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At least 865 records · Page 48

Machine-to-machine variability of roughness and corrosion in additively manufactured 316L stainless steel

Numerous studies on the corrosion response of metal AM have been conducted. Nonetheless, the specimens being tested are commonly ground or polished to remove the outer as-built surface. If metal AM is truly going to be employed as a transformative technology that can produce complex shapes that do not require traditional machining, then the material needs to be evaluated in the as-built state. The reality is that AM alloys have shown significant inconsistencies regarding as-built surface texture, topology, and residual stress. One metric that has shown significant unpredictability in the literature is the susceptibility to localized corrosion of typically passive alloys, such as stainless steel (SS). There are a large number of studies that have attempted to understand the corrosion response of metal AM materials, but these studies are typically performed on materials that have been printed on a single machine and often mechanically polished to a smooth finish. This study compares the corrosion response of as-built AM, laser-beam powder bed fusion (LB-PBF), 316L SS parts that have been fabricated on five different machines. The majority of this work focused on understanding the susceptibility to localized corrosion of AM metals with respect to machine-dependent variables, namely surface roughness, and build angle. Surface roughness data was collected using scanning white light triangulation, laser scanning confocal microscopy, and coherence scanning interferometry. The results show that there is significant variability (p two-tail < 0.05) in the susceptibility to local corrosion initiation of LB-PBF 316L SS samples built on different machines. Surface oxides were probed with electron dispersive spectroscopy and revealed that variations in local corrosion susceptibility likely arise from differences in the stability of the passive film caused by chemical segregation, unique microstructure, and tortuous roughness features at the as-built surfaces. The variability of roughness and corrosion properties from test samples printed on different machines was corroborated by property measurements performed at five different testing sites, proving reproducibility of the data. Most importantly, this study shows that if the as-built surface layer is removed through grinding or electropolishing the machine-to-machine variation observed in the corrosion susceptibility is reduced.

36 MATERIALS SCIENCE↗

Interfacial characteristics of P91 steel - Inconel 740H bimetallic structure fabricated using wire-arc additive manufacturing

Although bimetallic structures can offer unique solutions to engineering problems with varying functionality, joining two dissimilar alloys using additive manufacturing involves challenges such as cracking and segregation. In this work, bimetallic structures of Inconel 740H superalloy and P91 steel are processed using wire-arc additive manufacturing (WAAM) for the first time. P91 steel is directly deposited over 740H with a cooling time of 20 minutes in between the two depositions. During microstructure characterization, a large gradient zone with coarse grains spanning for ~2200 μm is observed. Moreover, the microhardness of the gradient zone is the least in comparison with the P91 and 740H deposits. No deleterious phase formation is found; however, intergranular cracks are observed along the gradient zone. In order to deduce the reason for cracking, non-equilibrium solidification simulations are performed for the mixed compositions of P91 and 740H in the gradient zone. Here, the reasons for crack formation in the gradient zone are the sudden change in the volumetric coefficient of thermal expansion due to the formation of MC carbides as well as the development of local strains from the thermal residual stresses. Therefore, altering the deposition sequence and introducing gradient layers with mixed composition between the P91 and 740H deposits will be beneficial in achieving defect-free builds. Through the integration of experiments and simulation, this work gains valuable insights into the processability of dissimilar alloy manufacturing using the WAAM technique.

20 FOSSIL-FUELED POWER PLANTS↗

Validating continuum theory for Cottrell atmosphere solute drag by molecular dynamics simulations

When a dislocation moves through a field of mobile solute atoms, solutes segregate to the dislocation and form Cottrell atmospheres which exert solute drag forces. Over the last 70 years, continuum theory has been used extensively to estimate these drag forces and their dependence on the dislocation velocity, however few prior works have validated the accuracy of continuum theories. Here, in this work, molecular dynamics (MD) simulations of dislocation motion in face-centered cubic Ni containing interstitial H atoms were performed in order to test the accuracy of continuum theory predictions. Our results demonstrate that continuum theory provides an accurate estimate of the solute drag force for velocities below the critical velocity at which the solute drag force is maximized. Above the critical velocity, continuum theory systematically deviates from MD. Additional analysis reveals that this deviation results from the multi-valued and unstable nature of solute drag under load control, and also from the transition to random solute drag which occurs at high velocities.

Dislocations↗

Collaborative or competitive phase transformation processes in an additively manufactured-maraging steel M300

Although retained austenite is present in minor amounts in as-built additively manufactured-maraging steels, its evolution during ageing is key to controlling the final microstructure. This study investigates the relationship between austenite reversion and precipitation evolution during ageing, particularly whether these processes compete or cooperate. Using Scanning/Transmission Electron Microscopy, Atom Probe Tomography and Thermo-Calc® PRISMA simulations, the presence and evolution of retained austenite, Ni 3 Ti and Fe 7 Mo 6 intermetallic phases was characterised across different ageing conditions. Experimental results revealed the presence of non-enriched austenite in the as-built condition. Nevertheless, with increasing ageing temperature, Ni and Mo segregation became evident. High-Resolution Transmission Electron Microscopy revealed that Ni 3 Ti precipitation primarily occurred within the martensitic matrix, while Fe 7 Mo 6 nucleated preferentially at the austenite-martensite interface. PRISMA simulations indicated early and rapid precipitation in solute-enriched areas (i.e., intercellular regions), with Ni 3 Ti forming prior to Fe 7 Mo 6 . Both experimental and simulation results suggested Ni diffusion controls retained austenite growth, while Ti and Mo drive Ni 3 Ti and Fe 7 Mo 6 precipitation, respectively. The evidence reported in this work supports a both collaborative and independent phase transformation mechanism, where austenite reversion and precipitation co-evolve.

42 ENGINEERING↗

Structural uniformity and compositional homogeneity of solid-phase alloyed rod

Solid-phase processes have emerged as an alternative to fusion-based alloying to avoid coarse microstructures, undesirable phase formation, and high energy consumption. However, achieving uniform distribution of alloying elements during friction-based processing remains challenging due to highly heterogeneous thermomechanical conditions. This work evaluates the structural uniformity and compositional homogeneity of Al–Cu–Zn alloyed rods produced by friction extrusion (FE) and establishes the role of the rotational speed to feed rate ratio (N/V) on alloying effectiveness. A systematic matrix of FE experiments was conducted at constant extrusion ratio with N/V values ranging from 3.7 to 300. Compositional uniformity was assessed along the rod length (ICP-OES), in three dimensions (X-ray computed tomography), and at the microscale (SEM–EDS), supported by a gray-level co-occurrence matrix (GLCM)–based homogeneity metric. Smoothed particle hydrodynamics (SPH) simulations were used to reveal material flow and thermomechanical fields. Results show that N/V = 100 produces a high-shear mixing zone that eliminates the unmixed core and enables near-full dissolution and dispersion of Cu and Zn. At lower N/V, a laminar flow region persists at the rod center, causing segregation and large composition gradients. The combined experimental–computational analysis provides mechanistic insight into the transition from fragmented particle dispersion to thermomechanically assisted metallurgical mixing. This study establishes processing–structure relationships for solid-phase alloying and provides guidance for achieving homogenized compositions comparable to wrought alloys via rapid, scalable FE processing.

Aluminum↗

Origins of high ductility exhibited by an extruded magnesium alloy Mg-1.8Zn-0.2Ca: Experiments and crystal plasticity modeling

Low ductility and strength are major bottlenecks against Mg alloys' wide applications. In this work, we systematically design the composition and fabrication process for a low-alloyed Mg-Zn-Ca alloy, showing that it can be extruded at low temperatures (~ 250 degrees C) and high speeds (~2 mm/s). After the extrusion, this alloy exhibits a substantially weakened basal texture, relatively small grain size, very high tensile elongation (~ 30%), and good strength. The origin of the considerably improved ductility was studied using a combination of three-dimensional atom probe tomography (3D-APT), transmission electron microscopy (TEM), electron backscattered diffraction (EBSD) in conjunction with surface slip trace analysis, in-situ synchrotron X-ray diffraction, and elasto-plastic self-consistent (EPSC) modeling. Co-segregation of Zn and Ca atoms at a grain boundary is observed and associated with texture weakening and grain boundary mediated plasticity, both improving the ductility. While basal slip and prismatic slip are identified as the dominant deformation systems in the alloy, the ratio between their slip resistances is substantially reduced relative to pure Mg and most other Mg alloys, significantly contributing to the improved ductility of the alloy. This Mg-Zn-Ca alloy exhibiting excellent mechanical properties and low fabrication cost is a promising candidate for industrial productions.

36 MATERIALS SCIENCE↗

Martensitic transformation induced strength-ductility synergy in additively manufactured maraging 250 steel by thermal history engineering

Maraging steels are known for their exceptional strength but suffer from limited work hardening and ductility. Here, in this study, we report an intermittent printing strategy to tailor the microstructure and mechanical properties of maraging 250 steel via tuning the thermal history during wire-arc directed energy deposition. By introducing a dwell time between adjacent layers, the maraging 250 steel is cooled below the martensite start temperature, triggering thermally-driven martensitic transformation during the printing process. Thermal cycling during subsequent layer deposition results in the formation of reverted austenite which shows a refined microstructure and induces elemental segregation between martensite and reverted austenite. The Ni enrichment in the austenite promotes stabilization of the reverted austenite upon cooling to room temperature. The reverted austenite is metastable during deformation, leading to strain-induced martensitic transformation under loading. Specifically, a 3 min interlayer dwell time produces a maraging 250 steel with approximately 8% reverted austenite, resulting in improved work hardening via martensitic transformation induced plasticity during deformation. Meanwhile, the higher cooling rate and refined prior austenite grains lead to substantially refined martensitic grains (by approximately fivefold) together with an increased dislocation density. With 3 min interlayer dwell time, the yield strength of the printed maraging 250 steel increases from 836 MPa to 990 MPa, and the uniform elongation is doubled from 3.2% to 6.5%. This intermittent deposition strategy demonstrates the potential to tune the microstructure of maraging steels for achieving strength-ductility synergy by engineering the thermal history during additive manufacturing.

Additive manufacturing↗

Revealing the complex chemistry of grain boundaries in K-doped BaFe 2 As 2 with atom probe tomography

Iron-based superconductors have attractive properties for high-field applications, but there is a lack of understanding of the effect of grain boundary chemistry on the in-field performance. The near atomic-scale resolution, ppm sensitivity and 3D analysis offered by atom probe tomography make it a powerful tool to investigate the nanoscale structure and chemistry of these defects in fine-grained K-doped BaFe 2 As 2 samples. A computational method to systematically extract and compare the Gibbsian interfacial excess of chemical species across grain boundaries has been explored in this work. The robustness of the method has been tested by evaluating the effects of selected variables on simulated APT datasets. The accuracy and precision of the calculated Gibbsian interfacial excess were found to be stable over a range of analysis conditions: varying grain boundary widths and detection efficiencies, spatial precisions below 1.5 nm, and bin widths between 1.2 and 1.6 nm. For the K-doped BaFe 2 As 2 samples studied, segregation of As, Ba, K and impurities of O, Na, and Sb were found at grain boundaries. The Gibbsian excess values were found to vary widely between different boundaries, showing the complexity of the grain boundary chemistry in this material. Possible links between the observed critical current density (Jc) of these samples and their nano- and micro-structure have also been investigated and discussed.

36 MATERIALS SCIENCE↗

Evolution of glass structure during femtosecond laser assisted crystallization of LaBGeO 5 in glass

Single crystal LaBGeO 5 architecture formed in La 2 O 3 -B 2 O 3 -2GeO 2 glass serves as a model system for understanding of the transformation from glass to single crystal under fs laser irradiation. This transformation is highly sensitive to glass composition, raising the need to understand how the glass structure and composition evolve during crystallization. In this work, micro X-ray absorption spectroscopy and X-ray fluorescence mapping were used to study the glass structure and composition preceding LaBGeO5 crystallization in the region surrounding the single crystal growth front. The results show precipitation of germanium nanoparticles, as well as anisotropic segregation of Ge and La prior to LaBGeO5 crystallization, which are explained assuming electromigration in high fields within the plasma formed by the fs laser irradiation. However, these nanoparticles do not serve as sites for heterogeneous nucleation. Furthermore, the similarity of local structure around Ge in the starting glass and the ultimate crystal appears to enhance the crystallization process.

36 MATERIALS SCIENCE↗

Method for measurement of TRISO kernel and layer volumes by X-ray computed tomography

Layer dimensions are key parameters for as-fabricated tristructural-isotropic (TRISO) particle fuel as well as for post-irradiation examination of particle performance. Layer thicknesses are typically measured by optical microscopy of the particle cross section near mid-plane, while layer volumes are estimated with serial sectioning and microscopy. This method for measuring layer volumes is limited due to the resolution limit imposed by slice thickness and the effect of the polishing process on delicate irradiated particle microstructures. In this study, image processing software has been developed to segregate the three-dimensional (3D) TRISO particle images provided by x-ray computed tomography (XCT) into high-resolution volumetric data for the kernel, all particle layers, and any internal voids introduced during irradiation. These data can be used to analyze key in-reactor behaviors of TRISO particles such as kernel swelling or buffer shrinkage, which are important inputs for fuel performance modeling.

36 MATERIALS SCIENCE↗

Microstructural characterization of cold-worked 316 stainless steel flux thimble tubes irradiated up to 100 dpa in a commercial Pressurized Water Reactor

Two flux thimble tubes (FTT) made of 15% cold-worked 316 stainless steel (SS) were harvested from Ringhals Pressurized Water Reactor (PWR) Unit 2, with peak damages of 76 and 100 displacements per atom (dpa) after 29 and 34 years’ service, respectively. Specimens sectioned from parent tubes were comprehensively characterized with nominal damage levels of ~0, ~41, ~74, 76, and 100 dpa at a nominal temperature range of 285-323 °C. Both FTTs contained helium and hydrogen gases as transmutation products. The helium follows a production rate of ~9.8 appm/dpa, while environmental factors complicate hydrogen production obscuring an exact H/dpa ratio. Irradiation-induced dislocation loops, nano-cavities, solute clusters, and microsegregation were all observed. The dislocation loops and nano-cavities indicated saturation at 41 dpa. The solute clusters continued to evolve with Ni-Si clusters formed at 41 dpa, and Ni-Si-Mn-P clusters formed at 74 and 100 dpa, but neither clusters exhibited distinct diffraction patterns at any damage levels. Solute clusters were observed to frequently be co-located with dislocation loops, but fully decorated loops were rarely detected. Significant radiation-induced segregation (RIS) was observed around grain boundaries at all damage levels. The modified inverse Kirkendall (MIK) model captured the RIS behavior of major elements. Large cavities within or around an Mn-S rich region were observed for the first time. Through all the damage levels, void swelling is always below 0.05%, making significant dimensional change unlikely in core internals when used at similar conditions. Meanwhile, the role of overwhelming nanocavities, presumably helium bubbles, should be considered in other potential degradation mechanisms, including irradiation-assisted stress corrosion cracking, embrittlement, and loss of fracture toughness, which remain the concerns for extended operation of nuclear power plants.

Post Irradiation Examination, Isotope Dilution Mas↗

Atom Probe Tomography Characterization of High-Dose Ion Irradiated MA957

This paper presents a comprehensive characterization study of the microstructural responses to ion irradiation of the oxide dispersion strengthened (ODS) ferritic alloy MA957 using atom probe tomography (APT). The MA957 specimens were irradiated by 1.8 MeV Cr3+ ions to doses and temperatures relevant to advanced fast reactors (100 and 500 dpa at 400-500 °C). The average sizes of the YTiO particles decreased slightly after irradiation at all temperatures, with the most pronounced change at 400 °C. The particle number densities for 400 and 500 °C were slightly below number densities for the unirradiated condition, while the values were slightly higher at 420 and 450 °C. This behavior is consistent with the Nelson-Hudson-Mazey rate theory model that considers the competing effects between recombination and dissolution. An increase in the Y/Ti ratio of the YTiO particles was observed at the two lower temperatures. The formation of Cr-rich precipitates (a') was observed in specimens irradiated at temperatures up to 450 °C. Irradiation-induced segregation on grain boundaries was also investigated. Grain boundary element concentration profiles and ion maps demonstrate differences among the irradiation temperatures, with most datasets differing from the unirradiated condition. A key focus of this ion irradiation study is the high-dose response, and this quantitative assessment revealed relatively small but distinct effects of irradiation on microstructure evolution. Overall, these results showing minor second phase evolution suggest that MA957 should retain mechanical performance generally well up to 500 dpa for the irradiation temperatures studied.

Wang, Jing↗

Formation of multicomponent alloy particles in doped ceria under I 2+ ion irradiation and thermal annealing

Multicomponent alloys resembling the e-phase particles in nuclear fuel have the potential to immobilize 99 Tc in a stable waste form. Formation of such multicomponent alloys under extreme conditions is studied in a non-activated model system: CeO 2 doped with 2 wt% Mo, 1.5 wt% Ru, 0.75 wt% Pd, 0.5 wt% Re and 0.25 wt% Rh. The doped CeO 2 films were irradiated with I 2+ ions (610°C, 10 16 and 5×10 16 I 2+ /cm 2 ). For selected samples post-irradiation heat treatment was conducted (900°C, 1100°C). Analytical TEM revealed the formation of 5-20 nm precipitates containing Pd, Mo, and Re sometimes associated with cavities. Iodine was found to segregate to grain boundaries and cracks. After heat treatment at 1100°C, the CeO 2 matrix had recrystallized. Precipitates containing Pd, Mo, Re, and Ru were observed near the interface with the polycrystalline YSZ substrate. It follows that Pd is the most mobile element, followed by Mo and Re. Finally, while irradiation promotes precipitation, high-temperature effects are more significant.

36 MATERIALS SCIENCE↗

(S)TEM/EDS study of native precipitates and irradiation induced Nb-rich platelets in high-burnup M5®

We have investigated microstructure and microchemistry of precipitates and dislocation loops in high-burnup M5® using (scanning) transmission electron microscopy ((S)TEM) equipped with energy dispersive X-ray spectroscopy (EDS). Two (S)TEM lamellae were made by cryo-FIB from the same cladding sample. The Nb-rich native precipitates were found in the metal, in the suboxide and in the oxide. Upon diffraction analysis, most of the Nb-rich native precipitates in the metal matrix remain as β-Nb phase, while no β-Nb native precipitates were found in the oxide. Nearby the oxide and metal (O/M) interface, the native precipitates in the oxide were already oxidized into t-NbO2 phase. At further distance away from the O/M interface, the Nb-rich native precipitates were gradually oxidized and became amorphous. Besides the native precipitates, Nb-rich irradiation induced precipitates (IIPs) were found in the metal matrix. Using g = <0002> vector for imaging, the length of the IIPs was aligned with dislocation loops. However, no Nb segregation to the dislocation loops themselves was observed. For the first time, we report that IIPs indeed exist in the oxide but only within about 1.5 µm away from O/M interface. However, the oxidation state of the IIPs in the oxide is still unclear. The presence of both native precipitates and IIPs in the oxide may indicate the Nb concentration in the oxide solid solution remain low nearby the O/M interface, which may explain the reduced corrosion kinetics of in-pile M5®. On the other hand, no IIPs were observed in the oxide at further distance and this may indicate that they have eventually dissolved back into the oxide. A few mechanisms related to IIPs stability in the oxide are presented.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Perspectives on multiscale modelling and experiments to accelerate materials development for fusion

Prediction of material performance in fusion reactor environments relies on computational modelling, and will continue to do so until the first generation of fusion power plants come on line and allow long-term behaviour to be observed. In the meantime, the modelling is supported by experiments that attempt to replicate some aspects of the eventual operational conditions. In 2019, a group of leading experts met under the umbrella of the IEA to discuss the current position and ongoing challenges in modelling of fusion materials and how advanced experimental characterisation is aiding model improvement. This review draws from the discussions held during that workshop. Topics covering modelling of irradiation-induced defect production and fundamental properties, gas behaviour, clustering and segregation, defect evolution and interactions are discussed, as well as new and novel multiscale simulation approaches, and the latest efforts to link modelling to experiments through advanced observation and characterisation techniques.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Evolution of the role of molybdenum in duplex stainless steels during thermal aging: From enhancing spinodal decomposition to forming heterogeneous precipitates

Thermal aging of ferrite in duplex stainless steels leads to a complex microstructural evolution that can give way to large deleterious changes in mechanical properties. The microstructural evolution mechanisms that happen concurrently are strongly linked to minor changes in composition. By characterizing duplex stainless steels with various compositions over a range of aging conditions, it was revealed that adding a modest amount of Mo to cast austenitic stainless steel (such as changing from grade CF3 to grade CF3M) not only increases the kinetics of spinodal decomposition and Ni-Si-Mn-rich G-phase precipitation, but it also forms a separate Mo-rich phase. At shorter equivalent aging times, Mo segregates from Fe and towards Cr accelerating spinodal decomposition. At longer aging times, Mo enriches in the Ni-Si-Mn clusters before phase separating into an adjoined Mo-rich cluster. We found that these phase changes and precipitation events result in a rather steep drop in fracture and impact toughness. These results will inform the design of similar alloys for use at high temperatures.

36 MATERIALS SCIENCE↗

Investigation of constituent redistribution in U-Pu-Zr fuels and its dependence on varying Zr content

This contribution investigates fuel constituent segregation and fuel-cladding chemical interactions (FCCI) in three U-Pu-Zr fuel pins irradiated to ~11% burnup in Experimental Breeder Reactor-II as part of the X441 DP-1 experiment. In examined pins, Zr content ranged from 6 to 10 and 14 wt.%, while Pu concentration was constant at 19 wt.% Pu. The primary goal of the investigation was to determine the role Zr content plays in fuel performance and this manuscript provides assessment of both constituent redistribution and FCCI as a function of axial position. FCCI was observed in all pins, though no cladding failure was noted. Optical and scanning electron microscopy (SEM) results show that variation in Zr content alters the number and relative size of constituent redistribution zones in the fuel. For example, larger Zr-rich central regions and smaller U-rich intermediate regions were observed in 14 wt.% Zr fuels. More importantly, all examined fuels have four or more discrete constituent redistribution regions, where each region has dissimilar morphological features. The existence of four to six distinctive regions deviates from traditionally accepted three region redistribution model, highlights complexity of constituent redistribution in this metal fuel, and identifies the need to conduct additional studies using state-of-the-art instrumentation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Helium interaction with solutes and impurities in neutron-irradiated nanostructured ferritic alloys: A first principles study

Density functional theory calculations are performed to explore the binding between He and alloying solutes, impurities, and transmutation products expected in neutron irradiated nanostructured ferritic alloys (NFAs), here 14YWT is taken as an example. Elements that exhibit significant binding (attraction) with an interstitial He are Y (binding energy = 0.46 eV), Mg (0.32), O (0.33), Ti (0.16), and C (0.15). Those that provide significant binding to a substitutional He are O (1.44), Y (1.24), N (0.73), H (0.56), Mg (0.52), Ti (0.34), Si (0.34), C (0.33), Al (0.32), Ni (0.26), Ta (0.23), and Mn (0.16). The presence of these elements in Fe matrix could reduce the transport of He towards oxide particles, dislocations, and internal boundaries, and could promote He bubble nucleation in the matrix. For convenience, we compile existing binding energy data of He with He n and He n V (He-vacancy) clusters. Dissociation pathway analysis reveals that, in general, the most likely dissociation of a He n V cluster is by a sequential emission of individual He atoms. Furthermore, larger bubbles are more prone to dissociation than smaller ones. In addition, we estimate the binding energy (segregation energy) of He in bulk Y 2 Ti 2 O 7 (YTO) single crystal, YTO/Fe interface, and YTO particle embedded in Fe, with respect to interstitial He in Fe, from existing formation energies of He in these structures. We also compile available data of He binding with Fe self-interstitial atom (SIA), SIA clusters, and edge and screw dislocations. Note that given the absence of DFT data, the binding with SIA clusters and dislocations are gathered from simulations with empirical potentials. Finally, the data presented in this paper is important to inform multiscale simulations of He bubble accumulation.

36 MATERIALS SCIENCE↗