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At least 433 records · Page 24

Extending Interfaces in 3D to Achieve Superior Nanoscale Strength in Ti/Nb Nanolaminates

Tuning the atomic-level structure of nanolaminates enables high strength, increased deformability, and the ability to absorb and mitigate damage due to varied crystalline defects, including dislocations. Here, we present the enhanced strength of Ti/Nb nanolaminates containing thick 3D interfaces (3DIs), relative to their chemically abrupt 2D counterparts. We examine the effects of crystallographic alignment and compositional gradients on mechanical behavior via experiments and phase-field-dislocation dynamics (PFDD) modeling. Mechanical testing reveals that nanolaminates containing thicker 3DIs demonstrate a 28% hardness enhancement compared with sharp-interface nanolaminates. PFDD modeling shows that the critical resolved shear stress (CRSS) increases with the 3DI thickness. Gradual compositional transitions in 3DIs were confirmed via scanning transmission electron microscopy and high-resolution transmission electron microscopy, showing sharp crystallographic transitions and a heightened interface topography. The findings establish a positive function between the 3DI thickness and mechanical robustness for hexagonal-closest-packed-containing composites, emphasizing the role of defect–interface interactions in tailoring the mechanical performance and providing a foundation for future interfacial engineering.

36 MATERIALS SCIENCE↗

X-ray Micro-Computed Tomography for Structural Analysis of All-Solid-State Battery at Pouch Cell Level

Characterizing the microstructure of all-solid-state batteries (ASSBs) during fabrication and operation is vital for their advancement, particularly as scaling to pouch cell levels introduces challenges in probing large-scale microstructural evolution. This work highlights the potential of synchrotron X-ray micro-computed tomography (sXCT) as a nondestructive, rapid (<30 min), and high-resolution technique for visualizing and quantifying key microstructural features, including overhang, porosity, contact loss, active surface area, and tortuosity, in all-solid-state pouch cells. The large field of view (up to millimeters) of sXCT enables detailed analysis at an industry-relevant scale, bridging the gap between laboratory research and commercial applications. Furthermore, integrating realistic sXCT-derived 3D models into multiphysics simulations could provide insights into chemo-mechanical degradation, particularly at the edges of the pouch cells, offering a pathway for designing robust, high-performance ASSBs. This perspective establishes sXCT as an indispensable tool for advancing both the understanding and the engineering of next-generation energy storage systems.

25 ENERGY STORAGE↗

Preliminary hyperspectral neutron radiography of binder jet 3D printed and melt infiltrated Si–SiC

The preliminary results of hyperspectral neutron radiography of Si–SiC made with binder jet additive manufacturing, subsequent carbon addition, and silicon melt infiltration are presented. The samples were measured in the processing states before and after the melt infiltration to determine if neutrons would help characterize the microstructure to better understand the melt infiltration process. Theoretical Bragg edges were calculated for comparison with the radiographic results. The changes in the Bragg edges from pre- to post-infiltrated reaction-bonded SiC were evident, that could be used to address the differences in microstructures. In conclusion, the preliminary results presented in this study demonstrated that neutron Bragg-edge imaging is possible with Si–SiC reaction-bonded ceramics and can help determine the microstructure of melt infiltrated samples.

SiC↗

Direct selective laser sintering of hexagonal barium titanate ceramics

Abstract A direct selective laser sintering (SLS) process was combined with a laser preheating procedure to decrease the temperature gradient and thermal stress, which was demonstrated as a promising approach for additive manufacturing of BaTiO 3 ceramics. The phase compositions in BaTiO 3 ceramics fabricated by SLS were investigated by X‐ray and neutron diffractions. The surface morphologies and cross‐section microstructures were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). A dense hexagonal h‐BaTiO 3 layer was formed on the surface and extended to a depth of 500 μm, with a relative density higher than 97% and absence of pores or microcracks. SLS resulted in the formation of the high‐temperature phase, h‐BaTiO 3 , which was retained at room temperature possibly due to the high cooling rate. The grain boundaries of SLSed h‐BaTiO 3 ceramics consist of a Ti‐rich secondary phase. Compared with that of the pressureless sintered t‐BaTiO 3 ceramics, the Vickers hardness of SLSed h‐BaTiO 3 is 70% higher.

Zhang, Xiang↗

Additive Manufacturing of Lattice Structures for Catalyst Applications

Abstract The design and fabrication of Inconel 718 open-pore lattice structures via Laser Powder Bed Fusion (LPBF) has been investigated in this research, focusing on applications such as catalyst supports in jet fuel production. The study explores the impact of laser power and scanning speed on the geometrical resolution of these structures aiming to achieve high porosity (porosity > 60%) and specific pore sizes ranging from 500–1000 μm, intending to serve as catalyst supports, replacing conventionally manufactured foams to reduce costs. Results demonstrate the significant influence of processing parameters on the geometrical aspects of printed lattice structures, with laser power having a more pronounced effect on geometrical accuracy than scanning speed. Additionally, the mechanical properties of the printed lattice structures showed a correlation with the lattice strut sizes, as lattices with less porosity and thicker struts resulted in higher maximum shear stress.

36 MATERIALS SCIENCE↗

Direct Measurements of Ionic Transport Behavior of Dual-Layer Porous Electrodes

To improve power and cycling performance of lithium-ion batteries, dual-layer or porosity-gradient electrodes have been proposed. By engineering a higher porosity close to the separator, the intention is to improve ion transport where it is most impactful. In this research, MacMullin numbers of two dual-layer anode samples are tested using an impedance measurement technique developed previously. To characterize the microstructure of each layer independently, we developed an improved transmission-line model that accounts for each layer's properties.Virtual experiments using COMSOL Multiphysics to simulate impedance measurements are used to examine and improve the accuracy of the numerical inversion procedure. The results for the two dual-layer anodes studied show that MacMullin numbers follow expected trends, though the anodes are quite different from each other.

Dual-Layer Electrodes↗

On the regeneration of fish scales: structure and mechanical behavior

Fish scales serve as a dermal armor that provides protection from physical injury. Owing to a number of outstanding properties, fish scales are inspiring new concepts for layered engineered materials and next-generation flexible armors. Although past efforts have primarily focused on the structure and mechanical behavior of ontogenetic scales, the structure–property relationships of regenerated scales have received limited attention. In the present study, common carp ( Cyprinus carpio ) acquired from the wild were held live in an aquatic laboratory at 10°C and 20°C. Ontogenetic scales were extracted from the fish for analysis, as well as regenerated scales after approximately 1 year of development and growth. Their microstructure was characterized using microscopy and Raman spectroscopy, and the mechanical properties were evaluated in uniaxial tension to failure under hydrated conditions. We note the strength, strain to fracture and toughness of the regenerated scales were significantly lower than those of ontogenetic scales from the same fish, regardless of the water temperature. Scales that regenerated at 20°C exhibited significantly higher strength, strain to fracture and toughness than those regenerated at 10°C. The regenerated scales exhibited a highly mineralized outer layer, but no distinct limiting layer or external elasmodine; they also possessed a significantly lower number of plies in the basal layer than the ontogenetic scales. The results suggest that a mineralized layer develops preferentially during scale regeneration with the topology needed for protection, prior to the development of other qualities.

59 BASIC BIOLOGICAL SCIENCES↗

Solid Phase Gradient Alloying Method via ShAPE

Alloying has been used to confer desirable properties to various metallic systems since the bronze age. For example, Ni, Mn, and Cr are alloyed into an Fe matrix to make steel, which has improved strength and corrosion resistance (as displayed in Fig. 1). In addition to the type of alloying elements, the amount of alloying elements added into a matrix is also very critical for a material’s mechanical property, physical property, machinability, and cost. Conventionally, new alloys are discovered by combining alloy precursors and elemental constituents into a mixture and melting them together. The solidified product or ingot represents a usually non-homogeneous combination of the chemistry with a microstructure dictated by the physics of solidification. It is time and energy intensive to optimize the alloying amounts via the casting process and hence, economically not conducive to rapid alloy discovery. In addition, the cast microstructure seen in the as-cast ingot is often not the ideal, nor even desired structure for optimized performance. Cast materials often need further processing such as homogenization, annealing, and deformation work put in through rolling, forging, extruding, etc. to have favorable microstructures and properties. A faster method to discover new alloy combinations and evaluate them in their worked or processed form is needed. Recently, Laser Engineered Net Shaping was applied to fabricate gradient compositional material for alloy designing. However, the mechanical properties of this gradient alloy were poor due to the existence of impurities, oxidation and cracks that are inherent in the melt-solidification process. Because of these limitations, we propose to use a solid-phase process (ShAPE) to create bulk materials (extrudates) that vary in composition from one end of the extruded solid to the other. Various manufacturing methods for alloy design including conventional casting method, laser based combinatorial method and current solid phase gradient alloying method are displayed and compared in Fig. 2. ShAPE machine and a schematic of ShAPE process are displayed in Fig. 3. Starting material is processed by a rotating and plunging die to form an extrudate. We are proposing through this methodology to invent a new, bulk-scale combinatorial technique. With this novel technique, alloying element can be dissolved into the matrix with a continued gradient without bulk melting. Formation of inter-metallics and defects originating from melt processing can be avoided. In addition, the ShAPE process creates the mixed alloy chemistry, and meanwhile subjects the material to severe plastic strain, which induces the favorable “worked” microstructure. Products from the ShAPE process can be tested in hardness directly providing a path to rapid evaluation of mechanical properties. The ability to create graded structures using friction stir processing (FSP) has been demonstrated, however using the ShAPE process we believe will lead to much faster and higher fidelity results. When combined with high throughput screening methods of physical, mechanical and microstructural property characterization, efficiency and accuracy of alloy design can be significantly improved.

36 MATERIALS SCIENCE↗

Reconstruction of 3D Concrete Microstructures Combining High-Resolution Characterization and Convolutional Neural Network for Image Segmentation

After water, concrete is the second most used material in the world. Concrete’s forming adaptability and low-cost constituents make it a predominant material used in the construction of civil infrastructures in nuclear power plants such as concrete biological shields, containment buildings, turbine buildings, fuel handling and storage buildings, underground piping for cooling, cooling towers, and so on. Depending on environmental and operating conditions, these passive structures are subject to time-dependent phenomena that can either enhance (e.g., continued hydration) or degrade concrete’s structural performance. Unlike components such as the reactor pressure vessel and the primary circuit, concrete composition varies regionally because it is manufactured using local aggregates and cement. Hence, concrete performance metrics over time cannot be derived confidently using empirical relations. Alternatively, the specific characteristics of the local concrete constituents and their assemblage in concrete must be considered.

36 MATERIALS SCIENCE↗

Manufacturing of Fabric Electrodes using a High-Throughput Screening Platform for Redox Flow Batteries

The objective of this project is to establish a new manufacturing methodology with machine learning- based high-throughput screening for the design and development of hierarchical structured, high-performance fabric electrodes for redox flow batteries (RFBs). The end goal of the project is to design and manufacture fabric electrodes for RFB applications that can provide 250 mA/cm2 current density operation for 100-cycles with 80% average energy efficiency. This was accomplished by first examining the structure-performance-property linkages of the electrodes provided by our partner, AvCarb. The electrodes’ microstructure was characterized by determining their pore size distribution, tortuosity, specific surface area, and porosity. The ohmic, charge transfer and mass transfer resistances were then calculated using electrochemical impedance spectroscopy. Carbon cloth electrodes showed the greatest resistance, which was dominated by charge transfer resistance, which we believe is related to the surface functionalization. Full cell cycling was used in order to determine the area specific resistance and energy efficiency of the cells. All of this experimental data and the results of the mathematical model (to increase the amount of inputs with parametric sweeping) were used to develop a machine learning-based model for the design of high-performance fabric electrodes. Using the results from the machine learning tool, optimized electrodes were fabricated by AvCarb. The ohmic, charge transfer and mass transfer resistances for these new electrodes were measured, and both performed better than any of the initial samples which had been provided by AvCarb.

25 ENERGY STORAGE↗

FY24 Progress Report: Disposition of Cracks & Features Observed in the Inner Can Closure Weld Region (ICCWR) of the 3013 Package

The long-term integrity of the 3013 containers is of interest for the safe storage of Pu materials. Although the 3013 standard embodies multiple barrier concept, the integrity of the inner container is considered to be crucial since it protects the Safety Class outer container from its contents. The container is designed to withstand high pressures that could result from the complete radiolysis of the maximum water content permissible by the 3013 standard. Shelf-life studies and destructive examination have not found high gas pressures but have found that corrosive gases are generated. Pitting and stress corrosion cracking (SCC) are considered to be critical corrosion modes for the performance of the inner container and have been observed during destructive examinations. Considerable research has been conducted on the possibility of aqueous electrolytes condensing on the inner container that can promote SCC. These studies indicate the uncertainties surrounding the formation of corrosive environments and the corrosion behavior of container materials. In this initial report, a Bayesian network (BN) model is described that can consider the uncertainties and the causal connections between various factors influencing the corrosion modes of the inner container. The BN model is preliminary and provides an initial framework to identify the necessary information. The report also provides initial experimental results on the electrochemical behavior of stainless steels in anticipated condensed environments from gas phase migration of acidic gases. The experimental results are consistent with the corrosion model. Recommendation for further work on the BN model include assembling an expert group to provide input to the BN structure and quantification of the conditional probability matrix, experimental studies to characterize the microstructure of the container, electrochemical studies to identify critical potentials for localized corrosion and SCC, and crack growth rate studies

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

Ni-based superalloy Haynes® 282® is being targeted for various applications in advanced power generation systems for its superior fabricability, weldability, and excellent high temperature creep and corrosion performance. This process optimization study aims to use a low heat-input, high deposition rate, controlled Gas Metal Arc Welding (GMAW) process, Cold Metal Transfer (CMT) by Fronius, attempting to achieve fully dense fabrication and possibly avoid the need for HIP. Twenty-one multilayer blocks (~25x100x40 mm3) were deposited to explore a large set of build parameters variations that focused on varying the travel speed from 14 to 42 inches per minute (ipm) and wire feed speed from 150 to 450 ipm. A strong correlation has been observed between arc energy – controlled primarily by travel and wire feed speed. Initial visual inspection, internal microstructural examination, and computed tomography (CT) have been used to determine the effects of built parameters on evolution of internal porosity and defects. Scanning electron microscopy techniques enabled structural and compositional imaging of heterogeneity and changes in microstructural properties.

additive manufacturing↗

Characterization of Build Parameters and Microstructure in Low Heat Input WAAM of Ni-Based Superalloy Haynes 282

Ni-based superalloy Haynes® 282® is being targeted for various applications in advanced power generation systems for its superior fabricability, weldability, and excellent high temperature creep and corrosion performance. This process optimization study aims to use a low heat-input, high deposition rate, controlled Gas Metal Arc Welding (GMAW) process, Cold Metal Transfer (CMT) by Fronius, attempting to achieve fully dense fabrication and possibly avoid the need for HIP. Twenty-one multilayer blocks (~25x100x40 mm3) were deposited to explore a large set of build parameters variations that focused on varying the travel speed from 14 to 42 inches per minute (ipm) and wire feed speed from 150 to 450 ipm. A strong correlation has been observed between arc energy – controlled primarily by travel and wire feed speed. Initial visual inspection, internal microstructural examination, and computed tomography (CT) have been used to determine the effects of built parameters on evolution of internal porosity and defects. Scanning electron microscopy techniques enabled structural and compositional imaging of heterogeneity and changes in microstructural properties.

additive manufacturing↗

NSUF RTE completion report for 23-4780: Microstructural Defect Induced Thermal Conductivity Reduction in Uranium Nitride and Thorium Nitride

Uranium nitride (UN) is known to have a higher thermal conductivity than traditional oxide fuels, which could lead to a more efficient energy transport and lower local temperature during its lifetime. But the thermal transport performance of UN in extreme environments has not been systematic studied. This study investigated the irradiation induced microstructural defects in UN and the impacts on thermal conductivity. The samples were produced by spark plasma sintering at University of Texas-San Antonio (UTSA), Los Alamos National Laboratory (LANL), and Idaho National Laboratory (INL). Thermal conductivity of UN before and after 2MeV proton irradiation were measured by using laser metrology at INL in a temperature range of 77-295K. Thermal conductivity measurements in this wide, cryogenic temperature range is critical to understand the phonon scattering mechanisms between the thermal energy carrier, phonons, and different types of irradiation-induced defects. In order to ensure the measurements were conducted in the same grains and minimize the impact of the local heterogeneities, the measurement locations were highlighted by fiducial marks using the focused ion beam (FIB) with grain orientation identified using the electron backscatter diffraction (EBSD) at the Center of Advanced Energy Studies (CAES). Irradiation experiment was conducted at the Ion Beam Laboratory at Texas A&M University (TAMU). A total of 6 samples were irradiated with different irradiation doses and temperatures. After irradiation, the microstructure was characterized by using Transmission Electron Microscope (TEM) at CAES (also in the FIB marks).

36 - MATERIALS SCIENCE↗

Additive Manufacturing of C/C-SiC Ceramic Matrix Composites by Automated Fiber Placement of Continuous Fiber Tow in Polymer with Pyrolysis and Reactive Silicon Melt Infiltration

An additive manufacturing process for fabricating ceramic matrix composites has been developed based on the C/C-SiC system. Automated fiber placement of the continuous carbon fibers in a polyether ether ketone matrix was performed to consolidate the carbon fibers into a printed preform. Pyrolysis was performed to convert the polymer matrix to porous carbon, and then Si was introduced by reactive melt infiltration to convert a portion of the carbon matrix to silicon carbide. The densities and microstructures were characterized after each step during the processing, and the mechanical properties were measured. The C/C-SiC composites exhibited a porosity of 10–20%, characteristic flexural strength of 234.91 MPa, and Weibull modulus of 3.21. The composites displayed toughness via a significant displacement to failure.

36 MATERIALS SCIENCE↗

Tensile Performance Sensitivity to Variations of Standard 17-4 PH Heat Treatments on LPBF-Produced Material

Standard heat treatments for metals of a particular composition are typically designed with the assumption of a conventional starting microstructure, such as that produced by casting or wrought processing. When applied to metals fabricated by Laser Powder Bed Fusion (LPBF) metal additive manufacturing (AM), these heat treatments can produce inconsistent performance due to the unique as-built microstructures. This study investigates how modifications to standard heat treatments for 17-4 PH steel influence the microstructure and mechanical properties of LPBF-fabricated material. Specimens were produced and subjected to varying solutionizing and homogenizing treatments followed by standard aging treatments. Microstructures were characterized using optical microscopy, Electron Backscatter Diffraction (EBSD), and X-ray diffraction (XRD), and mechanical properties were evaluated through uniaxial tensile testing. Based on these results, recommendations are provided for achieving improved wrought-like performance in LPBF 17-4 PH steel.

17-4 PH↗

Combinatorial Cu-Ni Alloy Thin-Film Catalysts for Layer Number Control in Chemical Vapor-Deposited Graphene

We synthesized a combinatorial library of CuxNi1−x alloy thin films via co-sputtering from Cu and Ni targets to catalyze graphene chemical vapor deposition. The alloy morphology, composition, and microstructure were characterized via scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), and X-ray diffraction (XRD), respectively. Subsequently, the CuxNi1−x alloy thin films were used to grow graphene in a CH4-Ar-H2 ambient at atmospheric pressure. The underlying rationale is to adjust the CuxNi1−x composition to control the graphene. Energy dispersive x-ray spectroscopy (EDS) analysis revealed that a continuous gradient of CuxNi1−x (25 at. % < x < 83 at.%) was initially achieved across the 100 mm diameter substrate (~0.9%/mm composition gradient). The XRD spectra confirmed a solid solution was realized and the face-centered cubic lattice parameter varied from ~3.52 to 3.58 A˙, consistent with the measured composition gradient, assuming Vegard’s law. Optical microscopy and Raman analysis of the graphene layers suggest single layer growth occurs with x > 69 at.%, bilayer growth dominates from 48 at.% < x < 69 at.%, and multilayer (≥3) growth occurs for x < 48 at.%, where x is the Cu concentration. Finally, a large area of bi-layer graphene was grown via a CuxNi1−x catalyst with optimized catalyst composition and growth temperature.

2D materials↗

Develop Renewable/Sustainable Material to Displace Petroleum-Derived Polymer Foams (CRADA Final Report)

NLR and EDEN will partner together to develop renewable, biodegradable alternatives to polyfoam (polyurethane) polymer foams. The initial focus will be on developing cellulose-based foam with tunable mechanical properties. NLR will produce and test the cellulose-based foam materials and characterize its microstructure and mechanical properties. Relationships between mechanical performance formulation and fabrication methods will be developed.

09 BIOMASS FUELS↗