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At least 307 records · Page 17

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗

HYDRODYNAMIC TESTING OF ZIRCALOY TO STEEL HUB COUPLINGS FOR USE IN ADVANCED TEST REACTOR I-LOOP TUBE

The ATR I-positions' isolation from the flux trap region provides an opportunity for a test facility that could create conditions representative of commercial light water reactors. Such a facility requires piping couplings and joints that withstand extreme thermal and pressure cycling. Also, transitioning from steel to zircaloy piping inside the reactor vessel allows the neutronic properties of zircaloy to be leveraged while using cost-effective stainless steel outside of the core. Grayloc-style hub couplings will act as transition points between stainless steel piping and zircaloy piping inside the reactor vessel. These couplings have not been sufficiently tested for leakage where there is a transition between materials. This transition is a concern because the thermal expansion coefficients of the materials differ. Seal integrity between the two components may be greatly affected by thermal expansion at the connection. Thus, the effect of thermal cycling must be assessed. Thermal and pressure cycling and hydrodynamic testing will be conducted to verify seal integrity of the steel to zircaloy hub coupling when subjected to ATR conditions.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Wire Arc Additive Manufacturing of Multi-material Parts Using H-13 Tool Steel

H-13 tools steel’s relative hardness, resistance to thermal fatigue, and high tolerance of thermal shock, make it very desirable for use in forging, pressing, casting, and extrusion processes[1]. H-13 is however typically quite expensive when compared to many other steel compositions. It is therefore desirable to encase a lower cost steel composition with H-13. This configuration allows for the benefits of H-13 tooling to be realized, at a considerably reduced cost. To demonstrate the viability of this concept, a casting tool was fabricated using a Wire Arc Additive Manufacturing (WAAM) process. Initial materials testing was conducted on a multi-material wall which consisted of one section of H-13 tool steel, and one section of 410NiNmo. These tests included scanning electron microscopy, energy dispersive X-ray spectroscopy, and hardness testing. This testing generated favorable results and subsequently a casting tool was fabricated for evaluation. Utilization of a Multi-Material WAAM process to fabricate large tooling in this manner could yield significant improvements in material cost, manufacturing agility, and supply chain complexity.

Lambert, Nathan [ORNL] (ORCID:0009000324134206)↗

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↗

Elucidating the temperature dependence of TRIP in Q&P steels using synchrotron X-Ray diffraction, constituent phase properties, and strain-based kinetics models

Understanding the deformation-induced martensitic transformation (DIMT) is critical for interpreting the structure-property relationships that govern the performance of transformation-induced plasticity (TRIP) assisted steels. However, modern TRIP-assisted steels often exhibit DIMT kinetics that are not easily captured by existing empirical models based on bulk tensile strain. We address this challenge by combined bulk uniaxial tensile tests and in-situ high energy synchrotron X-ray diffraction, which resolved the phase volume fractions, stress-strain response, and microstructure evolution of each constituent phase. A modification of the Olson-Cohen model is implemented, which describes the martensitic transformation kinetics as a function of the estimated partitioned strain in austenite, rather than the bulk tensile strain. This DIMT kinetic model is used as a framework to clarify the root cause of an insufficiently understood toughness trough reported for TRIP-assisted steels during deformation at elevated temperatures. Here, the importance of the temperature-dependent toughness is discussed, based on the opportunity to modify deformation processes to tailor the DIMT kinetics and mechanical properties during forming and in service.

36 MATERIALS SCIENCE↗

The compositional optimization and secondary phases evaluation regarding the creep resistance in Grade 91 steel through the CALPHAD approach

The critical secondary phases along with critical temperatures in regard to the creep resistance of Grade 91 steel alloy were evaluated in order to optimize the composition of the alloy to improve the creep resistance. The critical temperatures which are highlighted in this paper are Ac1 (the threshold temperature in which austinite begins to form), and Ac3 (the threshold temperature at which ferrite is fully transformed into austenite). Furthermore, optimization was presented through various Cr, V, Nb, and N concentrations in Gr.91 in relation to these critical temperatures and the mole fraction of M 23 C 6 , MX, and Z-Phase as critical secondary phases. Here, the results indicate that increasing V and Nb will increase MX stability, whereas decreasing Cr and N lead to a decrease in Z-Phase and M 23 C 6 stability, which may lead to an increased creep resistance of the material. Upon further analyzing the V, Nb, and N concentrations in Gr.91, results indicate that increasing Nb content in the steel can lead to an increased stability of Nb-rich MX2 carbide which can be used to replace Z-Phase in low N steels. Simulation results indicate that elimination of N with a dramatic increase in Nb concentrations result in the stability increase of only M 23 C 6 and MX2 phases at temperature regions between 600 °C and 1370 °C and a complete removal of Z-Phase precipitation. Overall, with the elimination of N, which destabilizes Z-Phase precipitation, and an increase in Nb for NbC carbide stability, a possible solution to increasing both long-term and short-term creep resistance for Gr.91 can be achieved, though further optimization and creep experiments need to be conducted for final conclusions.

36 MATERIALS SCIENCE↗

Pressureless Sintering of Pre-Alloyed Nanostructured Bainitic Steel Powders

A recent study shows that powder metallurgy and pressureless sintering are a viable pathway to realize full-density bulk components of nanostructure bainitic steels. A scalable, pressureless supersolidus liquid phase sintering (SLPS) approach to process nanostructured bainitic steel is evaluated. Furthermore, to address the oxidation issues associated with the mechanical alloying of elemental powders, powder atomization is used to produce pre-alloyed nanostructured bainitic steel powders.

mechanical alloying↗

Tempering and Austempering of Double Soaked Medium Manganese Steels

The addition of a tempering or austempering step to the double soaking of a 0.14C–7.17Mn (wt pct) steel was investigated in the present contribution. The double soaking heat treatment is a two-step intercritical annealing heat treatment, which generates microstructures of athermal martensite, retained austenite and ferrite when applied to medium manganese steels. Microstructures following double soaking and (aus)tempering contained a combination of retained austenite, athermal or tempered martensite, and blocky or bainitic ferrite. X-ray diffraction, dilatometry and transmission Kikuchi diffraction were utilized to investigate microstructural changes which occurred during tempering or austempering. The resulting mechanical properties were measured using uniaxial tensile testing. The double soaking plus tempering heat treatment was shown to generate an ultimate tensile strength of 1,340 MPa in combination with 28 pct total elongation while the double soaking plus austempering heat treatment resulted in an ultimate tensile strength of 1,675 MPa and total elongation of 22 pct. Overall, both novel heat treatments produced a combination of strength and ductility desired for the third generation of advanced high strength steels.

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↗

Armor for Steel: Facile Synthesis of Hexagonal Boron Nitride Films on Various Substrates

Abstract While hexagonal boron nitride (hBN) has been widely used as a buffer or encapsulation layer for emerging electronic devices, interest in utilizing it for large‐area chemical barrier coating has somewhat faded. A chemical vapor deposition process is reported here for the conformal growth of hBN on large surfaces of various alloys and steels, regardless of their complex shapes. In contrast to the previously reported very limited protection by hBN against corrosion and oxidation, protection of steels against 10% HCl and oxidation resistance at 850 °C in air is demonstrated. Furthermore, an order of magnitude reduction in the friction coefficient of the hBN coated steels is shown. The growth mechanism is revealed in experiments on thin metal films, where the tunable growth of single‐crystal hBN with a selected number of layers is demonstrated. The key distinction of the process is the use of N 2 gas, which gets activated exclusively on the catalyst's surface and eliminates adverse gas‐phase reactions. This rate‐limiting step allowed independent control of activated nitrogen along with boron coming from a solid source (like elemental boron). Using abundant and benign precursors, this approach can be readily adopted for large‐scale hBN synthesis in applications where cost, production volume, and process safety are essential.

2D materials↗

Amphilic Water-Lean Carbon Capture Solvent Wetting Behavior through Decomposition by Stainless-Steel Interfaces

In this work, we report on a combined experimental and theoretical study of the wetting and reactivity of water-lean carbon capture solvents on the surface of common column packing materials. Paradoxically, we find that these solvents are equally able to wet hydrophobic and hydrophilic surfaces. The solvents are amphiphilic and are able to adapt to any interfacial environment due to their inherent heterogeneous molecular structure. Ab initio molecular dynamics indicates that these structures enable the formation of a strong adlayer on the surface of hydrophilic surfaces like oxidized steel which promotes solvent decomposition akin to hydrolysis from surface oxides and hydroxides. This decomposition passivates the surface, making it effectively hydrophobic, and the decomposed solvent promotes leaching of the iron into the bulk fluid. This study links the wetting behavior to the observed corrosion of the steels via decomposition of solvent at steel interfaces. The overall affect is strongly dependent on the chemical composition of the solvent, in that amines are stable, whereas imines and alcohols are not. We also observed that plastic packing shows little to no solvent degradation, but an equal degree of wetting.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Evaluation of coated steels in supercritical CO 2

The carburizing supercritical CO 2 (sCO 2 ) environment limits the use of lower cost steels in the lower temperature (450–650°C) portions of the sCO 2 Brayton cycle because of concerns about internal carburization and embrittlement. Results on a ferritic–martensitic steel and conventional and advanced austenitic steels at 450–650°C in 30 MPa sCO 2 with and without 1% O 2 and 0.1% H 2 O additions have indicated that sCO 2 environments will have lower maximum operating temperatures compared to steam plants. Pack Al and Cr coatings were evaluated at 650°C on T91 and 316H substrates and showed some benefit for up to 2000 h at 650°C, especially without impurities. However, characterization indicated Al 2 O 3 was not formed and Cr-rich carbides formed in the Cr coatings. With the addition of impurities in the sCO 2 , the coatings were less protective at 650°C. Subsequent exposures at 600°C in sCO 2 showed similar behavior. Postexposure evaluations included measuring the bulk C content and room temperature tensile properties. Finally, improvements were indicated but the tensile results were complicated by the high temperature pack coating process affecting the substrate properties.

36 MATERIALS SCIENCE↗

Data-Driven Surrogate Modeling with Microstructure-Sensitivity of Viscoplastic Creep in Grade 91 Steel

Abstract To support the development of advanced steel alloys tailored to withstand extreme conditions, it is imperative to account for the mechanical performance of components, while considering the influence of local microstructure on the macroscopic response. To this end, this study focuses on the development of microstructure-sensitive constitutive models for the mechanical response of Grade 91 steel exposed to extreme thermo-mechanical environments. Polynomial chaos expansion (PCE) surrogates are used to emulate high-fidelity polycrystal simulations of the viscoplastic response of Grade 91 steel as a function of the microstructure fingerprint (e.g., dislocations and precipitates). To cover a wide temperature–stress domain, two separate PCE surrogates—one that captures softening and the other that captures hardening behavior—are combined using another (sparse) Gaussian process regression model. The resulting constitutive creep surrogate model is integrated within the MOOSE finite element framework to simulate the intricate effects of microstructure, in particular MX-phase precipitates, on a component with a graded microstructure. Surrogate sensitivity analysis is applied to quantify the relevant impact of spatially varying microstructure on the creep response in a test-case involving a Grade 91 alloy with a prototypical weld.

36 MATERIALS SCIENCE↗

High temperature high strength austenitic steel fabricated by laser powder-bed fusion

Extremely fast cooling rates during laser powder-bed fusion (LPBF) can result in materials with unique microstructures. For LPBF 316L stainless steel, the formation of sub-grain cellular structures with high dislocation density has been linked to superior tensile properties at room temperature. This cellular structure offers also a new route for the development of high temperature LPBF steels with the nucleation of nano-size strengthening carbides in the cell walls. HK30Nb steel (Fe-25Cr-20Ni-Nb-C) was, therefore, fabricated by LPBF to evaluate its potential for high temperature applications. Optimization of the fabrication parameters yielded material with density greater than 99.7%, with nano Nb-rich precipitates in the cell walls. Annealing at 800 °C for 5h resulted in the nucleation and growth of additional precipitates mainly in the cell walls and at grain boundaries. Furthermore, the high dislocation density led to yield strength at 20–900 °C two to three times higher than yield strength for cast HK30Nb and the nano carbides in the cell walls significantly improved the cellular structure stability at 800 °C.

36 MATERIALS SCIENCE↗

Synthesis of a 316L stainless steel-copper composite by laser melting

This paper demonstrates a laser melting method to produce a metal matrix composite with a higher thermal conductivity compared to 316 L stainless steel using a Jettable Cu ink. A novel canister was used to control the oxygen level during laser processing to emulate a hybrid inkjet-powder bed fusion technique for doping the stainless steel powder bed with Cu precursor ink. Here, the thermal conductivity of the composite was found to be 187% higher than that of 316 L stainless steel, while the microhardness decreased by 39%. Microstructural results show opportunities to further enhance the thermal conductivity and mechanical properties of the composite by eliminating interfacial cracking.

36 MATERIALS SCIENCE↗

Mechanical properties and strain localization of WA-DED printed P91 steel

This paper discusses a P91 steel block that was additively manufactured by wire arc direct energy deposition (WA-DED) followed by two types of post-process heat treatment (PPHT). Vickers microhardness and digital image correlation tensile tests were performed along the building direction. The global mechanical properties (i.e., microhardness and tensile properties) and the local mechanical responses (i.e., hardness fluctuation and strain localization) were systematically investigated. Results showed that (1) all P91 specimens showed higher strengths than American Society of Mechanical Engineers standard requirements for wrought P91 steel, (2) the as-printed P91 exhibited much higher average hardness and fluctuations than that after PPHT, (3) PPHT reduced P91 strengths but improved the ductility significantly, and (4) strain localization presented in the as-printed specimen during uniform deformation in tensile tests. The hardness fluctuation and strain localization along the building direction of the AP P91 were caused by different thermal histories received during WA-DED. The study indicated that PPHT, ideally tempering-only heat treatment, is necessary for the WA-DED printed P91 steel.

Mechanical properties↗

Multi-scale characterization of supersolidus liquid phase sintered H13 tool steel manufactured via binder jet additive manufacturing

Additive manufacturing (AM) of H13 tool steel by binder jet 3D printing (BJ3DP) followed by pressureless supersolidus liquid phase sintering (SLPS) provides a low-cost alternative manufacturing method for components with intricate geometric features. However, the microstructure-mechanical property relationships for BJ3DP-SLPS produced H13 tool steel are not well understood, which makes it challenging to develop printing and post-processing methods that maximize part performance. In this work, we leverage atom probe tomography and transmission electron microscopy along with thermodynamic calculations to rationalize the microstructure-mechanical property relationships in as-sintered BJ3DP H13 tool steel. Here, we report for the first time, the presence of a continuous eutectic film-like carbide in H13 along with the more commonly observed cuboidal MX carbides in the prior liquid channels of the microstructure. Further, atom probe tomography revealed the interconnected nature of the MX carbides that appear to be discrete in two-dimensional micrographs. These continuous eutectic carbides and interconnected MX carbides result in brittle failure of the material. Characterization of these microstructural features will be critical in developing appropriate post-processing heat treatments for the improved mechanical performance of BJ3DP H13.

36 MATERIALS SCIENCE↗

Inverse design of hypoeutectoid pearlite steel microstructures using a deep learning and genetic algorithm optimization framework

Goal-oriented microstructure design in metallic materials is a challenging task due to complex structure-property relationships. Traditional experimental and computational approaches are time-intensive and economically inefficient, limiting their applicability for large-scale design space exploration. Here, in this work, we propose an end-to-end framework that integrates deep learning models with genetic optimization to design microstructures with targeted mechanical properties. Deep learning models enable accurate forward design, while their integration with genetic optimization enables efficient inverse design within a few hours, compared to days or weeks using conventional finite element simulations. The framework combines experimental characterization and finite element modeling to analyze the influence of microstructural features on the mechanical behavior of hypoeutectoid steels. Data from both experiments and simulations are used to train the deep learning models. To demonstrate its effectiveness, we apply the framework to 0.63% carbon steel with proeutectoid ferrite and pearlite phases, commonly used in industrial applications. In this study, 2D microstructures were used for modeling, selected primarily for computational efficiency and to establish proof of concept. The framework successfully optimizes microstructures for targeted yield strength, ultimate strength, and stress concentration factors while significantly reducing computational time. Beyond hypoeutectoid steels, this scalable framework can be extended to other material systems and integrated with additive manufacturing, offering an efficient approach for accelerating microstructure design for specific engineering applications.

ConvLSTM↗