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At least 865 records · Page 48

Microstructure of calcite deformed by high-pressure torsion: An X-ray line profile study

Calcite aggregates were deformed to high strain using high-pressure torsion and applying confining pressures of 1–6 GPa and temperatures between room temperature and 450 °C. The run products were characterized by X-ray diffraction, and key microstructural parameters were extracted employing X-ray line profile analysis. The dominant slip system was determined as r {$ 10\bar{1}4 $}⟨$ \bar{2}021 $⟩ with edge dislocation character. The resulting dislocation density and the size of the coherently scattering domains (CSD) exhibit a systematic dependence on the P-T conditions of deformation. While high pressure generally impedes recovery through reducing point defect mobility, the picture is complicated by pressure-induced phase transformations in the CaCO 3 system. Transition from the calcite stability field to those of the high-pressure polymorphs CaCO 3 - II, CaCO 3 - III and CaCO3-IIIb leads to a change of the microstructural evolution with deformation. At 450 °C and pressures within the calcite stability field, dislocation densities and CSD sizes saturate at shear strains exceeding 10 in agreement with earlier studies at lower pressures. In the stability field of CaCO 3 - II, the dislocation density reflects a more complex behavior. Furthermore, at a given strain and strain rate, the dislocation density increases and the CSD size decreases with increasing pressure within the stability fields of either calcite or of the high-pressure polymorphs. There is, in contrast, a jump from high dislocation densities and small CSDs in the upper pressure region of the calcite stability field to lower dislocation densities and larger CSDs in the low-pressure region of the CaCO 3 - II stability field. This jump is more pronounced at higher temperatures and less so at room temperature. The pressure influence on the deformation-induced evolution of dislocation densities implies that pressure variations may change the rheology of carbonate rocks. In particular, a weakening is expected to occur at the transition from the calcite to the CaCO 3 - II stability field, if aragonite does not form.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reconstructing parent microstructures in martensitic and pearlitic Ti-Cu

Evaluating the microstructural evolution of parent phases has long been a challenge in metals with a partial or complete solid state transformation. Most parent microstructure evolution has to be inferred from the product microstructure, with some information permanently lost. Parent microstructure reconstructions relying on orientation relationships and EBSD data are a useful tool to overcome this challenge, though much background knowledge is required to do so. Here, this work introduces a reconstruction process for a eutectoid composition Ti-Cu binary alloy to evaluate the high temperature β-Ti phase from martensitic and pearlitic product microstructures. Martensitic microstructures were accurately reconstructed, enabling elucidation of β-Ti grain size and texture, and the employed script included for scientific reference. Pearlitic microstructures did not reconstruct effectively with the current process. However, new insight into the interfacial crystallographic orientations of pearlitic Ti-Cu microstructures was gleaned via this analysis, and future investigations of interest are discussed accordingly. Ultimately, these findings demonstrate tools widely implemented on conventional titanium and ferrous alloys can also be applied to understand parent microstructures in Ti-Cu and other alloys of emerging interest. This is especially of use as new manufacturing processes for such materials require understanding how parent phase microstructures respond to new, novel material processing such as AM.

36 MATERIALS SCIENCE↗

Liquid immiscibility and core-shell morphology formation in ternary Al–Bi–Sn alloys

The effects of composition on liquid immiscibility, macroscopic morphology, microstructure and phase transformation in ternary Al–Bi–Sn alloys were investigated. Three types of morphology, the core-shell type, the stochastic droplet type and uniform dispersion type, of Al–Bi–Sn particles prepared by a jet breakup process were distinguished, and the relationships between which were discussed. The phase transformation behaviors of the Al–Bi–Sn alloys were studied by thermal analysis, in agreement with the microstructural observation and microanalysis. The liquid immiscibility and formation of the core-shell morphology in Al–Bi–Sn alloys are easily achieved when the composition lies in the liquid miscibility gap. The particles exhibit a high melting point Al-rich core with a low melting point Sn–Bi-rich solder shell, showing promise for application as high-density electronic packaging materials. - Highlights: • The liquid demixing, morphology and microstructure in Al–Bi–Sn alloys were studied. • Three types of morphology were classified and discussed. • The conditions for formation of the core-shell morphology were obtained. • The phase transition behaviors agree with the microstructure characterization. • The Al/Sn–Bi core-shell particles show promise for use in electronic packaging.

36 MATERIALS SCIENCE↗

Structural, microstructural and thermal properties of lead-free bismuth–sodium–barium–titanate piezoceramics synthesized by mechanical alloying

Graphical abstract: Mechano-synthesis of lead-free (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} piezoceramics with nanocrystalline/amorphous structure and homogeneous composition: partial transformation of constituents to BNBT, BNT and pyrochlore, amorphous phase formation, mechano-crystallization of the amorphous, pyrochlore-to-perovskite BNBT phase transformation during the process. Display Omitted Highlights: ► Perovskite BNBT powders with homogeneous composition were synthesized by MA. ► Partial transformation of constituents to BNBT, BNT and pyrochlore occurred by MA. ► Formation of an amorphous phase and afterwards its crystallization occurred by MA. ► Pyrochlore-to-perovskite BNBT phase transformation occurred after prolong milling. ► Polymorphic transformations of TiO{sub 2} act as the main alloying impediment during MA. -- Abstract: Bismuth–sodium–barium–titanate piezoceramics with a composition of (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} (BNBT) were prepared by mechanical alloying (MA). Structural analysis and phase identification were performed by X-ray diffraction (XRD). Microstructural studies and chemical composition homogeneity were performed by scanning electron microscope (SEM) coupled with energy dispersive X-ray analysis (EDX). Furthermore, thermal properties of the as-milled powders were evaluated by thermogravimetry/differential thermal analysis (TG/DTA). During the initial milling, the constituents were transformed to the perovskite, pyrochlore, and BNT phases; in addition, partial amorphization of the structure appeared during the milling cycle. As MA progressed, transformation of pyrochlore-to-perovskite and crystallization of the amorphous phase occurred and also, the BNBT phase was significantly developed. It was found that the MA process has the ability to synthesize the BNBT powders with a submicron particle size, regular morphology, and uniform elemental distribution.

36 MATERIALS SCIENCE↗

Yttrium enrichment and improved magnetic properties in partially melted Y-Ba-Cu-O materials

The yttrium-rich compositions in the Y-Ba-Cu-O system were mapped out in a systematic manner to quantify their magnetic properties and to correlate them with the microstructure and phase composition as determined by scanning electron microscopy and X-ray diffraction analysis. It is found that the microstructure of Y-Ba-Cu-O compositions is a sensitive function of both their composition and processing conditions. Measurements of magnetic susceptibility and maximum (low-field) and remanent magnetization for the system Y:Ba:Cu = x:2:3 show highest values for x = 2. The corresponding structures involve numerous small crystals of Y2BaCuO5 (211) embedded in highly ordered assemblages of continous YBa2Cu3O(7-y) (123) layers.

Alterescu, Sidney↗

Stress Distribution During Deformation of Polycrystalline Aluminum by Molecular-Dynamics and Finite-Element Modeling

In this paper, a multiscale modelling strategy is used to study the effect of grain-boundary sliding on stress localization in a polycrystalline microstructure with an uneven distribution of grain size. The development of the molecular dynamics (MD) analysis used to interrogate idealized grain microstructures with various types of grain boundaries and the multiscale modelling strategies for modelling large systems of grains is discussed. Both molecular-dynamics and finite-element (FE) simulations for idealized polycrystalline models of identical geometry are presented with the purpose of demonstrating the effectiveness of the adapted finite-element method using cohesive zone models to reproduce grain-boundary sliding and its effect on the stress distribution in a polycrystalline metal. The yield properties of the grain-boundary interface, used in the FE simulations, are extracted from a MD simulation on a bicrystal. The models allow for the study of the load transfer between adjacent grains of very different size through grain-boundary sliding during deformation. A large-scale FE simulation of 100 grains of a typical microstructure is then presented to reveal that the stress distribution due to grain-boundary sliding during uniform tensile strain can lead to stress localization of two to three times the background stress, thus suggesting a significant effect on the failure properties of the metal.

Yamakov, V.↗

Quantitative assessment of particle dispersion in polymeric composites and its effect on mechanical properties

In this work, an automated image analysis tool is developed to establish quantitative correlations between the particle/cluster size distribution and the mechanical properties of particle reinforced polymer composites (PRPC).This automated image analysis tool is developed within python programming software to process and analyze the microstructural images of the polymerbased composite materials. The spent coffee bean powder (SCBP) reinforced poly-propylene carbonate (PPC) polymer composite with differing wt.% of the filler is selected for the analysis. Detailed statistical analysis of the microstructural images reveals that ‘clustering of clusters’ is also presented in addition to the most commonly reported ‘clustering of particles’, and the distribution of particle/clusters is bimodal. Based on these findings, an effective volume fraction for the filler material is proposed to mainly capture the agglomeration effect. With this effective volume fraction, the standard rule-of-mixture model correctly captures the experimentally measured tensile strength and modulus as a function of filler wt.%. Further, the applicability of this effective volume fraction for other theoretical models is also analyzed. The detailed statistical analysis of the microstructure and the proposed effective volume fraction helps to develop a deeper quantitative understanding of the PRPC than the conventional qualitative correlation of microstructural features with the properties and failure processes.

36 MATERIALS SCIENCE↗

Microstructural Characterization of Felsite Fragments From the Apollo Next Generation Sample Analysis (ANGSA) Double Drive Tube 73001/73002

While the Moon’s surface is dominated by mafic igneous products formed through the crystallization of the lunar magma ocean, and the subsequent eruption of mare basalts – felsic magmatic fragments (variably referred to as felsites, granites, rhyolites or granophyres) have been identified from a number of Apollo samples (e.g. 12013[1], 14321[2], 15405[3] and 73215[4]). Magmatic edifices like the Gruithuisen Domes – silicic constructs sometimes found proximal to the basaltic mare provinces filling nearside basins, may represent a petrogenetic origin. However, this is, is complicated by the fact that they apparently predate mare volcanism (e.g. [5]). Additionally, crater-counting indicates that these silicic surface features also postdate radiogenic ages of Apollo felsites [6]. Various modes of felsic magmatism have been invoked to explain the presence of felsic lithologies on the Moon, including: 1) fractional crystallization and silicate liquid immiscibility; 2) partial melting of lunar crust through basaltic underplating; and 3) fractional crystallization of the mare parent magmas. Although these models are plausible, based on known Apollo samples and lunar meteorites, they are complicated by the lack of sample lithologies with intermediate composition between basaltic magmas and the felsic components, and the fact that partial melting of many crustal rock types on the Moon (e.g., anorthosite, troctolites) are unlikely to form granites. Along with other unique magmatic lithologies, new felsites have been identified within the < 1 mm size fractions of the ANGSA double drive core tube (73001/73002) from Apollo 17 station 3, sampling the light mantle landslide deposit from the South Massif [7]. These additional examples of lunar felsite will help us to better constrain the processes that lead to the formation of these evolved lithologies. To do this, we have employed a gambit of high-resolution scanning electron microscopy (SEM) and scanning transmission electron microscopy (TEM) analytical techniques, including electron backscatter diffraction (EBSD), cathodoluminescence and high-angle annular dark field (HAADF) imaging. These data provide unique insights into the felsite mineralogy and microstructures including the coexistence of quartz and tridymite in many of the fragments. In addition, these analyses provide petrological context and assist targeted in situ secondary ion mass spectrometry (SIMS) measurements of the U-Pb systematics of accessory minerals, and the volatile abundances and D/H ratios of apatite grains identified within the clasts.

lunar↗

Characterization of High Temperature Mechanical Properties Using Laser Ultrasound

Mechanical properties are controlled to a large degree by defect structures such as dislocations and grain boundaries. These microstructural features involve a perturbation of the perfect crystal lattice (i.e. strain fields). Viewed in this context, high frequency strain waves (i.e. ultrasound) provide a natural choice to study microstructure mediated mechanical properties. In this presentation we use laser ultrasound to probe mechanical properties of materials. This approach utilizes lasers to excite and detect ultrasonic waves, and as a consequence has unique advantages over other methods—it is noncontacting, requires no couplant or invasive sample preparation (other than that used in metallurgical analysis), and has the demonstrated capability to probe microstructure on a micron scale. Laser techniques are highly reproducible enabling sophisticated, microstructurally informed data analysis. Since light is being used for generation and detection of the ultrasonic wave, the specimen being examined is not mechanically coupled to the transducer. As a result, laser ultrasound can be carried out remotely, an especially attractive characteristic for in situ measurements in severe environments. Several examples involving laser ultrasound to measure mechanical properties in high temperature environments will be presented. Emphasis will be place on understanding the role of grain microstructure.

36 MATERIALS SCIENCE↗

Multiscale mechanical behavior and microstructure evolution of extruded magnesium alloy sheets: Experimental and crystal plasticity analysis

Highlights: • Experimental stress-strain responses were reproduced by CPFE simulation based on Voronoi grains on three strain paths. • Textures predicted by simulation were in accordance with the ones measured by EBSD at the strain of 0.085. • Deformation heterogeneity in slip-dominated cases was found more significant than that in twin-favored case. • For slip-dominated cases, both high m′ value and high SFs in adjacent grains are responsible for strain localization. - Abstract: A phenomenological crystal plasticity finite element (CPFE) model based on Voronoi grains was applied to reproduce basic deformation features of a hot-extruded magnesium alloy sheet under various strain paths. Corresponding experimental investigations, including mechanical tests, electron back scattered diffraction (EBSD) measurements and optical observation, were also carried out as either a validation or a supplement of the numerical results. Predicted average stress-strain responses and texture evolution are in good accordance with measured ones. Furthermore, deformation heterogeneity at the mesoscopic and intergranular scale were investigated based on the proposed model. At the mesoscale, the heterogeneity in the slip-dominated cases tends to develop continuously, whereas the heterogeneity is retarded in twin-favored deformation. At the intergranular scale, it is concluded from the slip-dominated case that a high slip-transfer parameter and high Schmid factors (SFs) of principal slip systems in adjacent grains could accommodate higher local strain.

36 MATERIALS SCIENCE↗

Analysis of thermal history effects on mechanical anisotropy of 3D-printed polymer matrix composites via in situ X-ray tomography

The tensile behavior of an additively manufactured (AM) polymer matrix composite (PMC) is studied with in situ X-ray computed microtomography (CT) and digital volume correlation (DVC). In this experiment, the effects of recycled material content and print direction on the selective laser-sintered (SLS) material's mechanical response are explored. The PMC samples are printed in a tensile specimen geometry with gage lengths parallel to all three orthogonal, primary sintering directions. In situ tensile-CT experiments are conducted at Argonne National Laboratory's Advanced Photon Source 2-BM beamline. Analysis of the AM PMC's tensile response, failure, and strain evolution is analyzed both from a conventional standpoint, using the load-displacement data recorded by the loading fixture, and from a microstructural standpoint by applying DVC analysis to the reconstructed volumes. Significant variations on both strength and ductility are observed from both vantages with respect to print direction and the recycled material content in the printed parts. As a result, it is found that the addition of recycled source material with a thermal history reduces the tensile strength of the SLS composite for all directions, but the effect is drastic on the strength in the layering direction.

36 MATERIALS SCIENCE↗

Influence of the interface structure on the thermo-mechanical properties of Cu-X (X = Cr or B)/carbon fiber composites

Highlights: Black-Right-Pointing-Pointer Two copper alloys/carbon fibers composites have been produced. Black-Right-Pointing-Pointer Correlation of the thermo-mechanical properties with the microstructure and the chemistry. Black-Right-Pointing-Pointer A composite with CTE 25% lower than a classic Cu/CF composite has been obtained. -- Abstract: This study focuses on the fabrication, for power electronics applications, of adaptive heat sink material using copper alloys/carbon fibers (CF) composites. In order to obtain composite material with good thermal conductivity and a coefficient of thermal expansion close to the ceramic substrate, it is necessary to have a strong matrix/reinforcement bond. Since there is no reaction between copper and carbon, a carbide element (chromium or boron) is added to the copper matrix to create a strong chemical bond. Composite materials (Cu-B/CF and Cu-Cr/CF) have been produced by a powder metallurgy process followed by an annealing treatment in order to create the carbide at the interphase. Chemical (Electron Probe Micro-Analysis, Auger Electron Spectroscopy) and microstructural (Scanning and Transmission Electron Microscopies) techniques were used to study the location of the alloying element and the carbide formation before and after diffusion. Finally, the thermo-mechanical properties have been measured and a promising composite material with a coefficient of thermal expansion 25% lower than a classic copper/carbon heat sink has been obtained.

36 MATERIALS SCIENCE↗

Modeling of microstructural effects on electromigration failure

Current electromigration models used for simulation and analysis of interconnect reliability lack the appropriate description of metal microstructure and consequently have a very limited predictive capability. Therefore, the main objective of our work was obtaining more sophisticated electromigration tools. The problem is addressed through a combination of different levels of atomistic modeling and already available, continuum level macroscopic models. A novel method for an ab initio calculation of the effective valence for electromigration is presented and its application on the analysis of EM behavior is demonstrated. Additionally, a simple analytical model for the early electromigration lifetime is obtained. We have shown that its application provides a reasonable estimate for the early electromigration failures including the effect of microstructure. A simulation study is also applied on electromigration failure in tin solder bumps, where it contributed the understanding of the role of tin crystal anisotropy in the degradation mechanism of solder bumps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

ML-based Micro-CT SOFC Microstructure Models (from Kent 2026 Microstructural Augmentation paper)

Overview -------------------------- This repository contains datasets from the manuscript **"Enhanced Generalizability to Deep-Learning Quantification of 3D Microstructural Characteristics through Microstructurally Aware Augmentation of Scarce Data"** (*William F. Kent, Rochan Bajpai, Rachel C. Kurchin, William K. Epting, Harry W. Abernathy, Paul A. Salvador. Submitted 2026*). The methods are also described in the dissertation **Data Intensive Analysis of Solid Oxide Cell Microstructures** (*Doctoral dissertation, Carnegie Mellon University, 2025*). The datasets here are trained convolutional neural network (CNN) models for predicting key microstructural properties of solid oxide cell (SOC) electrodes from low-res, 2-channel 3D images, as well as some helpful code. The parameters for input images are provided in the paper. Sample data is provided in the file `Combined_anode_aug_dual_1k_examples` - that particular data was used to train `anode_all_aug.pth` and will work most accurately with that model. Please familiarize yourself with all caveats on accuracy and applicability, as detailed in the associated paper. Usage -------------------------- The basic usage is as follows, assuming `model_fn` is the path to the .pth file, and `X` is 2-channel input image(s) of the proper dimensions (either one image of shape `[2,12,24,24]`, or a batch of N input images of shape `[N,2,12,24,24]`): from CNN_inferencer import load_model_for_inference model = load_model_for_inference(model_fn) y_predicted = model(X) The model object automatically handles input scaling and output de-scaling based on the way the models were trained - in other words, pass in a 2-channel micro-CT image, and it will output microstructural property values in real units. ## Other model object attributes Note that model has useful attributes other than its forward pass model(X). * `model.output_descaler` - returns the output descaler object. Model does the de-scaling when generating inferences, but you may want to re-use this de-scaler on other values to e.g. compare predictions to ground truth from already-scaled training data. * `model.prop_names` - Gives the property names of the predicted y values, in order. Only exists if there's an output scaler as part of the model object, which there will be in the models provided here. ## Usage with sample data Here is a short script to use with the included sample data. from CNN_inferencer import display_predictions, load_model_for_inference, calculate_mape, parity_plot import h5py import numpy as np model_fn = 'anode_all_aug.pth' data_fn = 'Combined_anode_aug_dual_1k_examples.h5' N_samples = 200 figure_outdir = '.' model = load_model_for_inference(model_fn) with h5py.File(data_fn,'r') as f: XX = f['X'] #These are the 2-channel 3D images yy = f['y'] #These are the ground-truth microstructural properties, but they have been scaled for training - need to de-scale below N = XX.shape[0] #How many images total in the input data file #Run inferences on N_samples random samples from XX. #Run in a batch, much more efficient than one at a time. ii = np.random.choice(N,N_samples,replace=False) ii.sort() y_pred = model(XX[ii]) #Get the original/true (but normalized/scaled) values from the training dataset... #Because they were normalized, they are not in real units yet. So let's also de-scale them using model.output_scaler. y_true = model.output_scaler.transform(yy[ii]) #Let's display actual values for just 5 random ones for i in np.random.choice(N_samples,5,replace=False): display_predictions(y_true[i], y_pred[i], model.prop_names) #Make parity plots for each property (ground truth vs predicted values) #Also label each plot with the mean abs. percent error (MAPE) of the predicted values for i,key in enumerate(model.prop_names): mape = calculate_mape(y_true[:,i], y_pred[:,i]) parity_plot(y_true[:,i], y_pred[:,i], figure_outdir, key, extra_title=f' ({mape:.2f}% MAPE)')

3D microstructure↗

Microstructure-based modeling of inner oxygen pressure in solid oxide electrolysis cells: Analysis of electrode delamination and mitigation

One major degradation mechanism during long-term operation of solid oxide electrolysis cells (SOECs) is delamination of oxygen electrodes (OEs). The driving force for the electrode delamination could be the generated high inner oxygen pressure near the electrode-electrolyte interface during operation. However, the effects of transport properties and electrode thickness on the inner oxygen partial pressure are not well understood. Here a microstructure-based electrochemical model, which includes the conduction of electrons and oxygen ions coupled with Butler-Volmer-type chemical reactions at triple-phase-boundaries (TPBs), is employed to investigate the oxygen pressure in lanthanum strontium manganate (LSM)-based SOECs. The model is applied to both two-dimensional (2D) prototype microstructures and three-dimensional (3D) realistic microstructures, and the oxygen pressure is analyzed as a function of transport properties and electrode thickness under both potentiostatic and galvanostatic operations. The simulation results suggest strategies to suppress electrode delamination. The simulation results are compared to an analytical solution, and the discrepancies are attributed to the Butler-Volmer-type kinetics included in the microstructure-based model.

25 ENERGY STORAGE↗

A new analysis approach based on Haralick texture features for the characterization of microstructure on the example of low-alloy steels

Highlights: • Microstructures were characterized based on orientation-invariant image-texture features. • A new parameter called “amplitude”, was formulated and is based on image rotation and the Haralick parameters: texture contrast, correlation, homogeneity and energy. • The proposed method is insensitive to changing image resolution and image contrast/brightness settings. - Abstract: Microstructures were analyzed by an improved texture-based method using gray level co-occurrence matrices (GLCM). This method is based on a new parameter calculated from the stepwise rotation of images and thereby, calculating the values independent of the original texture orientation. The proposed method was applied on a database of etched and scanning electron microscopy (SEM)-imaged low-carbon steel microstructures that are currently extensively used for automated microstructure classification. The results on the microstructures consisting of pearlitic, lath martensitic and lower bainitic constituents revealed that the method allows a significant separation of various types of microstructures in the ideal case of square-shaped cutouts. For complete grains of the corresponding second phases, the results imply that the application of a classifier is advantageous to distinguish them with a sufficient accuracy. The robustness and workability of the method was further demonstrated by discussing the effect of varying the image resolution and contrast/brightness settings during image acquisition. It was shown that such user-dependent setting parameters do not impair the separability of the steel constituents by using the proposed method.

36 MATERIALS SCIENCE↗