies completed by the Electric Power Research Institute (EPRI), the cost of an A-USC plant is approximately 20% higher than a non-A-USC plant because of its use of nickel-based alloys needed for the high temperature operating conditions. However, CO 2 reductions of approximately 30% from the current fleet average provide a strong incentive for its consideration. The actual costs and perceived value for CO 2 abatement will determine whether new or retrofitted plants are undertaken, although decisions to build A-USC plants in India would indicate its economic feasibility while also being part of a global carbon emissions strategy. The work by the A-USC Consortium, prior to the start of the ComTest project, has included lab scale and pilot scale materials testing, both in air and oxy-combustion. This testing has included air-cooled and steam-cooled “loops” that were installed into existing operating utility boilers to gain exposure of these materials to realistic conditions of high temperature and corrosion caused by the constituents in the coal ash. The A-USC Consortium also gained ASME Code approval of the Inconel 740 material, has cast and extruded the largest high nickel precipitation hardened alloys, and developed unique welding techniques to avoid problems identified by the competing European program. However, as valuable as these material test loops and accomplishments have been for obtaining information, their scale is below that required to minimize the risk associated for a U.S. utility to build a multibillion-dollar A-USC power plant. To reduce the final identified risk barrier to full-scale commercialization of these advanced materials and systems, the A-USC Consortium (guided by a utility industry advisory committee) has identified the key areas of the technology they desire to see as being capable of full-scale manufacturing and/or fabrication from an identified, capable U.S. domestic supplier base. A significant amount of work was accomplished during Phase 1 to identity the components, as well as the component size, that would be manufactured from advanced alloys such as Inconel 740H or Haynes 282 alloys. Pathways to supply these components for ComTest have been identified, as well as any further development that would be required. The Phase 2 effort used Phase 1 findings for designing these key full-scale components for A-USC boilers and turbines to include large castings; extrusions, forgings, fabrication of water walls and steam loops with headers from advanced materials, raw material (such as pipe extrusion billets) are at the commercial readiness level to permit advancement to a demonstration project. The Phase 2 work scope was addressed by a diverse team, including government, industry, and not-for-profit partners. The work scope under Phase 2 addressed fabrication of components identified as being outside of the proven capabilities of the existing supply chain, including the following: Steam turbine rotor forging and Haynes 282 nozzle carrier casting Superheater and reheater header and tube assemblies Large-diameter pipe extrusions and forgings Test valve articles to support ASME Code approval. In addition, key fabrication steps were completed, including boiler weld overlays and simulated field repairs. Throughout, extensive inspection and quality assurance testing of the components were performed. The team worked to advance ASME Code approval for key components and processes. Although much of the focus of ComTest Phase 2 was the high-temperature nickel-based alloy materials, a broader range of materials were incorporated, which would be representative of the materials used in full-scale A-USC power plant applications and have cross-cutting applicability on other high-temperature power generation options, such as advanced nuclear, supercritical CO 2 cycles, and central solar receivers. This report that has been submitted is organized in the following manner: Section 1 contains an Executive Summary. Section 2 discusses the ComTest project background and organization. Section 3 discusses project management and reporting. Section 4 discusses the procurement of nickel-based alloy and other A-USC materials and components. Section 5 discusses the fabrication of procurement of nickel-based alloy and other A-USC materials and components. Section 6 discusses the fabrication of cast nickel-based A-USC steam turbine components. Section 7 discusses the fabrication of forged nickel-based A-USC steam turbine piping and steam pipe components. Section 8 discusses the qualification of pressure relieve valves (PRVs) for A-USC power plants. Section 9 discusses proposed plans for future evaluation of A-USC components. Section 10 contains the summary and conclusion.

01 COAL, LIGNITE, AND PEAT↗

Second Target Station Target Segment PIE Dose Estimates

The purpose of the analysis described in this document is to support post irradiation examination (PIE) future decisions as related to the Second Target Station (STS) Project. The STS Project is discussing plans for future PIE studies, and the radionuclide inventories and dose rates included in this study will aid decision makers as they consider the need for various PIE-related machinery. Three configurations of the lasagna-type target segment are evaluated for this analysis: a single bare tungsten plate, a slice of the segment containing a single tungsten plate, and the upstream half of a segment. The lasagna type target segment used in this analysis has a precipitation hardenable nickel alloy (UNS N07718 or inconel 718) shroud, copper (C10100) cladding, and pure tungsten plates. The target segment is evaluated for 10 years of operation followed by two decay periods: 6 months and 2 years. For each decay period, decay gamma dose rates are tallied 30 cm from the upstream, downstream, top, bottom, and sides of the configurations. Radionuclide inventories are also provided in this report separated by material. The highest dose rates calculated in this study are 2872 rem/hr 30 cm away from the top and bottom of the half-target configuration after 6 months of decay.

36 MATERIALS SCIENCE↗

Feature Based Qualification of 17-4PH Stainless Steel to Evaluate Location-Specific Variability in Wire Arc Additive Manufacturing

Qualifying large-scale metal additive manufacturing (M-AM) technologies such as wire arc additive manufacturing (WAAM) can be challenging. This is especially significant in precipitation hardened martensitic stainless steels like SS 17-4PH, where thermal histories induce location-specific microstructural variability and property anisotropy. The Department of Defense (DOD) and the United States Army Combat Capabilities Development Command Ground Vehicle Systems Center (GVSC) Ground Vehicle Materials Engineering (GVME) aim to build robust and qualified large-scale M-AM workflows that could reduce the time and cost through quick and informed evaluation, testing, and development of feedstock, processes, and parts. The report presents the findings from the collaborative efforts between Oak Ridge National Laboratory (ORNL) and the U.S. Army GVSC GVME. The aim of this project was to develop a geometric feature-based qualification framework for WAAM of SS 17-4PH components. This report outlines selection methodology of representative build geometries, optimization of WAAM process parameters, in-situ monitoring, microstructure-property evaluation, thermal simulations, as well as data visualization techniques incorporated in this project. The results from this project demonstrate a clear understanding of thermal history dependent phase evolution and consequent location-specific property variations in WAAM of SS 17-4PH. These results in conjunction with the data-driven methodologies used in this project are expected to reduce qualification timelines, improve predictability, and accelerate the development of reliable feature-based qualification strategies for part production via large-scale M-AM technologies.

36 MATERIALS SCIENCE↗

Alloy Partitioning Effect on Strength and Toughness of κ-Carbide Strengthened Steels

Alloy partitioning during heat treatment in a lightweight precipitation hardened steel was investigated using transmission electron microscopy and atom probe tomography. The mechanical properties are discussed as a function of the effect of solution treatment temperature and aging time, giving rise to variations in chemical modulation. A wrought lightweight steel alloy with a nominal composition of Fe-30Mn-9Al-1Si-1C-0.5Mo (wt. %) was solution-treated between 1173–1273 K and aged at 773 K. Lower solution treatment temperatures retained a finer grain size and accelerated age hardening response that also produced an improved work hardening behavior with a tensile strength of -1460 MPa at 0.4 true strain. Atom probe tomography indicated these conditions also had reduced modulation in the Si and Al content due to the reduced aging time preventing silicon from diffusing out of the κ-carbide into the austenite. This work provides the framework for heat-treating lightweight, age hardenable steels with high strength and improved energy absorption.

36 MATERIALS SCIENCE↗

How Austenitic Is a Martensitic Steel Produced by Laser Powder Bed Fusion? A Cautionary Tale

Accurate phase fraction analysis is an essential element of the microstructural characterization of alloys and often serves as a basis to quantify effects such as heat treatment or mechanical deformation. Additive manufacturing (AM) of metals, due to the intrinsic nonequilibrium solidification and spatial variability, creates additional challenges for the proper quantification of phase fraction. Such challenges are exacerbated when the alloy itself is prone to deformation-induced phase transformation. Using commonly available in-house X-ray diffraction (XRD) and electron backscatter diffraction (EBSD) and less commonly used synchrotron-based high-energy X-ray diffraction, we characterized nitrogen-atomized 17-4 precipitation-hardening martensitic stainless steel, a class of AM alloy that has received broad attention within the AM research community. On the same build, our measurements recovered the entire range of reported values on the austenite phase fractions of as-built AM 17-4 in literature, from ≈100% martensite to ≈100% austenite. Aided by Calphad simulation, our experimental findings established that our as-built AM 17-4 is almost fully austenitic and that in-house XRD and EBSD measurements are subject to significant uncertainties created by the specimen’s surface finish. Hence, measurements made using these techniques must be understood in their correct context. Our results carry significant implications, not only to AM 17-4 but also to AM alloys that are susceptible to deformation-induced structure transformation and suggest that characterizations with less accessible but bulk sensitive techniques such as synchrotron-based high energy X-ray diffraction or neutron diffraction may be required for proper understanding of these materials.

17-4 steel↗

PROCESS-STRUCTURE-PROPERTY RELATIONSHIPS IN LASER POWDER BED FUSION PRODUCED 17-4 PH STEEL

Laser powder bed fusion (LPBF) is a metal additive manufacturing method that produces non-traditional microstructures as a result of the rapid solidification and thermal cycling inherent to the process. When using LPBF-produced material in application, these unique microstructures challenge the applicability of well developed mechanical property databases achieved by conventional heat treatments. For wider adoption of this technology, a more holistic understanding is necessary on how process attributes develop material structure, which dictate mechanical properties. This dissertation explores the process– structure–property relationships in LPBF 17-4 PH steel through systematic evaluation of atmospheric processing and heat treatment effects on microstructure and mechanical performance. Specimens were fabricated under controlled build environments, subjected to a range of solutionizing, homogenizing, and aging treatments, and characterized using optical microscopy, electron back scatter diffraction (EBSD), and X-ray diffraction (XRD) to quantify phase evolution. Tensile testing was performed to directly link heat treatment pathway and nitrogen absorption to mechanical performance. This work demonstrates where conventional heat treatment standards are applicable to LPBF 17-4 PH steel and where modifications are required. By directly correlating phase stability, nitrogen effects, and tensile response, this work provides practical guidelines for tailoring post-processing strategies. These findings underscore that successful application of LPBF 17-4 PH steel requires explicit consideration of both build environment and post-processing. By linking processing conditions to microstructure and performance, this work advances understanding of critical variables that govern reliability of additively manufactured precipitation-hardened stainless steels in demanding applications.

Brown, Benjamin [Kansas City National Security Cam↗

Crystallographic orientation-dependent strain hardening in a precipitation-strengthened Al-Cu alloy

While the strengthening of Al-Cu alloys due to precipitation has been extensively studied, the effect of crystallographic orientation of the matrix and precipitates, as well as precipitate morphology, on the strain hardening behavior is not well understood. In this paper, we investigate this effect with in situ neutron diffraction during deformation of an Al-Cu alloy (206) after multiple aging treatments. Precipitate-dislocation interactions were found to change from precipitate shearing for microstructures predominantly containing GPI and θ" precipitates to Orowan looping for microstructures with primarily θ' and θ precipitates. Notably, significant anisotropy in strain hardening behavior was observed when θ' precipitates were present, which was attributed to crystallographic orientation dependent load transfer from the Al matrix to the θ' precipitates. The anisotropic load transfer is hypothesized to be caused by the extent of rotation of high aspect-ratio θ' precipitates, owing to dislocations looping around them during plastic deformation of the matrix. Predictions from an analytical model describing the anisotropic magnitude of load transfer from precipitate rotation agree well with experimental results, successfully validating the precipitate rotation hypothesis and explaining the anisotropic strain hardening behavior. This model allows for the prediction of stresses separately in the precipitate and matrix phases as a function of crystallographic orientation, only given the bulk mechanical properties.

36 MATERIALS SCIENCE↗