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At least 307 records · Page 17

Tracing Phase Transformation and Lattice Evolution in a TRIP Sheet Steel under High-Temperature Annealing by Real-Time In Situ Neutron Diffraction

Real-time in situ neutron diffraction was used to characterize the crystal structure evolution in a transformation-induced plasticity (TRIP) sheet steel during annealing up to 1000 °C and then cooling to 60 °C. Based on the results of full-pattern Rietveld refinement, critical temperature regions were determined in which the transformations of retained austenite to ferrite and ferrite to high-temperature austenite during heating and the transformation of austenite to ferrite during cooling occurred, respectively. The phase-specific lattice variation with temperature was further analyzed to comprehensively understand the role of carbon diffusion in accordance with phase transformation, which also shed light on the determination of internal stress in retained austenite. These results prove the technique of real-time in situ neutron diffraction as a powerful tool for heat treatment design of novel metallic materials.

Yu, Dunji [ORNL] (ORCID:0000000189467851)↗

Tracking Dendritic Growth in Hydrogen-Based Hematite Reduction via Computer Vision

The reduction of hematite to metallic iron using hydrogen (H2) as a reducing agent presents a promising pathway for decarbonizing steel production. In this study, we employ a combination of in situ confocal scanning laser microscopy (CSLM) and advanced computer vision techniques to quantitatively analyze dendritic growth of ferrite during H2-based reduction of iron oxide at high temperatures. A workflow integrating Watershed Image Segmentation (WIS) and Lucas-Kanade Optical Flow (LKOF) is developed to extract both global and local kinetic information from time-resolved micrograph sequences. H2 reduction experiments conducted at 1400 degrees C and 1500 degrees C demonstrate a clear correlation between temperature and reduction rate, as evidenced by accuracy of fitted Johnson-Mehl-Avrami-Kolmogorov (JMAK) parameters. Optical flow analysis further elucidates the anisotropic and branched nature of dendritic growth, providing spatially resolved velocity fields that correlate well with global transformation kinetics. The proposed methodology demonstrates strong agreement with experimental measurements and literature values, offering a robust framework for automated image-based analysis to study kinetics through microstructural evolution in the reduction of iron ore, and likely other reaction-diffusion phenomena.

08 HYDROGEN↗

Heat affected zone liquation cracking evaluation on FeMnAl alloys

FeMnAl steels are currently generating a lot of interest with potential applications for structural parts in armored vehicles due to their lower density and outstanding mechanical properties. Despite the extensive mechanical performance and heat treatment exploration of this alloy class, further weldability investigation is required for future large-scale deployment. In the present study, the liquation cracking of four heats of cast FeMnAl alloys was investigated by the spot-Varestraint technique. The study focuses primarily on the effect of the major elements of the FeMnAl system: C, Mn and Al. Optical and electron microscopy were employed to investigate the microstructural features, and CALPHAD was employed to aid the discussion regarding the alloy’s composition differences and their effect on the liquation cracking susceptibility. The study was able to identify that compositions with the higher Mn, C, and lower Al presented the highest liquation cracking susceptibility. Conversely, composition presenting lower Mn, C, and Al showed the most resistant behavior. Furthermore, lower Al content promoted a fully-γ microstructure at low temperatures, which encouraged the appearance of longer cracks as a γ-matrix is more susceptible to HAZ cracking than a fully ferritic (α) or duplex (α + γ) microstructure.

36 MATERIALS SCIENCE↗

Flight Planning for the International Space Station - Levitation Observation of Dendrite Evolution in Steel Ternary Alloy Rapid Solidification (LODESTARS)

During rapid solidification, a molten sample is cooled below its equilibrium solidification temperature to form a metastable liquid. Once nucleation is initiated, growth of the solid phase proceeds and can be seen as a sudden rise in temperature. The heat of fusion is rejected ahead of the growing dendrites into the undercooled liquid in a process known as recalescence. Fe-Cr-Ni alloys may form several equilibrium phases and the hypoeutectic alloys, with compositions near the commercially important 316 stainless steel alloy, are observed to solidify by way of a two-step process known as double recalescence. During double recalescence, the first temperature rise is associated with formation of the metastable ferritic solid phase with subsequent conversion to the stable austenitic phase during the second temperature rise. Selection of which phase grows into the undercooled melt during primary solidification may be accomplished by choice of the appropriate nucleation trigger material or by control of the processing parameters during rapid solidification. Due to the highly reactive nature of the molten sample material and in order to avoid contamination of the undercooled melt, a containerless electromagnetic levitation (EML) processing technique is used. In ground-based EML, the same forces that support the weight of the sample against gravity also drive convection in the liquid sample. However, in microgravity, the force required to position the sample is greatly reduced, so convection may be controlled over a wide range of internal flows. Space Shuttle experiments have shown that the double recalescence behavior of Fe-Cr-Ni alloys changes between ground and space EML experiments. This program is aimed at understanding how melt convection influences phase selection and the evolution of rapid solidification microstructures.

Flemings, Merton C.↗

Process-driven roadmap for depositing super duplex stainless steel via wire Arc additive manufacturing

Here, this study systematically investigates the effects of shielding gas, bead spacing, weld mode, and travel speed on the phase balance, porosity, and hardness of wire arc additively manufactured (WAAM) super duplex stainless steel (ER2594). Robotic WAAM was employed to fabricate multilayer walls under systematically varied process conditions, followed by phase transformation simulations, X-ray computed tomography (XCT), electron backscatter diffraction (EBSD), and microhardness evaluation. Thermodynamic simulations predicted rapid cooling of AM process can suppress the potential formation of deleterious precipitates which was later validated via cross-sectional microstructure analyses of printed samples. XCT revealed porosity levels below 0.2% for all deposits, with reduced travel speed significantly lowering defect volume. Microstructural analyses revealed the evolution of various austenite precipitates, including grain boundary austenite (GBA), Widmanstätten austenite (WA), and intergranular austenite (IGA), sequentially upon cooling of the ferrite phase. Among all process parameters, weld transfer mode exhibited the strongest influence on phase balance; pulsed mode promoted higher ferrite retention (~ 36%) compared to RapidX mode. No consistent relationship between stabilized phase fraction and captured microhardness was observed. This work provides critical insights for optimizing WAAM parameters to control phase balance and mechanical performance, which is essential for producing high-integrity super duplex stainless-steel components for nuclear and marine applications.

Grain orientation↗

Physics-based model of irradiation creep for ferritic materials under fusion energy operation conditions

Irradiation creep is known to be an important process for structural materials in nuclear environments, potentially leading to creep failure at temperatures where thermal creep is generally negligible. While there is a great deal of data for irradiation creep in steels and zirconium alloys in light water reactor conditions, much less is known for first wall materials under fusion energy conditions. Lacking suitable fusion neutron sources for detailed experimentation, modeling, and simulation can help bridge the dose-rate and spectral-effects gap and produce quantifiable expectations for creep deformation of first wall materials under standard fusion conditions. In this paper, we develop a comprehensive model for irradiation creep created from merging a crystal plasticity representation of the dislocation microstructure and a defect evolution simulator that accounts for the entire cluster dimensionality space. Both approaches are linked by way of a climb velocity that captures dislocation-biased defect absorption and a dislocation strengthening term that reflects the accumulation of defect clusters in the system. Here, we carry out our study in Fe under first wall fusion reactor conditions, characterized by a fusion neutron spectrum with average recoil energies of 20 keV and a damage dose rate of ≈3×10 –7 dpa/s at temperatures between 300 and 800 K.

36 MATERIALS SCIENCE↗

The effect of secondary phases on microstructure and irradiation damage in an as-built additively manufactured 316 L stainless steel with a hafnium compositional gradient

Additive manufacturing (AM) or rapid prototyping has become a crucial tool for reducing both cost and time while increasing efficiency in qualifying structural materials for reactor use. In this study, directed energy deposition (DED) was used to develop an as-built 316 L stainless steel sample with three regions of increasing Hf-dopant to study the effects of Hf on the irradiation response of the material. Morphological and microstructural changes were analyzed before and after 2 MeV proton irradiation at 360 °C to a damage of 2.5 dpa at ~ 10 µm below the surface. The addition of Hf effectively suppressed radiation-induced damage (dislocation loops, radiation-induced segregation) due to enhanced point defect recombination. The radiation damage seen in the as-built sample was further compared to a thermo-mechanically treated counterpart of the same fabrication and irradiation parameters which was found to behave superiorly. In conclusion, the increased radiation resistance of this material may be attributed to the as-built microstructure, which includes undissolved Hf particles, delta ferrite grains and cellular sub-grain boundaries that can hinder defect motion.

316L Stainless Steel↗

Interfacial microstructure and mechanical properties of rotary inertia friction welded dissimilar 422 martensitic stainless steel to 4140 low alloy steel joints

In this work, dissimilar rotary inertia friction welds between 422 martensitic stainless steel and 4140 martensitic low-alloy steel were made to fabricate prototype heavy-duty diesel engine pistons. The influence of the inertia friction welding process and post weld heat treatment (PWHT) temperature on the interfacial microstructure evolutions and corresponding effects on mechanical properties of the 422/4140 welds were evaluated in detail. Carbon diffused from the 4140 side to the 422 side during PWHT at 650 °C for 1.5 h, causing the formation of a hard carbide-rich layer on the 422 side, and a softer but discontinuous C-depleted layer the 4140 side. PWHT at 700 °C for 1.5 h greatly accelerated C diffusion across the interface relative to 650 °C, resulting in a thicker hard carbide-rich layer and a relatively thick and continuous layer of coarse C-depleted grains (ferrite) on the 4140 side. In addition, the PWHT temperature greatly influenced the tensile properties and fracture behavior of the welds, with the 650 °C PWHT-ed samples failing predominately in a ductile manner in the 4140 heat affected zone during tensile testing. Conversely, the 700 °C PWHT specimens exhibited a strength reduction compared with the 650 °C PWHT specimens because of additional coarsening of the interfacial ferrite layer and softening of the base materials during PWHT, with brittle fracture between the hard and soft layers the predominate failure mechanism. Based on the findings, a reduced PWHT temperature and/or time, minimizing the hardness differential of the base metals, and pre-heating the 422 steel prior to welding are the potential pathways to achieve a more optimal balance between desirable tempering and stress relief of the weld microstructure and undesirable C migration across the weld interface, and to reduce the strength mismatch across the weld.

36 MATERIALS SCIENCE↗

The In Situ Observation of Phase Transformations During Intercritical Annealing of a Medium Manganese Advanced High Strength Steel by High Energy X-Ray Diffraction

Microstructural changes during thermal processing of a medium manganese steel containing (in wt%) 0.19C and 4.39 Mn were evaluated in situ with a high energy X-ray diffraction system (HEXRD). Samples with an initial fully martensitic microstructure were heated to intercritical annealing (IA) temperatures of 600 or 650°C, held for 30 min, and cooled to room temperature. Diffraction data were analyzed to determine the variations in austenite and ferrite phase fractions and phase lattice constants throughout the ICA cycles. On heating, the 2 vol. pct of austenite present in the starting microstructure decomposed, and cementite precipitation then occurred. During isothermal holding, the austenite fraction increased, up to 20% for the sample annealed at 650°C. The measured austenite fractions were less than those calculated by Thermo-Calc for equilibrium conditions, indicating that the 30-min hold time was insufficient to achieve near-equilibrium conditions. Observed changes in lattice parameters during isothermal holding were interpreted to reflect composition changes due to redistribution of the C and Mn between austenite and ferrite. The results are discussed in relation to the potential for controlling austenite stability during ambient temperature deformation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High-Throughput Nanoindentation Mapping of Additively Manufactured T91 Steel

Here, this work aims to adapt nanoindentation mapping combined with a k-means algorithm as a high-throughput technique to study the nano-scale spatial changes in mechanical properties for a heterogeneous material. This technique can also classify the individual data points based on their properties. Hundreds to thousands of indents were performed on additively manufactured T91 at room temperature, 300°C, 400°C, and 500°C across a square area with a side length of 120 μm to 400 μm. From this data, the hardness and reduced modulus at each point could be calculated and mapped. Using k-means clustering, we were able to arrange the data into three or four clusters corresponding roughly to the ferritic and martensitic phases as well as one or two intermediate clusters sampling both the phases. The hardness of these two phases appears to be quite stable as a function of temperature. Nanoindentation mapping and the k-means algorithm can therefore be used to rapidly assess the feasibility of heterogeneous materials under extreme conditions, such as nuclear reactor steels.

36 MATERIALS SCIENCE↗

Detecting Thermally-Induced Spinodal Decomposition with Picosecond Ultrasonics in Cast Austenitic Stainless Steels

Destructive techniques to monitor nuclear reactor component health may not always be available during service, as they are time-consuming and often require pre-installed inspection coupons. Non-destructive evaluation (NDE) techniques can bridge this gap by rapidly identifying the state of mission-critical reactor components, via inference between NDE-measurable material properties and those of ultimate interest, such as ductility and toughness. Here, we demonstrate one such inference about the health of thermally aged cast austenitic stainless steels. Observations of surface acoustic wave peak (SAW) splitting correlate with spinodal decomposition-induced embrittlement as destructively measured by Charpy impact energy. Elastodynamic calculations and molecular dynamics simulations of the effects of spinodal decomposition on elastic moduli support that the new acoustic modes present are due to stiffening in the δ-ferrite domains. Finally, this discovery enables one to probe structure-property relationships in materials in a greatly accelerated manner, suggesting that similar inference methods can be used to determine material fitness-for-service, or to quickly uncover new structure-property relationships.

304-type stainless steel↗

Clarification of creep deformation mechanism in heat-affected zone of 9Cr steels with In Situ experiments

This work quantified nonuniform creep deformation across the heterogeneous heat-affected zone (HAZ) of Grade 91 steel with sophisticated experiments, including an electric-thermal finite element model–assisted Gleeble thermomechanical simulation and a high-temperature creep testing with in situ digital image correlation (DIC). High temperature creep properties of HAZ sub-zones were quantitatively measured by the DIC. Furthermore, by utilizing peak temperature, hardness, local creep strain, and underlying microstructures, creep deformation mechanisms in HAZ were further understood. DIC measurements reveal a creep-vulnerable zone (CVZ) exposed to a peak temperature of 932°C (close to A C3 ) in the intercritical HAZ experienced the fastest creep strength degradation instead of the soft zone with the lowest hardness prior to creep. The significantly reduced precipitation strengthening from misplacement of undissolved and coarsened M 23 C 6 carbides led to a faster recrystallization of tempered martensite in the CVZ. Weak untransformed tempered martensite (ferrite grains) stabilized by local Cr enrichment from dissolved M 23 C 6 also harmed the CVZ's creep resistance.

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↗

Effects of magnetic field assisted heat treatment on the microstructure and mechanical properties of Fe-0.63 %C alloy

This study investigates the influence of an applied magnetic field on the microstructural evolution and mechanical properties of hypoeutectoid steels subjected to heat treatment. Tensile tests and microstructural analysis were performed on samples processed under varying magnetic field strengths (0 T, 5 T, and 9 T) and different austenitization incubation times. The results indicate that the application of a magnetic field alters the fraction of proeutectoid ferrite phase without changing the cooling rates and heat treatment process. Additionally, pearlite microstructural features such as lamellar spacing and misorientation angles exhibit variations under different field strengths. While the pearlite nodule diameter remains largely unaffected, an increase in percentage elongation and strength is observed in the 5 T treated sample, attributed to changes in microstructural features with the magnetic field. Additionally, the percentage elongation is reduced in the samples heat treated with reduced austenitization incubation times. The study further demonstrates that low-angle misorientations increased in the samples taken parallel to the magnetic field direction, influencing the mechanical response. These findings suggest that applying a magnetic field during heat treatment provides an additional driving force for phase transformations, offering a manufacturing process for tailoring microstructures and optimizing mechanical properties. Moreover, integrating magnetic fields in heat treatment processes has potential benefits in energy efficiency.

High magnetic field↗

Influence of nonmartensitic transformation products on mechanical properties of tempered martensite

The influence of nonmartensitic transformations products on the mechanical properties of tempered martensite is presented for samples of a SAE 4340 steel, partially isothermally transformed to specific high-temperature transformation products and quenched and tempered to hardness values of from 25 to 40 Rockwell c. The effects of upper bainite in amounts of 1,5, 10, 20 and 50 percent, of 5 percent ferrite, and of 5 percent pearlite on the tensile, impact, and fatigue properties are evaluated. (author)

Hodge, J M↗

Irradiation-assisted cracking of SA508-304L weldments with 308L groove filler and 309L butter in hot water immersion constant rate extension tests

Low alloy SA508 bainitic steel is often welded to 300 series austenitic stainless steel in nuclear power plants. These dissimilar metal weldments use 309L butter applied to the low alloy steel and 308L groove filler material to join the 309L to austenite. High alloy steels (such as the 308L and 309L material used here) have been identified as having greater susceptibility to irradiation-assisted stress corrosion cracking (IASCC). Evidence is presented here of cracking under tensile loads in 309L weldment butter in LWR hydrothermal conditions that correlates irradiation induced changes at δ ferrite–γ austenite phase boundaries and γ–γ grain boundaries; specifically intergranular Cr 23 C 6 precipitates. Cracking is not observed in irradiated 308L groove filler under the same conditions. Both the 309L butter and 308L filler material have a duplex or mixed δ–γ phase microstructure due to solidification during the welding procedure. We have performed constant extension rate autoclave immersion tests in BWR normal water chemistry hot water (288 °C, 10 MPa, 2000 wt. ppb dissolved oxygen, <100 nS/cm conductivity, neutral pH) of proton irradiated (2 MeV, approximately 3 displacements per atom at a depth of 10 μm) tensile specimens. Proton irradiation to the dpa levels used here induced Cr 23 C 6 carbide precipitation at γ–γ grain boundaries and δ–γ phase boundaries in the 309L butter but not the 308L filler. Cracking was observed in the proton-irradiated volume of 309L at these interfaces in the vicinity of the Cr 23 C 6 precipitates. We hypothesis the SA508 is the source of carbon in the 309L butter. Cr depletion at γ–γ grain boundaries was also observed and may also be a root cause of cracking. Furthermore, the 309L butter is under significant tensile residual stress in the weldment that adds to applied tensile loads and this too may be a contributing factor.

309L weld butter↗

Laser spot welding of additive manufactured 304L stainless steel

Here, the goal of this work is to understand if an additively manufactured 304L stainless steel exhibits similar spot-welding behavior as wrought 304L stainless steel. Due to the many differences between an additively manufactured component and wrought product, it is important to determine how the material interacts with the laser and how it affects the weld bead morphology. In this paper, the laser coupling efficiency, weld size, and solidification of spot welds produced in wrought and additively manufactured 304L stainless steel were investigated. The coupling efficiency of wrought and additively manufactured 304L stainless steel of similar surface condition were approximately the same over a range of applied laser energies. Laser welding of the untreated (rougher) surface of additively manufactured 304L, however, showed improved coupling efficiency ranging between 3.3 and 100%. The rougher surface traps the incoming light and increases the coupling efficiency at lower laser energies, while at higher energy, the absorption efficiency is dominated by intrinsic absorption from the keyhole formation rather than surface roughness. The resulting spot weld microstructures differed from welds made in wrought 304L and additively manufactured 304L. Welds made in wrought 304L were fully austenitic containing what is suspected to be massive austenite, which suggests that these welds solidified as primary ferrite. Welds made in additively manufactured 304L were also fully austenitic and contained both cellular austenite and what is suspected to be massive austenite. These observations mean that welds made in additively manufactured 304L solidified as primary ferrite and primary austenite. The differences in weld microstructures made in wrought and AM 304L can be attributed to differences in the composition and solidification rate.

304L stainless steel↗

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↗