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At least 1,009 records · Page 56

Correlation of Microstructure and Mechanical Properties of Metal Big Area Additive Manufacturing

Metal Big Area Additive Manufacturing (MBAAM) is a novel wire-arc additive manufacturing method that uses a correction-based approach developed at the Oak Ridge National Laboratory (ORNL). This approach is an integrated software method that minimizes the dynamic nature of welding and compensates for build height. The MBAAM process is used to fabricate simple geometry thin walled specimens, using a C-Mn steel weld wire, to investigate the scatter in mechanical properties and correlate them to the underlying microstructure. The uni-axial tensile tests show isotropic tensile and yield properties with respect to building directions, although some scatter in elongation is observed. Large scatter is observed in the Charpy Impact tests. The microstructure characterization reveals mostly homogenous ferrite grains with some pearlite, except for some changes in morphology and grain size at the interface between the build and the base plate. The measured properties and microstructure are compared with the toughness and strength values reported in the literature, and a hypothesis is developed to rationalize the differences. Overall, the MBAAM process creates stable, isotropic, and weld-like mechanical properties in the deposit, while achieving a precise geometry obtained through a real-time feedback sensing, closed loop control system.

36 MATERIALS SCIENCE↗

Effects of Bi Addition on the Microstructure and Mechanical Properties of Nanocrystalline Ag Coatings

Here in this study we investigated the effects of Bi addition on the microstructure and mechanical properties of an electrodeposited nanocrystalline Ag coating. Microstructural features were investigated with transmission electron microscopy (TEM). The results indicate that the addition of Bi introduced nanometer-scale Ag-Bi solid solution particles and more internal defects to the initial Ag microstructures. The anisotropic elastic-plastic properties of the Ag nanocrystalline coating with and without Bi addition were examined with nanoindentation experiments in conjunction with the recently-developed inverse method. The results indicate that the as-deposited nanocrystalline Ag coating contained high mechanical anisotropy. With the addition of 1 atomic percent (at%) Bi, the anisotropy within Ag-Bi coating was very small, and yield strength of the nanocrystalline Ag-Bi alloy in both longitudinal and transverse directions were improved by over 100% compared to that of Ag. On the other hand, the strain-hardening exponent of Ag-Bi was reduced to 0.055 from the original 0.16 of the Ag coating. Furthermore, the addition of Bi only slightly increased the electrical resistivity of the Ag-Bi coating in comparison to Ag. Lastly, results of our study indicate that Bi addition is a promising method for improving the mechanical and physical performances of Ag coating for electrical contacts.

36 MATERIALS SCIENCE↗

Microcomputed X-Ray Tomographic Imaging and Image Processing for Microstructural Characterization of Explosives

Microstructural characterization of composite high explosives (HEs) has become increasingly important over the last several decades in association with the development of high fidelity mesoscale modeling and an improved understanding of ignition and detonation processes. HE microstructure influences not only typical material properties (e.g., thermal, mechanical) but also reactive behavior (e.g., shock sensitivity, detonation wave shape). A detailed nondestructive 3D examination of the microstructure has generally been limited to custom-engineered samples or surrogates due to poor contrast between the composite constituents. Highly loaded (>90 wt%) HE composites such as plastic-bonded explosives (PBX) are especially difficult. Here, we present efforts to improve measurement quality by using single and dual-energy microcomputed X-ray tomography and state-of-the-art image processing techniques to study a broad set of HE materials. Some materials, such as PBX 9502, exhibit suitable contrast and resolution for an automatic segmentation of the HE from the polymer binder and the voids. Other composite HEs had varying levels of success in segmentation. Post-processing techniques that used commercially available algorithms to improve the segmentation quality of PBX 9501 as well as zero-density defects such as cracks and voids could be easily segmented for all samples. Aspects of the materials that lend themselves well to this type of measurement are discussed.

36 MATERIALS SCIENCE↗

Effect of Initial Microstructure on the Toughness of Coarse-Grained Heat-Affected Zone in a Microalloyed Steel

Toughness of the coarse-grained-heat-affected-zone (CGHAZ) strongly depends on the prior austenite grain size. The prior austenite grain size is affected not only by chemical composition, thermal cycle, and dissolution of second-phase particles, but also by the initial microstructure. The effect of base metal microstructure (ferrite/pearlite obtained by air cooling and martensite obtained by water-quenching) on Charpy impact toughness of the CGHAZ has been investigated for different heat inputs for high-heat input welding of a microalloyed steel. A welding thermal cycle with a heat input of 100 kJ/cm and 400 kJ/cm were simulated on the MMS-300 system. Despite a similar microstructure in the CGHAZ of both the base metals, the average Charpy impact energy for the air-cooled base metal was found to be higher than the water-quenched base metal. Through thermo-kinetic simulations, it was found that a higher enrichment of Mn/C at the ferrite/austenite transformation interface of the CGHAZ of water-quenched base metal resulted in stabilizing austenite at a lower A1 temperature, which resulted in a coarser austenite grain size and eventually lowering the toughness of the CGHAZ.

36 MATERIALS SCIENCE↗

Investigation of Microstructures and Tensile Properties of 316L Stainless Steel Fabricated via Laser Powder Bed Fusion

In this study, a thorough investigation of the microstructures and tensile properties of 316L stainless steel fabricated via laser powder bed fusion (L-PBF) was done. 316L stainless steel specimens with two different thicknesses of 1.5 mm and 4.0 mm fabricated under similar conditions were utilized. Microstructural characterization was performed using optical microscopy (OM) and scanning electron microscopy (SEM) equipped with electron backscatter diffraction (EBSD). Melt pools and cellular structures were observed using OM, whereas EBSD was utilized to obtain the grain size, grain boundary characteristics, and crystallographic texture. The 1.5 mm thick sample demonstrated a yield strength (YS) of 538.42 MPa, ultimate tensile strength (UTS) of 606.47 MPa, and elongation to failure of 69.88%, whereas the 4.0 mm thick sample had a YS of 551.21 MPa, UTS of 619.58 MPa, and elongation to failure of 73.66%. These results demonstrated a slight decrease in mechanical properties with decreasing thickness, with a 2.4% reduction in YS, 2.1% reduction in UTS, and 5.8% reduction in elongation to failure. In addition to other microstructural features, the cellular structures were observed to be the major contributors to the high mechanical properties. Using the inverse pole figure (IPF) maps, both thicknesses depicted a crystallographic texture of {001} <101> in their as-built state. However, when subjected to tensile loads, texture transitions to {111} <001> and {111} <011> were observed for the 1.5 mm and 4.0 mm samples, respectively. Additionally, EBSD analysis revealed the pre-existence of high-density dislocation networks and a high fraction of low-angle grain boundaries. Interestingly, twinning was observed, suggesting that the plastic deformation occurred through dislocation gliding and deformation twinning.

316L stainless steel↗

Effect of heat treatment on microstructure and hardness of Grade 91 steel

The modified 9Cr-1Mo steel (Grade 91) is a material of choice in fossil-fuel-fired power plants with increased efficiency, service life, and reduction in emission of greenhouse gases. It is also considered a prospective material for the Next Generation Nuclear Power Plant for application in reactor pressure vessels at temperatures up to 650°C. In this paper, heat treatment of the modified 9Cr-1Mo steel was studied by normalizing and tempering the steel at various temperatures and times, with the ultimate goal of improving its creep resistance and optimizing material hardness. The microstructural evolution of the heat treated steels was correlated with the differential scanning calorimetric results. Optical microscopy, scanning and transmission electron microscopy in conjunction with microhardness profiles and calorimetric plots were used to understand the evolution of microstructure including precipitate structures in modified 9Cr-1Mo steel and relate it to the mechanical behavior of the steel. Thermo-CalcTM calculations were used to support experimental work and provide guidance in terms of the precipitate stability and microstructural evolution. Furthermore, the carbon isopleth and temperature dependencies of the volume fraction of different precipitates were constructed. The predicted and experimentally observed results were found to be in good agreement.

20 FOSSIL-FUELED POWER PLANTS↗

Influence of Thermal and Radiation Effects on Microstructural and Mechanical Properties of Nb-1Zr

Refractory metals and alloys offer attractive high-temperature properties, most of which are suitable for applications in nuclear environments including high temperature strength, good thermal conductivity, and compatibility with most liquid metal coolants. One of only two commercially produced Nb-alloys, Nb-1Zr has long been considered for various compact reactor designs. Nb-1Zr has also recently been considered for high-performance Gen IV gas reactor concepts. However, there are significant gaps in the irradiated materials database, especially at temperatures above 800 K. Recent work has shown that irradiated properties of Nb-1Zr are strongly controlled by phase-related transformations in the microstructure. Changes in the microstructure (obtained via scanning and transmission electron microscopy) and corresponding mechanical properties of Nb-1Zr were examined following fission reactor irradiation experiments at temperatures of 1073, 1223 and 1373 K to 1.9 dpa (displacements per atom) and compared with material thermally aged for similar exposure times of ~1100 h. Thermally driven changes in the development of precipitate phases showed a greater influence on mechanical properties compared to irradiation-induced defects for these irradiation conditions. The changes in material density, electrical resistivity and mechanical properties of the irradiated and thermally aged materials in association with microstructural developments are discussed.

36 MATERIALS SCIENCE↗

TEM Characterization of High Burn-up Microstructure of U-7Mo Alloy

As an essential part of global nuclear non-proliferation effort, the RERTR program is developing low enriched U-Mo fuels (< 20% U-235) for use in research and test reactors that currently employ highly enriched uranium fuels. One type of fuel being developed is a dispersion fuel plate comprised of U-7Mo particles dispersed in Al alloy matrix. Recent TEM characterizations of the ATR irradiated U-7Mo dispersion fuel plates include the samples with a local fission densities of 4.5, 5.2, 5.6 and 6.3 E+21 fissions/cm3 and irradiation temperatures of 101-136?C. The development of the irradiated microstructure of the U-7Mo fuel particles consists of fission gas bubble superlattice, large gas bubbles, solid fission product precipitates and their association to the large gas bubbles, grain subdivision to tens or hundreds of nanometer size, collapse of bubble superlattice, and amorphisation. This presentation will describe the observed microstructures specifically focusing on the U-7Mo fuel particles. The impact of the observed microstructure on the fuel performance and the comparison of the relevant features with that of the high burn-up UO2 fuels will be discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Understanding to Hierarchical Microstructures of Crab (Chinese hairy) Shell as a Natural Architecture

This work was done to better understand the microstructures, composition and mechanical properties of Chinese hairy crab shell. For fully revealing its hierarchical microstructure, the crab shell was observed with electron microscope under different magnifications from different facets. XRD, EDS, FTIR and TGA techniques have been used to characterize the untreated and chemically-treated crab shells, which provided enough information to determine the species and relative content of components in this biomaterial. Combined the microstructures with constituents analysis, the structural principles of crab shell was detailedly realized from different structural levels beyond former reports. To explore the relationship between structure and function, the mechanical properties of shell have been measured through performing tensile tests. The contributions of organics and minerals in shell to the mechanical properties were also discussed by measuring the tensile strength of de-calcification samples treated with HCl solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructural Characterization of Irradiated Fuels and Materials for the United States High Performance Research Reactor Fuel Development Program and the Fuel Cycle Research and Development Program

In an effort to contribute to the development of advanced nuclear fuel for research reactors, monolithic and dispersion plate fuels will be examined to determine how irradiation parameters such as fission density, fission rate, and irradiation temperature, as well as mechanical parameters such as composition and fabrication, affect the final microstructure of the fuel, post irradiation. Electron Backscatter Detection (EBSD) analysis capabilities of irradiated materials will be developed as well as improvements on irradiated sample preparation in order to provide higher quality samples for SEM, FIB, and TEM. In addition, image analysis techniques developed at Idaho National Laboratory (INL) will be employed to examine microstructural features such as fission product precipitates and fission gas bubbles. The main goals are to further develop EBSD capabilities on irradiated material; characterize microstructure of irradiated fuel to support qualification; develop a consistent, effective process for image analysis using INL developed software; and provide repeatable, statistically-confident, critically assessed data to further modeling efforts. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of Irradiation Mode on Irradiated Microstructure of HT9

Core components in Generation IV fast reactors are expected to be exposed to very high damage levels of 200 displacements per atom (dpa) and above. Numerous issues with in-reactor irradiations including residual radioactivity, expense, length of irradiation and availability have led to increased interest in ion irradiation as a surrogate. Self-ion irradiations can produce damage rates of around 10{sup -3} dpa/s with well-controlled temperature, doses and dose rates, allowing for accelerated irradiation testing. Along with these benefits, ion irradiations have been shown to reproduce many of the same irradiation-induced features as in reactor irradiations. Of particular interest at high doses is formation of voids, precipitates and evolution of the dislocation microstructure. However, the beam mode under ion irradiation must be addressed. Raster scanning has been shown to produce microstructural features similar to those observed in-reactor irradiations, however, since they are a pulsed type irradiation, they may induce artifacts as a result of annealing between pulses. Defocused beams have the benefit of full coverage 100% of the time, but may be challenging in terms of ensuring even irradiation over a large area as well as in reaching high enough currents to maintain acceptable damage rates to be useful as a surrogate. This paper reports upon the comparison of behavior of ferritic martensitic steels under a raster scanned or defocused beam mode. The objective is to determine the effect of beam condition the irradiated microstructural; specifically, on the formation of voids, precipitates and dislocation loops and analyze these results within the context of the FDRT model. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Microstructure of In-Core Molten Salt Corrosion Hastelloy N{sup R} and 316 Stainless Steel

Since 2011, many materials have been discussed for potential application in Fluoride salt-cooled High-temperature nuclear Reactors (FHRs), which are emerging as leading reactor concept for the next generation of nuclear reactors thanks to the benefits of a high degree of passive safety, high thermal efficiency, and low spent fuel volume. Among these discussed materials, Hastelloy N{sup R} and 316L stainless steel have been selected as the most likely candidate alloys for FHRs. To provide direct experience in integrating a real system using molten FLiBe salt for reactor operation, these two candidate alloys were experimentally tested in Li-7 enriched Li{sub 2}BeF{sub 4} (FLiBe) molten salt in the core of MIT Research Reactor (MITR) at 700 deg. C for 1000 hours. After in-core corrosion testing, some basic post-irradiation examinations (PIE) including weight change per unit area and surface profile as well as surface morphology were conducted in the MIT Nuclear Reactor Laboratory (NRL) and compared with out-of-reactor corrosion samples. The deep understanding of these alloys in high-temperature molten salt with strong neutron irradiation requires further microstructural analysis such as electron microscopy and energy dispersive spectroscopy on the surface and cross-section of the in-core corrosion tested samples. The challenge in the microstructural analysis is due to the high radioactivity from the gamma emitting isotopes formed in alloys during neutron irradiation. Additionally, the facilities that are authorized for radioactive materials are very limited on campus. In this study, the microstructure of the in-core corrosion tested Hastelloy N{sup R} and 316L stainless steel specimen was analyzed by using the facilities at the Center for Advanced Energy Studies (CAES) at Idaho National Laboratory (INL) through the Nuclear Science User Facilities (NSUF) Rapid Turnaround Experiment (RTE) program.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

SOC Microstructural Analyzer

This program was designed to analyze the 3-phase microstructure of the electrodes of a solid oxide fuel cell (SOFC) or electrolysis cell (SOEC), both referred to in combination as a solid oxide cell (SOC). It is agnostic to the exact system, so it could be repurposed to analyze any 3-phase microstructure. This tool directly analyzes segmented voxel-based data that has been segmented into phase IDs (1,2,3). The voxels will be analyzed directly for: - tortuosity factors - triple phase boundaries - 2-phase interfacial areas, using a meshed isosurface - mean diameters of each phase, using an inscribed sphere method - standard deviation of the diameters of each phase, from the same inscribed sphere data - connectivity information Comprehensive information is available in the readme file (within the zipped repository in Markdown language, and also available here as a rendered PDF). Please cite this page / DOI, as well as https://doi.org/10.1111/jace.14775, for usage.

3D microstructure↗

2nd World Congress on Integrated Computational Materials Engineering, Part II: Process Optimization: Multi-Objective Optimization of Microstructure in Wrought Magnesium Alloys.

The microstructural features that govern the mechanical properties of wrought magnesium alloys include grain size, crystallographic texture, and twinning. Several processes based on shear deformation have been developed that promote grain refinement, weakening of the basal texture, as well as the shift of the peak intensity away from the center of the basal pole figure — features that promote room temperature ductility in Mg alloys. At ORNL, we are currently exploring the concept of introducing nano-twins within sub-micron grains as a possible mechanism for simultaneously improving strength and ductility by exploiting a potential dislocation glide along the twin-matrix interface — a mechanism that was originally proposed for face-centered cubic materials. Specifically, we have developed an integrated modeling and optimization framework in order to identify the combinations of grain size, texture and twin spacing that can maximize strength-ductility combinations. A micromechanical model that relates microstructure to material strength is coupled with a failure model that relates ductility to a critical shear strain and a critical hydrostatic stress. The micro-mechanical model is combined with an optimization tool based on genetic algorithm. A multi-objective optimization technique is used to explore the strength-ductility space in a systematic fashion and identify optimum combinations of the microstructural parameters that will simultaneously maximize the strength-ductility in the alloy.

crystal plasticity↗

Tuning Microstructure of Mesophase Pitch Carbon Fiber by Altering the Carbonization Ramp Rate

The microstructure of mesophase pitch carbon fibers (CFs) are tuned by varying ramp rates from 1 to 50 °C min –1 up to 1000 °C to study the effect of ramp rate on CFs’ microstructure, thermal and mechanical properties with the goal of offsetting the cost by decreasing cycle time. The ramp rates represent carbonization times ranging from 16.4 to 1.17 h, not including cool down. Differential scanning calorimetry, thermogravimetric analysis, and derivative thermogravimetry are used to investigate the impact ramp rate has on the thermal properties of mesophase pitch. It is found that lower ramp rates are endothermic in nature with a lower temperature onset and maximum weight loss. Higher ramp rates possess an exothermic nature with higher temperatures resulting in maximal weight loss over a smaller range of temperatures. Mechanical testing shows varying CF strengths and moduli dependent on ramp rate and an optimized process is developed to produce the strongest CF. Furthermore, microstructural characterization revealed that faster ramp rates lead to smaller interplanar spacings and larger crystallites but possessed greater disorder.

36 MATERIALS SCIENCE↗

Optimization of Processing, Microstructure, and Hardness of an Al–Ce–Ni–Mn–Zr Alloy With Laser Additive Manufacturing

Here, this study examines the processing behavior, microstructure, surface roughness, and hardness properties of an aluminum alloy containing 8.2 Ce, 4.5 Ni, 0.5 Mn, and 0.7 Zr (wt%) fabricated using laser powder bed fusion. Sixty samples were produced across a range of laser powers, scan speeds, and hatch spacings to evaluate their effect on porosity, hardness, and microstructural features. Porosity was measured using X-ray computed tomography, while microstructure and surface roughness were characterized by scanning electron (SEM) and laser confocal microscopy. High dense and cracking-free Al–Ni–Ce alloy was successfully manufactured. Porosity showed a U-shaped dependence on energy input, increasing under both insufficient and excessive melting conditions. Hardness increased with cooling rate due to finer cellular structures and solute redistribution. A general statistical model was developed to capture the relationships between processing parameters and material response. Results identify a narrow processing window defined by laser powers between 350 and 370 W, scan speeds from 1400 to 1800 mm/s, and hatch distances between 0.14 and 0.18 mm. Within this window, porosity is minimized (below 0.01%) and hardness is maximized (up to 160 HV), demonstrating that careful control of these parameters enables dense, high strength aluminum components suitable for demanding structural applications.

Aluminum alloys↗

Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

Microstructure of argyrodite solid-state electrolyte (SSE) critically affects lithium metal electrodeposition/dissolution. While the stability of unmodified SSE is mediocre, once optimized state-of-the-art electrochemical performance is achieved (symmetric cells, full cells with NMC811) without secondary interlayers or functionalized current collectors. Planetary mechanical milling in wet media (m-xylene) is employed to alter commercial Li 6 PS 5 Cl (LPSCl) powder. Quantitative stereology demonstrates how milling progressively refines grain and pore size/distribution in the SSE compact, increases its density, and geometrically smoothens the SSE-Li interface. Mechanical indentation demonstrates that these changes lead to reduced site-to-site variation in the compact's hardness. Milled microstructures promote uniform early-stage electrodeposition on foil collectors and stabilize solid electrolyte interphase (SEI) reactivity. Analysis of half-cells with bilayer electrolytes demonstrates the importance of microstructure directly contacting current collector, with interface roughness due to pore and grain size distribution being key. For the first time, short-circuiting Li metal dendrite is directly identified, employing 1.5 mm diameter “mini” symmetrical cell and cryogenic focused ion beam (cryo-FIB) electron microscopy. The branching sheet-like dendrite traverses intergranularly, filling the interparticle voids and forming an SEI around it. Importantly, mesoscale modeling reveals the relationship between Li-SSE interface morphology and the onset of electrochemical instability, based on underlying reaction current distribution.

25 ENERGY STORAGE↗

A Comprehensive Experimental Study on Microstructure‐Graded Graphite Anodes for Enhancing Fast‐Charging Capability of Lithium‐Ion Batteries

Lithium‐ion batteries with high gravimetric capacity density and improved cycle life performance under fast‐charging conditions are crucial for widespread electric vehicle (EV) adoption. This study investigates how designing graphite anode microstructure, specifically porosity, and particle‐size gradients, improves lithium‐ion (Li + ) transport during fast‐charging conditions. Three‐layered graphite anodes with varying porosity (24%, 36%, 46%) and particle size gradients (3, 5, 10 μm) were compared to a conventional single‐layered electrode in half‐cell configurations. At room temperature and high discharge rate (2C), both gradient structures showed significantly enhanced capacity retention (80% and 67% vs. 50%) compared to the conventional electrode, highlighting the effectiveness of microstructure engineering for fast charging. The study also investigated the temperature's impact on cycle life. After 200 cycles at 2°C and 45°C, all gradient structures demonstrated superior capacity retention (≈80%) compared to the conventional electrode (35%), suggesting the gradients mitigate degradation rate at high temperatures. Electrochemical impedance spectroscopy confirmed superior Li+ diffusion and lower resistivity in gradient electrodes. Simulations explored the influence of gradient profiles on reaction kinetics across the electrode thickness. Overall, this research demonstrates that the fast‐charging capability of graphite electrodes can be greatly enhanced by engineering the electrode microstructure, thereby making EV technology more accessible and appealing.

Ahmadi, Soma↗