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At least 1,423 records · Page 79

Experimental verification of a crystal plasticity-based simulation framework for predicting microstructure and geometric shape changes: Application to bending and Taylor impact testing of Zr

This paper is concerned with experimental verification of a recently developed multi-scale simulation framework for plastic deformation of metallic materials from quasi-static to impact deformation conditions. The framework is a visco-plastic self-consistent (VPSC) polycrystalline model embedded in an implicit finite element method (FE-VPSC) to provide a microstructure-sensitive constitutive response at each material point. Each material point of the FEM model is a polycrystalline aggregate with crystallographic deformation mechanisms operating at the single crystal scale with their evolving activity based on a dislocation density-based hardening law and texture. Four beams and three cylinders machined in different orientations from a textured plate of high-purity zirconium are tested quasi-statically in 4-point bending and at speeds of 100 m/s, 170 m/s and 243 m/s during Taylor impact tests, respectively. The variation in dimensional changes resulting from different sample orientations in the plate with respect to loading directions is measured for each sample. Moreover, texture and twinning characterization is performed using electron backscattered diffraction (EBSD). The deformation processes and underlying evolution of microstructure are successfully simulated using the FE-VPSC framework. In doing so, the model parameters are optimized and validated across a broad range of strain rates and temperatures. Simulation results in terms of geometrical changes and microstructural evolution are compared with the experimental measurements. The model predicts anisotropic material flow resulting from the hard-to-deform crystallographic directions, the development of gradients in texture and twinning through the geometries, tension–compression asymmetry, as well as the extent of plasticity under impact.

42 ENGINEERING↗

Additive manufacturing of AISI M2 tool steel by binder jetting (BJ): Investigation of microstructural and mechanical properties

The presented research demonstrates for the first time the successful processing of AISI M2 tool steel by binder jetting, a promising additive manufacturing technique capable of producing complex shapes with minimal residual stresses and isotropic properties. The optimal printing parameters were explored by varying processing parameters such as the binder saturation (45 %–105 %), binder set time (0 to 10 s), targeted bed temperature (50–60 °C), oscillator (2600–2750 rpm), recoater (20–28 mm/s), and roller speeds (200–300 rpm). Microstructural characterization and evaluation of mechanical properties of binder jetted parts were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) to study their chemical composition, powder morphology, microstructure, carbide morphologies, relative density, hardness, compressive strength, and ductility. Two powder sizes (5 and 10 μm) were used, and sintering was performed at varying temperatures (1270, 1280, and 1300 °C) and durations (60 and 120 min), followed by a furnace, air, and water cooling. An optimum hardness of ~970 HV was obtained when parts were sintered at 1270 °C for 60 min, followed by water quenching. Impressive compressive strength of ~ 3580 MPa was observed in the sample sintered at 1280 °C for 60 min duration, followed by air cooling. Furnace-cooled parts showed the highest density of ~95 %, whereas the relative density of air- and water-cooled parts varied between ~91 to 93.50 %, respectively. The microstructure of sintered samples revealed the formation of M 6 C stable carbide, M 2 C metastable carbide, MC as a secondary carbide, and a-Fe matrix, which contributed to the observed increase in mechanical properties.

36 MATERIALS SCIENCE↗

Microstructural and Micro-Chemical Evolutions in the Irradiated UCO Fuel Kernels of AGR-1 and AGR-2 TRISO Fuel Particles

AGR-1 and AGR-2 TRISO fuel particles were fabricated with slightly different fuel kernel chemical compositions, modified fabrication processes, different fuel kernel diameters, and changed 235U enrichments. To correlate those differences with the fuel kernel responses to neutron irradiations in terms of irradiated fuel microstructure, fission products chemical and physical states, and fission gas bubble evolutions, extensive microstructural and analytical characterizations were conducted. The studies used a state of art transmission electron microscopy (TEM) equipped with Energy-dispersive X-ray spectroscopy (EDS) of four silicon solid-state detectors which have super sensitivity and fast speed. The TEM specimens were prepared from selected AGR-1 and AGR-2 irradiated fuel kernels exposed to safety testing after irradiation. The particles were chosen to represent a representative irradiation conditions with a fuel burnup within the range from 10.8 to 18.6% FIMA, and the time-average volume-average temperatures vary from 1070 to 1287°C. The 235U enrichment was 19.74 wt.% for the AGR1 fuel kernels and 14.03 wt.% for the AGR-2 fuel kernels. The TEM results show that there were significant microstructural reconstructions in the irradiated fuel kernels for both the AGR-1 and AGR-2 fuels. There are four major phases including fuel matrix of UO2 and UC, U2RuC2, and UMoC2 in the irradiated AGR2 fuel kernel. Zr and Nb form solid solution in the UC phase. UMoC2 phase often shows a detectable concentration of Tc. Pd was found to mainly locate in the buffer layer or to be associated with fission gas bubble within the UMoC2 phase. The EDS maps qualitatively show that the rare-earth fission products (Nb, et al.) preferentially reside in the UO2 phase. In contrast, in the irradiated AGR1 fuel kernel, no U2RuC2 or UMoC2 precipitates were positively identified. Instead, there is a high number of rod-shape precipitates enriched with Ru, Tc, Rh, and Pd observed in the fuel kernel center and edge zone. The difference of microstructural and micro-chemical evolutions in irradiated fuel kernels between the AGR-1 and AGR-2 TRISO fuel particle may result from a combined factor of irradiation temperature, fuel geometry and chemical composition. However, the irradiation temperature probably play a more deterministic role. Limited electron energy loss spectroscopy (EELS) characterizations on the AGR2 fuel kernel show that there is nearly no carbon in the UO2 phase while a small fraction of oxygen was detected in the UC/UMoC2 phase.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A comprehensive investigation of the strengthening effects of dislocations, texture and low and high angle grain boundaries in ultrafine grained AA6063 aluminum alloy

Highlights: • Evolution of microstructure and mechanical properties of AA6063 after severe plastic deformation was investigated. • Average cell size shows a more solid relationship with mechanical properties rather than the average grain size. • This indicates that in addition to high angle boundaries, cell boundaries play a strengthening role. - Abstract: The effect of equal channel angular pressing (ECAP) on the microstructure and mechanical properties of AA6063 aluminum alloy was investigated. For this purpose, samples of AA6063 aluminum alloy were deformed up to 10 passes using ECAP and the evolution of microstructure, texture and dislocation density was investigated. It was found that the dislocation density increased and cells mostly surrounded by low angle boundaries (LABs) formed after 2 passes ECAP. Increasing the dislocation density continued with further processing and reached a maximum at the 4th ECAP pass. With further deformation to 6 passes, the dislocation density reduced, the fraction of high angle boundaries (HABs) increased and the averages of cell size and grain size reduced, significantly, which indicated the occurrence of grain refinement. However, a slight increase in dislocation density, average cell size (ACS) and average grain size (AGS), indicating coarsening, occurred when 10 passes of ECAP are imposed. Hardness, yield (YS) and ultimate tensile strength (UTS) increased continuously although the most significant enhancement occurred after 2 passes of ECAP. Investigating the correlation between the microstructure and mechanical properties indicated that Hall-Petch relationship was valid for ultrafine grained AA6063 before the coarsening started provided that the property of interest was correlated to average cell size but not the average grain size.

36 MATERIALS SCIENCE↗

Effects of heat treatments on microstructure and properties of Ti-6Al-4V ELI alloy fabricated by electron beam melting (EBM)

Electron beam melting (EBM) is a metal powder bed fusion additive manufacturing (AM) technology that is used to fabricate three-dimensional near-net-shaped parts directly from computer models. Ti-6Al-4V is the most widely used and studied alloy for this technology and is the focus of this work in its ELI (Extra Low Interstitial) variation. The mechanisms of microstructure formation, evolution, and its subsequent influence on mechanical properties of the alloy in as-fabricated condition have been documented by various researchers. In the present work, the thermal history resulting in the formation of the as-fabricated microstructure was analyzed and studied by a thermal simulation. Subsequently different heat treatments were performed based on three approaches in order to study the effects of heat treatments on the singular and exclusive microstructure formed during the EBM fabrication process. In the first approach, the effect of cooling rate after the solutionizing process was studied. In the second approach, the variation of α lath thickness during annealing treatment and correlation with mechanical properties was established. In the last approach, several solutionizing and aging experiments were conducted.

36 MATERIALS SCIENCE↗

Anisotropy evolution of elastomeric foams during uniaxial compression measured via in-situ X-ray computed tomography

We have characterized the three-dimensional evolution of microstructural anisotropy of a family of elastomeric foams during uniaxial compression via in-situ X-ray computed tomography. Flexible polyurethane foam specimens with densities of 136, 160 and 240 kg/m 3 were compressed in uniaxial stress tests both parallel and perpendicular to the foam rise direction, to engineering strains exceeding 70%. The uncompressed microstructures show slightly elongated ellipsoidal pores, with elongation aligned parallel to the foam rise direction. The evolution of this microstructural anisotropy during deformation is quantified based on the autocorrelation of the image intensity, and verified via the mean intercept length as well as the shape of individual pores. Trends are consistent across all three methods. In the rise direction, the material remains transversely anisotropic throughout compression. Anisotropy initially decreases with compression, reaches a minimum, then increases up to large strains, followed by a small decrease in anisotropy at the largest strains as pores collapse. Compression perpendicular to the foam rise direction induces secondary anisotropy with respect to the compression axis, in addition to primary anisotropy associated with the foam rise direction. In contrast to compression in the rise direction, primary anisotropy initially increases with compression, and shows a slight decrease at large strains. These surprising non-monotonic trends and qualitative differences in rise and transverse loading are explained based on the compression of initially ellipsoidal pores. Microstructural anisotropy trends reflect macroscopic stress-strain and lateral strain response. These findings provide novel quantitative connections between three-dimensional microstructure and anisotropy in moderate density polymer foams up to large deformation, with important implications for understanding complex three-dimensional states of deformation.

36 MATERIALS SCIENCE↗

Microstructural and magnetic property evolution with different heat-treatment conditions in an alnico alloy

Further property enhancement of alnico, an attractive near-term, non-rare-earth permanent magnet alloy system, primarily composed of Al, Ni, Co, and Fe, relies on improved morphology control and size refinement of its complex spinodally decomposed nanostructure that forms during heat-treatment. Using a combination of transmission electron microscopy and atom probe tomography techniques, this study evaluates the magnetic properties and microstructures of an isotropic 32.4Fe-38.1Co-12.9Ni-7.3Al-6.4Ti-3.0Cu (wt.%) alloy in terms of processing parameters such as annealing temperature, annealing time, application of an external magnetic field, as well as low-temperature “draw” annealing. Optimal spinodal morphology and spacing is formed within a narrow temperature and time range (~840 °C and 10 min) during thermal-magnetic annealing (MA). The ideal morphology is a mosaic structure consisting of periodically arrayed ~40 nm diameter (Fe-Co)-rich rods (α 1 phase) embedded in an (Al-Ni)-rich (α 2 phase) matrix. A Cu-enriched phase with a size of ~3–5 nm is located at the corners of two adjacent {110} facets of the α 1 phase. The MA process significantly increased remanence (B r ) (~40–70%) of the alloy due to biased elongation of the α 1 phase along the <100> crystallographic direction, which is closest in orientation to the applied magnetic field. As a result, the optimum magnetic properties of the alloy with an intrinsic coercivity (H cj ) of 1845 Oe and a maximum energy product (BH max ) of 5.9 MGOe were attributed to the uniformity of the mosaic structure.

36 MATERIALS SCIENCE↗

Oxidation and Associated Pore Structure Modification During Experimental Alteration of Granite

Weathering plays a crucial role in a number of environmental processes, and the microstructure and evolution of multi-scale pore space is a critically important factor in the weathering of geological formations. In igneous rocks the infiltration of meteoric water into initially relatively dry material can cause the rock to begin to disaggregate, increasing porosity and surface area, and allowing further disaggregation and weathering to occur. These processes, in turn, allow biota to colonize the rock, further enhancing the weathering rate. In some igneous rocks this may be driven by oxidation of primary minerals. One such mineral, biotite, has been repeatedly mentioned as a cause of cracking during oxidation. However, the scale-dependence of the processes by which this occurs are poorly understood. We cannot, therefore, accurately extrapolate laboratory reaction rates to the field in predictive numerical models. In order to better understand the effects of oxidation and test the hypothesis that fracture and disaggregation are initiated by swelling of oxidizing biotites, we reacted granite cores in a selenic acid-rich aqueous solution at 200°C for up to 438 days. Elevated temperatures and selenic acid were used to provide relatively fast reaction rates and highly oxidizing conditions in sealed reaction vessels. These experiments were analyzed using a combination of imaging, X-ray diffraction, Mössbauer spectroscopy, and small- and ultra-small angle neutron scattering to interrogate porosity and microfracture formation. The experimental results show little observable biotite swelling, but significant transport and growth of iron oxides and/or clays along grain boundaries throughout the sample. Significant increases in porosity were also observed at the sample rim, likely associated with feldspar alteration. Fractures and transport were observed throughout the core, suggesting that stresses due to crystallization pressures caused by the growing iron phases may be the initiating factors in granite weathering, possibly followed by biotite swelling after sufficient permeability is achieved.

Anovitz, Lawrence M.↗

Microstructural Analysis and Texture Evolution of the CVCEDed AZ31 Magnesium Alloy by Hot Rolling

Grain refinement is one of the important methods to improve the performance of magnesium alloy sheets. This paper attempts to prepare the billets of AZ31 magnesium alloy sheets by continuous variable cross-section direct extrusion (CVCDE) and then prepare sheets by rolling. The results show that the average grain size of the sheets rolled from extruded products by CVCDE with 2 interim dies reduced by 30% and the tensile strength increased by 12.6% compared with the sheets rolled from extruded products by traditional extrusion (CE), which is related to the dislocation multiplication in the corresponding conditions. The high dislocation density hinders the plastic deformation of the material, which is one of the internal factors that cause the increase in the strength of the material and the decrease in the plasticity. In addition, the basal surface of a lot of grains of the sheets rolled from extruded products by CVCDE with 2 interim dies is parallel to the RD-TD plane and the strength of texture is high. Meanwhile, the value of average Schmid factor of the sheets rolled from extruded products by CVCDE with 2 interim dies along the rolling direction is lowest, which result in lower plasticity. The above research provides a new idea for the development of high-performance magnesium alloy sheets.

36 MATERIALS SCIENCE↗

Evolution of weld metal microstructure in shielded metal arc welding of X70 HSLA steel with cellulosic electrodes: A case study

The microstructure of weld joint in X70 line pipe steel resulted from shielded metal arc welding with E6010 cellulosic electrodes is characterized using optical and electron microscopy. A range of ferritic morphologies have been identified ranging from polygonal inter- and intra-prior austenite grains allotriomorphic, idiomorphic ferrites to Widmanstätten, acicular and bainitic ferrites. Electron Backscatter Diffraction (EBSD) analysis using Image Quality (IQ) and Inverse Pole Figure (IPF) maps through superimposition of IQ and IPF maps and measurement of percentages of high and low angle grain boundaries was identified to assist in differentiation of acicular ferrite from Widmanstätten and bainitic ferrite morphologies. In addition two types of pearlitic structures were identified. There was no martensite detected in this weld structure. The morphology, size and chemistry of non-metallic inclusions are also discussed briefly. - Highlights: • Application of EBSD reveals orientation relationships in a range of phases for shielded metal arc welding of HSLA steel. • Nucleation sites of various ferrite morphologies identified • Formation of upper and lower bainite and their morphologies.

36 MATERIALS SCIENCE↗

From Powder to Power: Tailored Pre-Milling Strategy that Optimizes Microstructure for Efficient Hydrogen Evolution

The hydrogen evolution reaction (HER) plays a critical role in enabling large-scale electrolytic hydrogen production and advancing future technologies and fuel production. Among non-precious metals, NiMo-based catalysts are particularly attractive due to their capability to promote both water dissociation and hydrogen adsorption in alkaline media. However, conventional NiMo catalysts often suffer from incomplete alloying, particle aggregation, weak metal–support interactions, and surface oxidation, which significantly limit active site utilization, electronic conductivity, and long-term stability. Herein, we report a scalable, solid-state, two-step ball milling strategy for constructing an efficient NiMo/C catalyst for the HER. Pre-milling the metal precursors prior to carbon incorporation promotes efficient solid-state activation, leading to the formation of uniformly alloyed, ultrafine, and defect-rich Ni–Mo nanoparticles with robust metal–carbon interfacial anchoring. Benefiting from this integrated structural design, the optimized NiMo/C catalyst exhibits low overpotentials and Tafel slopes, reduced charge-transfer resistance, and excellent durability under alkaline conditions. Comprehensive structural and surface analysis reveal that the enhanced HER performance can be attributed to the synergistic interplay of homogeneous Ni–Mo alloying, uniform nanoparticle dispersion on a defect-rich carbon scaffold, enhanced accessibility of catalytically active sites, and optimized electronic coupling that stabilizes the catalyst surface. This work highlights the two-step solid-state ball milling strategy as a simple, robust, and scalable route for the preparation of effective and durable non-precious metal HER electrocatalysts, offering practical insights toward large-scale and inexpensive hydrogen production.

Yang, Xiaoxuan [Oak Ridge National Laboratory (ORN↗

Outlook on texture evolution in additively manufactured stainless steels: Prospects for hydrogen embrittlement resistance, overview of mechanical, and solidification behavior

Abstract Realizing application specific manufacture with fusion-based additive manufacturing (F-BAM) processes requires understanding of the physical phenomena that drive evolution of microstructural attributes, such as texture. Current approaches for understanding texture evolution in F-BAM are majorly considerate of the phenomena occurring only during solidification. This hinders the comprehensive understanding and control of texture during F-BAM. In this perspective article, we discuss several physical phenomena occurring during and after solidification that can determine texture in F-BAM processed stainless steels (SS). A crystal plasticity-coupled hydrogen adsorption-diffusion modeling framework is also leveraged to demonstrate the prospects of grain boundary engineering with F-BAM for enhanced hydrogen embrittlement resistance of SS. Implications of varying thermokinetics in F-BAM for solidification behavior of SS are discussed. Additionally, microstructural attributes that are key to high temperature mechanical performance of SS are highlighted. Considerations as outlined in this perspective article will enable grain boundary engineering and application specific microstructural design of SS with F-BAM. Graphical abstract

36 MATERIALS SCIENCE↗

Accelerated Ion Irradiation for Emulation of In-reactor Radiation Damage

Reactor core materials in both fast reactors and LWRs granted life extension must withstand irradiation to high doses at high temperature. Ferritic-martensitic (F-M) alloys are attractive candidates for structural components and fuel cladding in fast and thermal reactors, and high chromium and high nickel-containing austenitic steels are potential replacement alloys for LWR core materials. To reach high doses, self-ion irradiation is conducted with simultaneous He injection into both F-M and austenitic alloys, accompanied by reactor irradiations conducted in the BOR-60 fast reactor to assess the capability of ion irradiation to emulate the evolution of microstructure and mechanical properties in reactor. Computational models for defect cluster evolution are being developed and benchmarked against experimental data to ultimately provide predictive capability for the response of both microstructure (loops, voids, precipitates, etc.), and mechanical properties (hardening, ductility, slip behavior) to irradiation. A research program is aimed at understanding how to emulate neutron irradiation using ion irradiation. Results to date have been focused on microstructure and properties of ion irradiated alloys T91, 800H and Fe21Ce32Ni. Data from single ion irradiations are thus far in good agreement with that expected based on previous ion and neutron irradiation data. Dual ion irradiations and neutron irradiated samples are being evaluated and these will be the focus of future work. (authors)

36 MATERIALS SCIENCE↗