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At least 361 records · Page 20

FFT-based model for irradiated aggregate microstructures in concrete

The concrete biological shield of light water reactors is exposed to neutron and gamma irradiation throughout its lifetime, which results in the long-term degradation of the concrete’s mechanical properties. Under neutron irradiation, the concrete’s aggregates are subjected to radiation-induced volumetric expansion (RIVE), which strongly depends on the mineral content of the aggregate and exhibits the largest expansion in silicate-bearing minerals. In this work, the authors used the fast Fourier transform-based code Microstructure-Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) in 2D to model the expansion of five different aggregates provided by the Japan Concrete Aging Management Program (JCAMP). Comparable rock specimens were irradiated at the JEEP-II test reactor. The model uses realistic aggregate microstructure reconstruction based on high-resolution characterization images. The model accounts for anisotropic RIVE, thermal expansion, and the associated initiation and propagation of damage. The RIVE models are calibrated based on expansion data in the literature. The authors assume that damage occurs exclusively at interfaces between the particles that compose an aggregate and that these interfaces also exhibit swelling. Using a micromechanical model, the evolution of Young’s modulus with RIVE is calculated for each aggregate and compared with Russian irradiation data. The modeled linear expansion agrees well with the experimentally measured expansion. Furthermore, the model also predicts that anisotropic RIVE and thermal expansion result in an earlier onset of damage with neutron fluence than in the isotropic case.

36 MATERIALS SCIENCE↗

Heat Conduction in Ceramic Coatings: Relationship Between Microstructure and Effective Thermal Conductivity

Analysis of the effective thermal conductivity of ceramic coatings and its relation to the microstructure continued. Results (obtained in Task 1) for the three-dimensional problem of heat conduction in a solid containing an inclusion (or, in particular, cavity - thermal insulator) of the ellipsoidal shape, were further advanced in the following two directions: (1) closed form expressions of H tensor have been derived for special cases of ellipsoidal cavity geometry: spheroid, crack-like spheroidal cavity and needle shaped spheroidal cavity; (2) these results for one cavity have been incorporated to construct heat energy potential for a solid with many spheroidal cavities (in the approximation of non-interacting defects). This problem constitutes a basic building block for further analyses.

Kachanov, Mark↗

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗

Uranium Oxide Synthetic Pathway Discernment through Unsupervised Morphological Analysis

We present a novel unsupervised machine learning method for quantitative representation of scanning electron micrographs and its applications and performance for nuclear forensic analysis of uranium ore concentrates. The method uses a vector quantizing variational autoencoder followed by a histogram operation to encode a micrograph into a single dimensional representation, called the latent vector. The method requires no extant labeling of the data and can be applied over large datasets of micrographs with minimal human interaction. The representations generated are broadly descriptive of each micrograph and the microstructure of the material imaged. In the case of uranium ore concentrate analysis, the representations were amenable to processing reagent and ore concentrate species classification with accuracy of 81:8%, which is competitive with state-of-the-art supervised networks. The representations were also used to classify previously unseen processing routes, were able to classify imaging parameters such as magnification (to 76:0% accuracy), were able to classify fine grained process parameters such as calcining temperature (to 74:4% accuracy), and their informatic properties indicate that they are generally descriptive of the image represented. This method can be applied across microstructure analysis fields to perform quantitative analysis without the need for labor intensive and possibly biased human analysis.

Scanning Electron Microscopy, Vector Quantizing Va↗

Optimization of direct aging temperature of Ti free grade 300 maraging steel manufactured using laser powder bed fusion (LPBF)

Maraging steels are of interest to the tool and die industry owing to their high strength, toughness and machinability. Additive manufacturing technologies like laser powder bed fusion (LPBF) can result in a paradigm shift in the design of maraging steel tools. Here, the lack of precipitates, in combination with solute segregation and non-equilibrium microstructure in Grade 300 maraging steel fabricated via LPBF makes the steel amenable to strengthening via direct aging post fabrication instead of the conventional solution treatment and aging. In this study we have focused on optimizing the direct aging temperature for a Ti-free Grade 300 maraging steel fabricated via LPBF for two different aging times. Through strain hardening analysis and detailed microstructural characterization, we show that direct aging at a temperature of 440 °C for 6 h resulted in the best strength-ductility combination. Aging samples at a lower temperature or shorter time resulted in no strain hardening prior to necking as a result of lower fraction of reverted austenite, whereas aging samples at a higher temperature resulted in extensive recrystallization of martensite, coarsening of precipitates, and extensive austenite reversion, resulting in softening of the fabricated parts.

36 MATERIALS SCIENCE↗

Thermal analysis of a functionally graded material subject to a thermal gradient using the boundary element method

The boundary element method is utilized in this study to conduct thermal analysis of functionally graded composites, materials in which the internal microstructure or properties are explicitly tailored in order to obtain an optimal response, on the micromechanical (constituent) scale. A unique feature of the boundary element formulations used here is the use of circular shape functions to convert the two-dimensional integrations of the composite fibers to one dimensional integrations. Using the computer code BEST-CMS, the through the thickness temperature profiles are computed for a representative material with varying numbers of fibers and fiber spacing in the thickness direction. The computed temperature profiles are compared to those obtained using an alternate analytical theory which explicitly couples the heterogeneous microstructure to the global analysis. The boundary element results compared favorably to the analytical calculations, with discrepancies that are explainable based on the boundary element formulation. The results serve both to demonstrate the ability of the boundary element method to analyze these types of materials, and to verify the accuracy of the analytical theory.

Goldberg, Robert K.↗

Homogenization of Dendritic Structures and the High-Temperature Strength of the Refractory High-Entropy Alloy MoNbTaVW

MoNbTaVW, a pioneering refractory high-entropy alloy (RHEA), is renowned for its exceptional strength at elevated temperatures. Like most RHEAs, it solidifies into a dendritic microstructure with steep concentration gradients, necessitating heat treatment for equilibration. Steep concentration gradients typically complicate mechanical property analysis and modeling, key challenges for high-throughput alloy discovery. This study examines the effects of high-temperature homogenization (1800 °C for 8 hours) on the microstructure and mechanical properties of MoNbTaVW across temperatures up to 1200 °C. Postmortem microstructural analysis, coupled with chemical, crystallographic, and mechanical assessments, revealed that yield strength was surprisingly insensitive to homogenization, with less than a 3 pct difference between as-cast and heat-treated materials. Nanoindentation confirmed minimal nanohardness changes across the dendritic structure at room temperature. However, homogenization significantly enhanced high-temperature work hardening, producing higher peak compressive strength. Both as-cast and homogenized MoNbTaVW exhibited room-temperature strengths of 1400 MPa, exceeding previously reported values. These findings demonstrate that high-temperature treatment enables microstructural homogenization without compromising strength, a unique behavior among RHEAs. In conclusion, while not universally applicable, this insight highlights the importance of understanding microstructural development in experimental alloys and offers a pathway to design alloys that achieve homogeneous-like properties without heat treatment.

Rietema, C. J. [Lawrence Livermore National Labora↗

Physical and chemical analysis of a Ni/H2 cell

A cycled aerospace nickel hydrogen (Ni/H2) cell was subjected to destructive physical analysis to determine the reason for a capacity loss after 5,967 cycles at 60 percent depth of discharge. The positive plates in the cell were analyzed in terms of chemical composition, active material utilization, charge efficiency, and thickness increase. The microstructure of a cross section of the positive plate was determined by backscattered electron image analysis. The results suggest that the capacity loss in the cell is caused by low charge acceptance and low active material utilization at the positive plate. The oxidized nickel species content of the positive plate increased due to corrosion of the nickel sintered skeleton. This appears to circumvent the orderly reaction of the active material. Microstructural analysis has indicated that a new phase of active material is formed with cycling.

H Vaidyanathan↗

Strain energy-based fatigue failure analyses of LB-PBF Inconel 718: Effect of build orientation

Additively manufactured Inconel 718 parts fabricated in three build orientations (horizontal, vertical, and angled at 45 degrees) are tested in fully-reversed bending fatigue mode. Damping measurements via the Impulse Excitation technique are used to assess the defects content in the microstructure and fractography analysis is performed to detect the root cause of failure. Two micro- and macro-scale methodologies of fatigue damage estimation based on the dissipated heat per cycle and the statistical estimation of micro-plastic strain energies are used to assess fatigue damage. It is shown that at a given stress level, the vertically built specimens endure the most fatigue damage before failure while the diagonally built ones sustain the least. As a result, the fatigue life is estimated for arbitrary load amplitudes via a microstructure-sensitive algorithm with acceptable accuracy as compared to the experiments.

36 MATERIALS SCIENCE↗

Characterization of build parameters and microstructure in low heat input WAAM of Ni-based superalloy Haynes 282

Conference paper for 2024 10th International Conference on Advances in Materials, Manufacturing & Repair for Power Plants. Ni-based superalloy Haynes 282 is a prime candidate for advanced power generation systems due to its superior fabricability, weldability, and high-temperature performance. Additive manufacturing offers potential cost and time savings for gas turbine components. Wire-arc direct energy deposition can create large components but often requires post-processing treatments, such as hot isostatic pressing (HIP), to address porosity. This study explores a low heat-input, high deposition rate GMAW process to achieve fully dense Haynes 282 without HIP. Twenty-one blocks were deposited, varying travel and wire feed speeds. Initial analysis (visual inspection, microstructural examination, and CT) revealed the impact of build parameters on internal porosity and defects. Scanning electron microscopy provided insights into structural heterogeneity and microstructural properties. Related journal article can be found at https://doi.org/10.31399/asm.cp.am-epri-2024p0001.

Adam, Benjamin↗

Reversible Binding Interfaces Made of Microstructured Polymer Brushes

The polymer brush architecture of the end-tethered polymer molecules is one of the most widely used efficient methods to regulate interfacial interactions in colloidal systems found in live matter and manufactured materials. Emerging applications of polymer brush structures require solutions to new tasks in the control of interfacial interactions. The rapid development of live cell manufacturing relies on scalable and efficient cell harvesting methods. Stimuli-responsive surfaces made of surface-grafted poly(N-isopropylacrylamide) (PNIPAM) can bind and detach the adherent cell upon changes in temperature and have been used for cell growth and harvesting. The applications are limited by the requirement to satisfy a range of PNIPAM coating characteristics that depend on the dimensions of the integrin complex in the cell membrane and the basal surface. The analysis of the microstructured surfaces, when adhesive and disjoining functions of the microdomains are decoupled, shows that many limitations of PNIPAM one-component coatings can be avoided by using a much broader range of structural characteristics of the microstructured interfaces composed of alternating disjoining PNIPAM domains and adhesive polymeric domains with cell-affinity functional groups. Temperature-controlled reversible adhesion to such microstructured interfaces is studied here experimentally with model systems of solid spherical particles and by employing simulations for solid and soft membranes interacting with the microstructured surfaces to mimic interactions with soft and solid disk-like particles.

36 MATERIALS SCIENCE↗

Microstructure prediction for Ti-22Al-25Nb in laser powder bed fusion

This work presents a physics-informed framework for predicting solidification morphology and defect susceptibility in additively manufactured Ti–22Al–25Nb across a broad processing space. The framework integrates solidification microstructure selection (SMS) analysis with a single-track defect-based printability map to establish a unified methodology linking processing parameters to both interfacial morphology and manufacturability. Thermal gradients G and solidification rates R are first computed using the Thermo-Calc Additive Manufacturing (TC-AM) module, a finite-interface-dissipation (FID) phase-field (PF) model coupled with CALPHAD method is then employed to systematically distinguish planar and dendritic regimes as functions of $G$ and $R$. By superimposing the printability map onto the morphology projections, a comprehensive process–structure framework is obtained. Across most processing conditions, the predicted microstructure is predominantly dendritic, while planar growth emerges only under selected laser power $P$ and scan speed $v$ combinations. In addition to morphology classification, the framework quantifies the dendritic area fraction and introduces a width-based morphology descriptor to characterize the spatial extent of planar/dendritic regions within the melt pool. It provides mechanistic insight into the interplay between solidification physics and defect formation, offering practical guidance for parameter selection and microstructural control in Ti–22Al–25Nb additive manufacturing (AM).

36 MATERIALS SCIENCE↗

Deep learning-based segmentation of lithium-ion battery microstructures enhanced by artificially generated electrodes

Accurate 3D representations of lithium-ion battery electrodes, in which the active particles, binder and pore phases are distinguished and labeled, can assist in understanding and ultimately improving battery performance. Here, we demonstrate a methodology for using deep-learning tools to achieve reliable segmentations of volumetric images of electrodes on which standard segmentation approaches fail due to insufficient contrast. We implement the 3D U-Net architecture for segmentation, and, to overcome the limitations of training data obtained experimentally through imaging, we show how synthetic learning data, consisting of realistic artificial electrode structures and their tomographic reconstructions, can be generated and used to enhance network performance. We apply our method to segment x-ray tomographic microscopy images of graphite-silicon composite electrodes and show it is accurate across standard metrics. We then apply it to obtain a statistically meaningful analysis of the microstructural evolution of the carbon-black and binder domain during battery operation.

25 ENERGY STORAGE↗

Analysis of Deformation and Fracture Mechanisms in the Harvested Low-Dose Baffle Former Bolt via Advanced Mechanical Tests

This report details the production of tensile specimens from in-service irradiated baffle former bolts (BFBs) and presents the results of a pilot in-situ SEM/EBSD test conducted at Oak Ridge National Laboratory’s Low Activation Materials Development and Analysis (LAMDA) facility. The SEM/EDS results confirmed that the material is AISI 316L steel, not AISI 347, and that no Nb addition was detected in several analyzed locations. EBSD analysis of the microstructure revealed in-grain misorientation gradients indicative of cold work, likely caused by material processing, and no retained ferrite was identified. During straining, dislocation channel formation was the primary deformation mechanism, with twinning also observed in favorably oriented grains at local strains as small as ~1.5%. No strain-induced phase instability was observed, likely due to the fact that the Ni and Cr content reached the upper limits for the 316L steel specification. Multiple microfracture events were observed during the tensile test. Fine strain-induced pores formed at the channel-grain boundary intersection points, while coarser microcracks were associated with non-metallic inclusions. Data analysis is ongoing, and additional tests are planned in the near future to provide more statistics and details.

36 MATERIALS SCIENCE↗

Outgassing of implanted He via short circuit transport along phase and grain boundaries in vapor co-deposited Cu-W nanocomposites

We investigate the response of physical vapor co-deposited copper (Cu)-tungsten (W) nanocomposites to helium (He) implantation. Nuclear reaction analysis (NRA) reveals that a substantial fraction of He implanted into these materials escapes during implantation. Analysis of nanocomposite microstructure shows that the He loss is likely due to its transport out of the material by diffusion along phase and grain boundaries. Lastly, our findings suggest that solid-state interfaces such as phase and grain boundaries are short circuit diffusion pathways for transport of He.

36 MATERIALS SCIENCE↗

Application of Image Analysis for Characterization of Spatial Arrangements of Features in Microstructure

A number of microstructural processes are sensitive to the spatial arrangements of features in microstructure. However, very little attention has been given in the past to the experimental measurements of the descriptors of microstructural distance distributions due to the lack of practically feasible methods. We present a digital image analysis procedure to estimate the micro-structural distance distributions. The application of the technique is demonstrated via estimation of K function, radial distribution function, and nearest-neighbor distribution function of hollow spherical carbon particulates in a polymer matrix composite, observed in a metallographic section.

Louis, Pascal↗

Stimuli‐Responsive Emission from Hybrid Metal Halides

Abstract Stimuli‐responsive photoluminescent (PL) materials have attracted considerable attention in recent years owing to their potential applications in anti‐counterfeiting, information encryption, and sensing. Further investigations of the transformation mechanism and potential applications of stimulus‐responsive PL materials are considerably important. In the current study, an organic–inorganic metal halide, C 9 H 15 N 3 SbCl 5 ([C 9 H 13 N 3 ] 2+ is a 1‐(2‐pyridyl) piperazine cation) is obtained, which exhibits a 0D structure withP‐1 space group. At room temperature, when excited by UV light, the C 9 H 15 N 3 SbCl 5 single crystals exhibit unimodal blue light emission at 405 nm, and grinding or hydrostatic pressure induces double‐peak emissions at 405 and 650 nm. Interestingly, double‐emission samples can be restored to single‐emission samples by short annealing or storage in air for 2 weeks, and this process is reversible. Luminescence response to mechanical stimuli can also be achieved in the presence of hydrochloric acid and water. Spectral analysis and the analysis of the microstructural changes revealed that the structural modifications of the inorganic group play a pivotal role in the response to the stimulus. Finally, a composite film device based on C 9 H 15 N 3 SbCl 5 is prepared to demonstrate the potential of these smart materials in anti‐counterfeiting and sensing applications.

Chemistry↗

Relationship between Grain Size and Sample Thickness on the Creep-Rupture Performance of Thin Metallic Sheets of INCONEL Alloy 740H

A study was conducted on INCONEL® alloy 740H® to examine the role of grain size and sheet thickness on the alloy’s creep-rupture behavior. Three different starting sheet thicknesses were utilized and multiple heat-treatment conditions anticipated for compact heat exchanger (CHX) manufacturing were applied to produce a range of grain sizes. Creep-rupture testing was conducted at 750 °C for times up to about 6000 h and the results were compared to wrought databases. The data show that both creep strength and ductility were important factors in the overall creep performance of the sheets. Reductions in performance were observed due either to accelerated creep when grain size was fine or loss of rupture ductility when grain sizes approached the sheet thickness. Some combinations of heat-treatment and thickness were able to produce typical expected wrought creep properties. Historically a ‘rule-of-thumb’ requirement for creep testing suggests 3-5 grains per sample minimum dimension to ensure homogeneous behavior. This research shows that to ensure representative wrought creep performance (i.e. no effect of sample size), the sample minimum cross-section should be 10 times the average ASTM grain size. Statistical analysis of the microstructures suggests the population of larger grains as a controlling feature in creep failure.

14 SOLAR ENERGY↗