Machine-Learning Microstructures 9CrSteel data in brief
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Chromium Steel↗
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Additive Manufacture of Multi-Functional, Large-Scale Components
The poster summarizes the main results for a LDRD focused on developing a arc-based additive manufacturing (AM) system capable of fabricating large components with a composition gradient otherwise known as functionally graded materials (FGMs). FGMs are capable of addressing local extreme conditions in an optimal and cost-effective manner. The AM system (referred to as multi-Wire Arc Additive Manufacturing or m-WAAM) consisted of modifying a standard automated gas tungsten arc welding system to deliver multiple welding wires to the weld pool at controlled rates to deposit desired alloy compositions at critical locations. Numerous shapes and composition gradients were fabricated with the system and the effect of various deposition parameters on the nature of the composition profile were evaluated. Additionally, heat treatment of the FGM was performed to develop graded microstructures which should enhance dynamic impact performance of inexpensive steels. The project highlights the potential of m-WAAM to efficiently fabricate FGMs. However, this project only explored the science behind the technique and additional development work will be required to develop a fully-functional system that can build more complex components.
36 MATERIALS SCIENCE↗
Understanding radiation effects in friction stir welded MA956 using ion irradiation and a rate theory model
We report an outstanding challenge in the manufacturing and joining of oxide dispersion strengthened steels is retaining the nanofeatures in the alloy throughout the fabrication and welding process. MA956 was friction stir welded with two different sets of welding parameters, resulting in a medium and high heat input. After welding, 5 MeV Fe ++ ion irradiations were performed at doses ranging from 50 to 200 dpa in the temperature range of 400 to 500°C. Post-irradiation characterization was performed with scanning transmission electron microscopy and energy-dispersive x-ray spectroscopy to investigate the Y-Al-O dispersoids, voids, and dislocations. After welding, the dispersoid microstructure coarsened, resulting in fewer and larger dispersoids regardless of heat input. After irradiation, the dispersoid behavior in the welded material was sensitive to temperature, exhibiting growth behavior attributed to Ostwald coarsening at 500 °C but a mixture of nucleation and more muted growth at 400 and 450 °C, attributed to competing mechanisms of radiation-enhanced diffusion and Ostwald coarsening. Void swelling correlated to heat input; being more prevalent in the welded conditions occurring at lower doses and in higher values relative to the base material. The low values of swelling despite microstructure coarsening caused by welding demonstrate the excellent swelling resistance of MA956, even after welding with the highest swelling values of 0.5% noted in the stir zone high heat input condition at 450 °C, 200 dpa. The dislocation behavior was inconsistent: the strongest trend was that network density was higher for welded versus base material, and an increase in loop diameter with temperature was observed. A rate theory model based on the observed microstructure suggests at high temperature interstitial loss to sinks was more likely to be dominant compared to mutual annihilation via point defect recombination, because of an increase of the radiation diffusion coefficient with temperature regardless of initial welded microstructure.
36 MATERIALS SCIENCE↗
Consistency of fatigue crack growth behavior of pipeline and low-alloy pressure vessel steels in gaseous hydrogen
Here, this study investigates the fatigue crack growth rate (FCGR) behavior of pipeline and low-alloy pressure vessel steels in high-pressure gaseous hydrogen. Despite a broad range of yield strengths and microstructures ranging from ferrite/pearlite, acicular ferrite, bainite, and martensite, the FCGR in gaseous hydrogen remained consistent (falling within a factor of 2–3). Steels with higher fractions of pearlite, typical of older vintage pipeline steels, exhibited modestly lower crack growth rates in gaseous hydrogen compared to steels with lower fractions of pearlite. Crack growth rates in these materials exhibit a systematic dependence on stress ratio and partial pressure of hydrogen, as captured in the recently published fatigue design curves in ASME B31 code case 220 for pipeline steels and ASME BPVC code case 2938 for pressure-vessel steels.
08 HYDROGEN↗
Corrosion testing needs and considerations for additively manufactured materials in nuclear reactors
Metal additive manufacturing holds significant promise as an enabling technology for the 21st century nuclear energy industry. Metal additive manufacturing (MAM) can allow the fabrication of novel materials and innovative component designs that are not achievable through conventional manufacturing. Due to its very different fabrication methods, as-fabricated MAM components are characteristically different from conventionally manufactured components. MAM materials exhibit very different microstructures from conventional cast or wrought materials. For example, austenitic stainless steels fabricated by laser powder bed fusion exhibit columnar grain structures, dislocation cell structures, and melt pool fingerprints. In addition, MAM fabrication may result in defects such as porosity, incomplete processing of the feedstock (e.g., lack of fusion in melt-based methods), and oxide inclusions. Heat treatments may further evolve the microstructure, microsegregation, and stresses within the component. Furthermore, MAM components have a rough surface with feature sizes on the order of the feedstock material, as opposed to smooth surfaces resulting from conventional machining and forming operations. As a result, the corrosion behavior of MAM components will likely be significantly different from that of conventionally formed components. Corrosive environments for structural materials within advanced reactor environments include molten fluoride and chloride salts, liquid sodium and lead-bismuth, and high-temperature helium. The Advanced Materials and Manufacturing Technologies program within the Department of Nuclear Energy in the United States Department of Energy is assessing the unique concerns of MAM component corrosion and testing methodologies in advanced nuclear reactor environments. We discuss these concerns and testing strategies in this paper.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Manufacturing ODS Steels from GARS Powders by Friction Consolidation and Extrusion
Previous research suggested that friction-based processing is a promising method for fabricating oxide dispersion-strengthened (ODS) steel. In this study, we combined friction consolidation and friction extrusion to successfully manufacture ODS steel rods using precursor powder made with gas atomization reaction synthesis. We examined the microstructure evolution from the initial powder to the final extruded rod, which revealed the dispersion process of Y. Additionally, by comparing the microstructures of three rods extruded at different temperatures, we showed that low-temperature friction extrusion effectively enhanced microstructure uniformity and prevented grain coarsening, leading to improved mechanical properties. Furthermore, our findings provide practical guidelines for adjusting processing parameters in the production of ODS steel using friction-based processing.
36 MATERIALS SCIENCE↗
Characterization and Quantification of Radiation-Induced Clusters/Precipitates in RPV Steels Using STEM-EDS and Machine Learning
Over the operational lifespan of a nuclear reactor, reactor pressure vessel (RPV) steels are subjected to significant neutron irradiation, resulting in complex microstructural changes and the consequent degradation of mechanical properties. Various physically motivated correlation models have been developed to predict neutron irradiation-induced embrittlement of RPVs under different irradiation conditions. However, the efficient and accurate characterizations and quantification of radiation-induced clusters in RPVs are still challenging, which will affect the precision of the predictive models for embrittlement of RPV components. In the DOE Visiting Faculty Program (VFP) research work at Oak Ridge National Lab (ORNL), I integrate machine learning to aid Scanning Transmission Electron Microscopy – Energy Dispersive X-ray Spectroscopy (STEM-EDS) analyses, which improve the characterization and quantification of radiation-induced clusters in RPV steels, thereby enabling more accurate predictions of material behavior under irradiation. The surveillance base- and welded- RPV steels were annealed at various temperatures of 340 °C, 450 °C and 500 °C for up to 168 hours, respectively. Afterwards, I have characterized radiation-induced clusters using advanced STEM-EDS techniques and subsequently applying machine learning algorithms to analyze and refine STEM-EDS datasets, enhancing the quantification of clusters compositions and distributions. In the end, an efficient workflow for integrating STEM-EDS data analysis with machine learning to address challenges including noise reduction has been developed. The completion of this VFP work will support bridge critical gaps in the accurate quantification of radiation-induced clusters in RPV steels using STEM-EDS and support the development of more precise models for predicting RPV embrittlement in the Light Water Reactor Sustainability program supported by Department of Energy and enhancing the collaboration between ORNL and Alred University. The outcome of the VFP project will leverage a few research papers submission to peer-reviewed journals in the relevant scientific field and a few oral presentations at national and international conferences.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Postweld Heat Treatment on Toughness of Electric- Resistance Welded X70 Steel
In this report the effect of postweld heat treatment (PWHT) on Charpy V-notch impact toughness of a highfrequency electric-resistance welded (HF-ERW) grade X70 pipeline steel is investigated. PWHT thermal cycles are simulated using the Gleeble on the as-welded specimens. Microstructure, along with crystallographic texture and microhardness, is characterized in specimens that are impact tested at –5°C (23°F), –30°C (–22°F), and –45°C (–49°F). The impact toughness values show a wide scatter band and decrease with the increasing peak temperature of the PWHT. For higher peak temperatures, the microstructure of the heat-affected zone (HAZ) gradually changed from equiaxed ferrite to bainitic ferrite. Furthermore, the prior austenite grain size (PAGS) increases with the increasing peak temperature. The density of high-angle grain boundaries decreases, and the fraction of cleavage planes {100} parallel to the impact fracture plane increases for higher peak temperatures of the PWHT
36 MATERIALS SCIENCE↗
Long-term thermal aging behavior and strength reduction in a laser powder bed fusion 316H stainless steel
The long-term thermal stability of structural alloys is essential for ensuring the safe and reliable operation of nuclear reactors and other power plants. While extensive research has explored the effects of thermal aging on conventional stainless steels, the behavior of additively manufactured (AM) alloys remains less understood. This study examines the thermal aging response of laser powder bed fusion (LPBF) 316H stainless steel (SS) at temperatures ranging from 550 °C to 750 °C over durations of up to 10,000 h (approximately 1.14 years). Advanced characterization techniques, including electron microscopy and synchrotron X-ray diffraction, were used to investigate dislocation recovery and phase evolution. Based on these findings, a time-temperature-precipitation (TTP) diagram was developed for LPBF 316H SS, revealing a 10- to100-fold acceleration in precipitation kinetics compared to wrought 316H SS. A physics-informed model was calibrated using the short-term experimental data, enabling predictions of average precipitate sizes, volume fractions of M 23 C 6 and Laves phases, and changes in molybdenum solute concentration for aging up to 1 × 10⁶ h (114 years). These microstructural insights were further utilized to estimate yield strength and extrapolate strength reduction factors over the extended aging period. Despite the accelerated aging kinetics, LPBF 316H SS demonstrated superior yield strength retention compared to its wrought counterpart. In conclusion, this study establishes a framework for evaluating long-term performance using short-term experimental data and supports the accelerated qualification of AM materials for high-temperature structural applications.
Laser powder bed fusion↗
Technological aspects in blanket design: Effects of micro-alloying and thermo-mechanical treatments of EUROFER97 type steels after neutron irradiation
Presently available data on neutron irradiation damage raise doubts on the feasibility of using EUROFER97 steel for a water-cooled starter blanket in a DEMO reactor, since the ductile-to-brittle transition temperature (DBTT) increases significantly for irradiation temperatures below 350°C. The additional DBTT shift caused by H and He transmutation can only be estimated based on very few results with isotopically tailored EUROFER97 steel. Conservative calculations show that the DBTT of EUROFER97 steel could exceed the operating temperature in water-cooled starter blankets within a relatively short time period. This paper presents results from a EUROfusion funded irradiation campaign that was performed in the High Flux Isotope Reactor at Oak Ridge National Laboratory. The paper compares ten newly developed reduced activation ferritic-martensitic (RAFM) steels irradiated to a nominal dose of 2.5 dpa at 300°C. The post-irradiation experiments using Small Specimen Test Technology included hardness, tensile, and fracture mechanics tests combined with fractography and microstructure analysis are presented. Results show that micro-alloying EUROFER97-type steels influenced the mechanical properties but a dominating impact on irradiation damage resistance could not be identified. In contrast, specific thermo-mechanical treatments lead to better DBTT behavior. Discussion about irradiation response to heat treatment conditions is also given. Here, despite requiring data also at high dpa values, the results indicate that with these modified materials an increased lifetime and potentially also an increased operating temperature window can be achieved compared to EUROFER97.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Coupling physics in machine learning to predict properties of high-temperatures alloys
Abstract High-temperature alloy design requires a concurrent consideration of multiple mechanisms at different length scales. We propose a workflow that couples highly relevant physics into machine learning (ML) to predict properties of complex high-temperature alloys with an example of the 9–12 wt% Cr steels yield strength. We have incorporated synthetic alloy features that capture microstructure and phase transformations into the dataset. Identified high impact features that affect yield strength of 9Cr from correlation analysis agree well with the generally accepted strengthening mechanism. As a part of the verification process, the consistency of sub-datasets has been extensively evaluated with respect to temperature and then refined for the boundary conditions of trained ML models. The predicted yield strength of 9Cr steels using the ML models is in excellent agreement with experiments. The current approach introduces physically meaningful constraints in interrogating the trained ML models to predict properties of hypothetical alloys when applied to data-driven materials.
36 MATERIALS SCIENCE↗
Machine-Learning Microstructure for Inverse Material Design
Metallurgy and material design have thousands of years’ history and have played a critical role in the civilization process of humankind. The traditional trial-and-error method has been unprecedentedly challenged in the modern era when the number of components and phases in novel alloys keeps increasing, with high-entropy alloys as the representative. New opportunities emerge for alloy design in the artificial intelligence era. Here a successful machine-learning (ML) method is developed to identify the microstructure images with eye-challenging morphology for a number of martensitic and ferritic steels. Assisted by it, a new neural-network method is proposed for the inverse design of alloys with 20 components, which can accelerate the design process based on microstructure. The method is also readily applied to other material systems given sufficient microstructure images. This work lays the foundation for inverse alloy design based on microstructure images with extremely similar features.
36 MATERIALS SCIENCE↗
Microstructure and high temperature tensile properties of 316L fabricated by laser powder-bed fusion
316L stainless steel fabricated by laser powder-bed fusion (LPBF) has attracted significant attention due to a unique combination of strength and ductility at room temperature. Understanding of high temperature tensile properties of LPBF fabricated 316L is, however, limited. In the present investigation, tensile testing was conducted at 20–700ºC on LPBF 316L in as printed condition and after annealing for 5 h at 500–800ºC. Room temperature data confirmed the excellent ductility of the LPBF-processed 316L steel due to the cellular structure with high dislocation density. However, a significant decrease in ductility was observed at temperatures above 200ºC. These results are consistent with a change of deformation mechanisms observed in wrought 316L, with twinning playing a key role at room temperature. Finally, microstructure characterization and tensile testing revealed that the cellular structure is stable up to 500ºC, but a decrease of yield strength was observed at temperatures above 600ºC likely due to a decrease in dislocation density via annealing.
36 MATERIALS SCIENCE↗
Decarburization and Carburization Behavior of Grade 91 Steel in Sodium Environments
Two heats of G91 steel have been investigated in sodium at 550-650°C to understand its corrosion behaviour, microstructural evolution, and tensile properties. Sodium exposure tests of subsized tensile and coupon specimens of G91 base metal and weldment were conducted in Argonne’s forced convection sodium materials testing loops. Maximum exposure times of ~39,000 h at 550°C, ~37,000 h at 600°C, and ~20,000 h at 650°C have been achieved, respectively. Thermal aging experiments of G91 steel were conducted in parallel, and the data of the sodium-exposed specimens were compared with the thermal aging data of the same heat to isolate the thermal aging effect from the effect of sodium exposure. It was found that the tensile strength of G91 steel can be reduced by more than 50% after sodium exposures at 650°C. The effect of a sodium environment on tensile properties is largely dependent on the carburization/decarburization behavior of G91 steel exposed to sodium. The carbon concentrations in sodium in Argonne’s SMT-1 and SMT-2 loops were determined by the equilibration method. The carbon activity in sodium was established by equilibrating high-purity nickel in sodium, analyzing the material for carbon, and using the reported data on the carbon solubility for this material. The carbon activity results were combined with the carbon solubility data in sodium to establish the carbon concentration in sodium. The carbon concentrations in the SMT-1 and SMT-2 loop were estimated to be 1.23 and 0.25 ppm, respectively. With this initial success, we will continue to monitor the carbon contents in the two loops to correlate the microstructural and mechanical property changes with the sodium purity. Future experiments will also consider sodium exposure tests in controlled carbon activities. Online monitoring and control of carbon contents in sodium in nuclear reactors would also be of interest. Thermodynamic analysis was conducted to understand the carburization-decarburization behavior of G91 steel exposed to sodium in the SMT-1 and SMT-2 loops. The equilibrium carbon activity in the alloy was evaluated by the thermodynamics of M 23 C 6 carbides. The calculated carburization-decarburization boundary showed that G91 would undergo decarburization at 650°C in the SMT-1 loop and carburization at 600°C in the SMT-2 loop, which is consistent with our findings from the sodium exposure tests. Future work will include thermodynamic analysis of the carbon concentration – activity relationship including the effect of carbide-forming elements, vanadium and niobium in G91 steel. Kinetics of carbon diffusion and the effect on microstructure and mechanical performance under various service conditions will also be investigated. The ultimate goal is to understand the mechanisms and the kinetics of carbon transfer in the sodium-steel system and to provide a basis for predicting the effect of long-term decarburization-carburization process on the integrity of reactor components.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Effects of lead and lean in multi-axis directed energy deposition
Here, the present study examines the effect of varying laser incidence angles on textural, microstructural, and geometric characteristics of directed energy deposition (DED) processed materials, providing a more comprehensive outlook on participating laser-matter interaction phenomena and ultimately devising strategies to ameliorate print performance. In this study, single-layer, single-/multi-track specimens were processed to examine the effect of non-orthogonal angular configurations on bead morphology, microstructure, phase composition, and textural representation of DED-processed 316L stainless steel materials. It was observed that bead size decreased at increasing lead and lean angles. Asymmetry in the distribution of the bead morphology as a function of lead angle indicates better catchment for acute lead angle configurations over obtuse configurations. No significant differences in phase composition, texture, and microstructure were observed in moderate off-axis configurations. When the penetration depth for the deposits was below 20 μm, columnar structures dominated the microstructure of the deposited material. At deeper penetration depths, columnar and equiaxed structures were observed at the bead-substrate interface and center of the bead, respectively. Compared to powder-blown DED, wire-DED dilution profiles were found to be asymmetric in both orthogonal and non-orthogonal wire DED samples.
36 MATERIALS SCIENCE↗
Laser Powder Directed Energy Deposition of Steels for Nuclear Applications
This comprehensive investigation examines the structure–property relationships in two nuclear alloy systems—Alloy 709 (A709) austenitic stainless steel and Grade 92 (G-92) ferritic/martensitic (F/M) steel—manufactured via directed energy deposition (DED) for sodium-cooled fast reactor applications. This study establishes the fundamental mechanisms for controlling microstructures for optimizing the mechanical performance of additively manufactured nuclear materials through systematic heat treatment optimization and multiscale characterization. As-deposited A709 steel develops a complex multiscale strengthening architecture consisting of a fine cellular solidification structure with diameter of 2-3 µm within10–50 µm grains, elevated dislocation densities from rapid thermal cycling, and grain boundary precipitates that activate concurrent Hall–Petch, dislocation, and precipitation hardening mechanisms to achieve exceptional properties [yield strength (YS): 603 MPa, ultimate tensile strength (UTS): 844 MPa, Vickers hardness: 220 HV] that achieve a 44% superior strength compared to that of the wrought material. Heat treatments produce different results. Solution annealing (SA) dissolves the cellular structure and reduces the hardness to 190 HV. Precipitation treatment (PT) keeps the cellular structure but adds carbides, allowing the hardness to reach 205 HV. The best approach combines both treatments (SA+PT) and creates uniform precipitate distributions with M 23 C 6 carbides at the grain boundaries and MX carbonitrides in the matrix, achieving a hardness of 195 HV. However, directional differences persist, with a 12%–15% strength variation between orientations due to the inherited layered microstructural architecture that survives aggressive heat treatment. While tensile testing at 550°C demonstrates 40%–50% thermal softening with dynamic strain aging, DED A709 steel still maintains a 71% higher YS than that of the wrought material. Ion irradiation studies (100–400 dpa) of DED A709 steel reveal progressive radiation damage with increasing void density and radiation-induced segregation causing nickel enrichment and chromium depletion, which will ultimately compromise mechanical properties. As-deposited G-92 exhibits exceptional strength (UTS: 1650–1700 MPa, 430 HV) through a complex microstructure containing both ferrite and martensite phases, a high geometrically necessary dislocation (GND) density (17.04×10 14 /m 2 ), and fine carbides. Heat treatments create distinct changes. Normalizing produces fresh martensite with the highest hardness (460 HV) and an increased GND density (20.23×10 14 /m 2 ). Tempering develops dual precipitation systems and reduces the hardness to 290 HV. The optimal approach uses sequential normalizing plus tempering, achieving balanced properties with the lowest hardness (250 HV) and a reduced GND density (11.01×10 14 /m 2 ). A processing-dependent anisotropy is observed: horizontal specimens achieve superior ductile behavior, while vertical specimens exhibit brittle failure. A tempering heat treatment successfully mitigates this anisotropic behavior by transforming the hard martensitic as-deposited structure into tempered martensite enabling both horizontal and vertical specimens to exhibit similar stress–strain characteristics with visible necking behavior. Remarkably, testing at 550°C reveals a reversal in the anisotropy, where as-deposited specimens achieve near isotropy with superior thermal stability (a 15%–20% strength reduction), while tempered specimens develop an orientation dependence with a 25%–30% strength reduction. Both alloy systems demonstrate that DED processing creates specimens with a superior strength through refined microstructural features, though with distinct strengthening mechanisms—austenitic through cellular structures and precipitates versus F/M through phase transformations and precipitates. Heat treatment optimization requires alloy-specific approaches, with A709 benefiting from controlled precipitation while G-92 requires careful phase transformation control. The results show that DED manufacturing can produce nuclear materials with exceptional performance, but directional effects and temperature-dependent behavior must be carefully considered for reactor component design and qualification.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Analysis of Pitting Corrosion on Wrought and Additively Manufactured 316L Stainless Steel in Atmospheric Environments
Additive manufacturing of metal components enables rapid fabrication of complex geometries. However, metal additive manufacturing also introduces new morphological and microstructural characteristics which might be detrimental to component performance. Here we report the pitting corrosion properties of wrought and additively manufactured 316L stainless steel after atmospheric exposure to coastal environments and laboratory-created environments. Qualitative visualization in combination with quantitative analysis of resulting pits provided an in-depth understanding of pitting differences between wrought and additively manufactured 316L stainless steel and between coastal and laboratory-based exposure. Optical and scanning electron microscopy were utilized for visualization, while white light interferometry measured pits across approximately 5mm x 5mm areas on each sample. Post-processing of the interferometry data enables quantification of pitting attack for each sample in terms of both pit depth and pit volume. The pitting analysis introduced herein offers a new technique to compare pitting attack between different manufacturing processes and materials.
36 MATERIALS SCIENCE↗
Creep behavior of an additively manufactured 9Cr steel in the as-built condition
Limited studies have evaluated the creep behavior of additively manufactured (AM) ferritic-martensitic (FM) steels. This work investigated the creep behavior of a 9Cr FM steel fabricated by powder blown directed energy deposition (DED) technique. Here, the creep testing at 550–650 °C and 150 MPa for the specimens along the deposition direction in the as-built condition, together with corresponding microstructural characterization, revealed a threshold temperature between 600 and 625 °C, below which the steel has creep resistance comparable with Grade 91 cross-welds and noticeably greater than 9Cr-1Mo steel. The threshold temperature distinguishes the creep behavior in two regimes differentiated in creep activation energy, creep deformation, and failure mechanism. Unlike the creep rupture surface ~45° from the loading direction when tested above the threshold temperature, the creep rupture for testing below the threshold temperature resembles type IV failure in the cross-welds of ferritic steels. The DED-induced layer structure in the as-built steel played a significant role on the change of creep behavior.
36 MATERIALS SCIENCE↗