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At least 595 records · Page 33

Framework of compressive sensing and data compression for 4D-STEM

Four-dimensional Scanning Transmission Electron Microscopy (4D-STEM) is a powerful technique for high-resolution and high-precision materials characterization at multiple length scales, including the characterization of beam-sensitive materials. However, the field of view of 4D-STEM is relatively small, which in absence of live processing is limited by the data size required for storage. Furthermore, the rectilinear scan approach currently employed in 4D-STEM places a resolution- and signal-dependent dose limit for the study of beam sensitive materials. Improving 4D-STEM data and dose efficiency, by keeping the data size manageable while limiting the amount of electron dose, is thus critical for broader applications. Here we introduce a general method for reconstructing 4D-STEM data with subsampling in both real and reciprocal spaces at high fidelity. The approach is first tested on the subsampled datasets created from a full 4D-STEM dataset, and then demonstrated experimentally using random scan in real-space. The same reconstruction algorithm can also be used for compression of 4D-STEM datasets, leading to a large reduction (100 times or more) in data size, while retaining the fine features of 4D-STEM imaging, for crystalline samples.

4D-STEM↗

Exploring Domain-Wall Pinning in Ferroelectrics via Automated High-Throughput Atomic Force Microscopy

Domain-wall dynamics in ferroelectric materials are strongly position-dependent, since each polar interface is locked into a unique local microstructure. This necessitates spatially resolved studies of wall pinning using scanning-probe microscopy techniques. The pinning centers and pre-existing domain walls are usually sparse within the image plane, precluding the use of dense hyperspectral imaging modes and requiring time-consuming human experimentation. Here, a large-area epitaxial PbTiO 3 film on cubic KTaO 3 was investigated to quantify the electric-field-driven dynamics of the polar–strain domain structures using ML-controlled automated piezoresponse force microscopy. Analysis of 1500 switching events reveals that domain-wall displacement depends not only on field parameters but also on the local ferroelectric–ferroelastic configuration. For example, twin boundaries in polydomains regions, like a 1 – /c+ ∥ a 2 – /c – , stay pinned up to a certain level of bias magnitude and change only marginally as the bias increases from 20 to 30 V, whereas single-variant boundaries, like the a 2 + /c + ∥ a 2 – /c – stack, are already activated at 20 V. These statistics on the possible ferroelectric and ferroelastic wall orientations, together with the automated high-throughput AFM workflow, can be distilled into a predictive map that links domain configurations to pulse parameters. Here, this microstructure-specific rule set forms the foundation for the design of ferroelectric memories.

automated scanning probe microscopy↗

Electron Microscopy Studies of Soft Nanomaterials

This review highlights recent efforts on applying electron microscopy (EM) to soft (including biological) nanomaterials. We will show how developments of both the hardware and software of EM have enabled new insights into the formation, assembly, and functioning (e.g., energy conversion and storage, phonon/photon modulation) of these materials by providing shape, size, phase, structural, and chemical information at the nanometer or higher spatial resolution. Specifically, we first discuss standard real-space two-dimensional imaging and analytical techniques which are offered conveniently by microscopes without special holders or advanced beam technology. The discussion is then extended to recent advancements, including visualizing three-dimensional morphology of soft nanomaterials using electron tomography and its variations, identifying local structure and strain by electron diffraction, and recording motions and transformation by in situ EM. On these advancements, we cover state-of-the-art technologies designed for overcoming the technical barriers for EM to characterize soft materials as well as representative application examples. Here, the even more recent integration of machine learning and its impacts on EM are also discussed in detail. With our perspectives of future opportunities offered at the end, we expect this review to inspire and stimulate more efforts in developing and utilizing EM-based characterization methods for soft nanomaterials at the atomic to nanometer length scales in academic research and industrial applications.

Imaging↗

Increased AGE Cross-Linking Reduces the Mechanical Properties of Osteons

Abstract The osteon is the primary structural component of bone, contributing significantly to its unique toughness and strength. Despite extensive research on osteonal structure, the properties of osteons have not been fully investigated, particularly within the context of bone fragility diseases like type 2 diabetes mellitus (T2DM). This study aims to isolate osteons from bovine bone, simulate the effects of increased advanced glycation end-products (AGEs) in T2DM through ribosylation, and evaluate the mechanical properties of isolated osteons. Osteons extracted from the posterior section of bovine femur mid-diaphysis were processed to achieve a sub-millimeter scale for microscale imaging. Subsequently, synchrotron radiation micro-computed tomography was employed to precisely localize and isolate the osteon internally. While comparable elastic properties were observed between control and ribosylated osteons, the presence of AGEs led to decreased strain to failure. Young’s modulus was quantified (9.9 ± 4.9 GPa and 8.7 ± 3 GPa, respectively), aligning closely with existing literature. This study presents a novel method for the extraction and isolation of osteons from bone and shows the detrimental effect of AGEs at the osteonal level.

Materials Science↗

Parasitic structure defect blights sustainability of cobalt-free single crystalline cathodes

Abstract Recent efforts to reduce battery costs and enhance sustainability have focused on eliminating Cobalt (Co) from cathode materials. While Co-free designs have shown notable success in polycrystalline cathodes, their impact on single crystalline (SC) cathodes remains less understood due to the significantly extended lithium diffusion pathways and the higher-temperature synthesis involved. Here, we reveal that removing Co from SC cathodes is structurally and electrochemically unfavorable, exhibiting unusual voltage fade behavior. Using multiscale diffraction and imaging techniques, we identify lithium-rich nanodomains (LRNDs) as a heterogeneous phase within the layered structure of Co-free SC cathodes. These LRNDs act as critical tipping points, inducing significant chemo-mechanical lattice strain and irreversible structural degradation, which exacerbates the voltage and capacity loss in electrochemical performance. Our findings highlight the considerable challenges of developing Co-free SC cathodes compared to polycrystalline ones and emphasize the need for new strategies to balance the interplay between cost, sustainability, and performance.

36 MATERIALS SCIENCE↗

X-ray diffraction at the National Ignition Facility

We report details of an experimental platform implemented at the National Ignition Facility to obtain in situ powder diffraction data from solids dynamically compressed to extreme pressures. Thin samples are sandwiched between tamper layers and ramp compressed using a gradual increase in the drive-laser irradiance. Pressure history in the sample is determined using high-precision velocimetry measurements. Up to two independently timed pulses of x rays are produced at or near the time of peak pressure by laser illumination of thin metal foils. The quasi-monochromatic x-ray pulses have a mean wavelength selectable between 0.6 Å and 1.9 Å depending on the foil material. The diffracted signal is recorded on image plates with a typical 2 θ x-ray scattering angle uncertainty of about 0.2° and resolution of about 1°. Analytic expressions are reported for systematic corrections to 2 θ due to finite pinhole size and sample offset. A new variant of a nonlinear background subtraction algorithm is described, which has been used to observe diffraction lines at signal-to-background ratios as low as a few percent. Variations in system response over the detector area are compensated in order to obtain accurate line intensities; this system response calculation includes a new analytic approximation for image-plate sensitivity as a function of photon energy and incident angle. This experimental platform has been used up to 2 TPa (20 Mbar) to determine the crystal structure, measure the density, and evaluate the strain-induced texturing of a variety of compressed samples spanning periods 2–7 on the periodic table.

47 OTHER INSTRUMENTATION↗

Assessing continuum plasticity postulates with grain stress and local strain measurements in triaxially compressed sand

Critical state and continuum plasticity theories have been used in research and engineering practice in soil and rock mechanics for decades. These theories rely on postulated relationships between material stresses and strains. Some classical postulates include coaxiality between stress and strain rates, stress–dilatancy relationships, and kinematic assumptions in shear bands. Although numerical and experimental data have quantified the strains and grain kinematics in such experiments, little data quantifying grain stresses are available. Here, we report the first-known grain stress and local strain measurements in triaxial compression tests on synthetic quartz sands using synchrotron X-ray tomography and 3D X-ray diffraction. We use these data to examine the micromechanics of shear banding, with a focus on coaxiality, stress-dilatancy, and kinematics within bands. Our results indicate the following: 1) elevated deviatoric stress, strain, and stress ratios in shear bands throughout experiments; 2) coaxial principal compressive stresses and strains throughout samples; 3) significant contraction along shear bands; 4) vanishing volumetric strain but nonvanishing stress fluctuations throughout samples at all stages of deformation. Our results provide some of the first-known in situ stress and strain measurements able to aid in critically evaluating postulates employed in continuum plasticity and strain localization theories for sands.

42 ENGINEERING↗

Rationalizing VICAR within a TAE framework: Some problems and some solutions

Transportable Applications Executive (TAE) implementation may impose a strain on centers with modest resources. This may be eased in a number of ways. The balance of a small number of expert users and a large number of computing novices at the Interactive Planetary Image-Processing System (IPIPS) imposes special constraints. Some solutions to these and other particular problems are described.

Harris, Colin P.↗

An approach for relating the results of quantitative nondestructive evaluation to intrinsic properties of high-performance materials

One of the most difficult problems the manufacturing community has faced during recent years has been to accurately assess the physical state of anisotropic high-performance materials by nondestructive means. In order to advance the design of ultrasonic nondestructive testing systems, a more fundamental understanding of how ultrasonic waves travel and interact within the anisotropic material is needed. The relationship between the ultrasonic and engineering parameters needs to be explored to understand their mutual dependence. One common denominator is provided by the elastic constants. The preparation of specific graphite/epoxy samples to be used in the experimental investigation of the anisotropic properties (through the measurement of the elastic stiffness constants) is discussed. Accurate measurements of these constants will depend upon knowledge of refraction effects as well as the direction of group velocity propagation. The continuing effort for the development of improved visualization techniques for physical parameters is discussed. Group velocity images are presented and discussed. In order to fully understand the relationship between the ultrasonic and the common engineering parameters, the physical interpretation of the linear elastic coefficients (the quantities that relate applied stresses to resulting strains) are discussed. This discussion builds a more intuitional understanding of how the ultrasonic parameters are related to the traditional engineering parameters.

Miller, James G.↗

Anatomical Fraction segmentation in the biomass bales

The U.S. Department of Energy Bioenergy Technologies Office (BETO) is committed to the development of sustainable, nationwide, commercial biofuel production to displace petroleum-derived fuels, increase domestic energy production, and encourage the creation of a domestic bioenergy and bioproducts industry. Operating a commercial-scale bioenergy operation requires significant technological advancements for determining biomass feedstock quality during the preprocessing stage. Usage of non-food feedstocks- e.g., corn-stover, pine residue, and forest residue - at the biorefineries reduces strain on the food supply chain. But the non-food feedstock heterogeneity- physical size, shape, and chemical composition-poses a significant challenge during milling, conveyance, feeding, and biofuel conversion processes. 3D X-Ray imaging (CT) is capable of distinguishing material features by detecting density and compositional differences. But the inherent complexity introduced during harvesting and bailing makes the reconstruction and interpretation of baled biomass materials from x-ray data time consuming, laborious, and expensive. Feedstocks are low-density materials that produce small contrast differences in the x-ray images. This paper focuses on using the shape and texture properties, using 3D image processing techniques like 3D skeletonization, directional statistics to characterize and extract volumetric content of the different tissue samples in the biomass bales.

09 BIOMASS FUELS↗

Real-Space Infrared Spectroscopy of Ferroelectric Domain Walls in Multiferroic h -(Lu,Sc)FeO 3

Herein we employ synchrotron-based near-field infrared spectroscopy to image the phononic properties of ferroelectric domain walls in hexagonal ( h ) Lu 0.6 Sc 0.4 FeO 3 , and we compare our findings with a detailed symmetry analysis, lattice dynamics calculations, and prior models of domain-wall structure. Rather than metallic and atomically thin as observed in the rare-earth manganites, ferroelectric walls in h -Lu 0.6 Sc 0.4 FeO 3 are broad and semiconducting, a finding that we attribute to the presence of an A -site substitution-induced intermediate phase that reduces strain and renders the interior of the domain wall nonpolar. Mixed Lu/Sc occupation on the A site also provides compositional heterogeneity over micron-sized length scales, and we leverage the fact that Lu and Sc cluster in different ratios to demonstrate that the spectral characteristics at the wall are robust even in different compositional regimes. This work opens the door to broadband imaging of physical and chemical heterogeneity in ferroics and represents an important step toward revealing the rich properties of these flexible defect states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Geophysical Signatures of Crack Network Coalescence in Rocks at Multiple Length Scales

The main goal of the research project was to identify the geophysical signatures of fracture growth in natural rocks by utilizing novel geophysical techniques. The research objectives were to (a) investigate the potential for geophysical methods to determine when cracks initiate, the types and locations of propagated cracks, and the coalescence of networks of cracks in natural rocks at multiple scales, (b) determine how damage at the microscale evolved into damage at the macroscale and then link the microscopic and macroscopic observations, (c) quantify crack coalescence in rocks under realistic stress conditions using coupled mechanical-geophysical-optical visualization, and (d) identify the precursors in geophysical signals to crack coalescence. The following research thrusts were explored to achieve the research objectives: (1) uniaxial compression testing of rock specimens with and without a set of pre‐existing flaws and (2) triaxial compression testing of natural rock specimens. These thrusts allowed for exploring fracturing in rocks under realistic in situ environments and at multiple scales. This project provided educational opportunities for nine graduate and undergraduate students and resulted in 27 peer-reviewed publications. This first research thrust focused on investigating the micromechanics of fractures in rocks through uniaxial compression testing combined with advanced geophysical and imaging techniques, specifically acoustic emission (AE) monitoring, ultrasonic imaging, and 2-dimensional Digital Image Correlation (2D-DIC). By examining damage processes under time-independent and time-dependent loading conditions, insights into damage localization, crack initiation, and fracturing mechanisms were gained. It was observed that the AE signals and the strain-based measurements directly reflect the state of damage in the rock specimen and could be used to identify the cracking levels, such as the crack initiation (CI) and crack damage (CD), and the mode of deformation. A novel calibration apparatus was developed to enhance the accuracy of AE sensors, allowing for the estimation of key parameters such as magnitude, source dimension, stress drop, and radiated seismic energy associated with the fractures. The findings highlighted significant variations in the temporal evolution of AE source parameters during the primary, secondary, and tertiary stages of creep, identifying tensile cracking as the primary deformation mode. The second research thrust focused on enhancing the understanding of fracturing processes in natural rocks through triaxial compression testing, real-time AE monitoring, and ultrasonic monitoring. We investigated the impact of various factors such as fracture propagation regimes, injection parameters, rock types, and pre-existing conditions on the hydraulic fracture (HF) behavior using scaled true-triaxially loaded specimens of Barre granite and Lyons sandstone. Custom sensor housing facilitated concurrent active and passive monitoring to analyze hydro-mechanical responses and microseismicity associated with different HF scenarios. A coupled investigation of passive microseismicity and active signal attributes permitted a detailed comprehension of the various HF processes (aseismic deformation, fracture initiation and propagation, fluid permeation, and leak-off) and their dependence on the specific rock type. The findings of this research demonstrated the effectiveness of AE monitoring techniques in providing valuable insights into the impact of various factors on the behavior and dynamics of HF processes. The advancements in monitoring techniques, offering a more thorough and precise approach, represent a significant step towards optimizing HF practices and ensuring sustainable resource extraction.

58 GEOSCIENCES↗

Mechanisms of paint bake response in resistance spot-welded first and third generation AHSS

Implementation of 3rd generation advanced high strength steels (3GAHSS) in automotive structures requires careful consideration of joining process implications. Due to the presence of increased carbon equivalent in 3GAHSS such as 980 HF relative to commonly-applied 1st generation AHSS such as 980 DP, the resultant properties of the weld nugget and heat affected zones in resistance spot welded must be engineered to provide consistent and acceptable performance, specifically in cross-tension loading mode. Although the as-welded cross-tension strength (CTS) of 980 HF is less than 980 DP, there is a significant improvement of the CTS after paint baking in 980 HF welds. 980 DP steel welds do not exhibit such marked improvement upon baking. The mechanism of the strong and beneficial effect of paint baking on 980 HF in comparison to 980 DP is discussed in light of its effect on residual stress distributions and microstructures. Although residual stress (strain) reduction is observed via synchrotron x-ray diffraction for all tested steels, this effect is demonstrated as secondary to the performance restoration of the weld joint in cross tension. High-resolution electron channeling contrast imaging (ECCI) micrographs reveal that paint baking affects a more beneficial degree of martensite tempering in 980 HF as compared to 980 DP. The martensite tempering is also evidenced by both a reduction in nano-hardness of critical microstructural features and re-emergence of ductile fracture behavior following the paint baking process. The tempering of martensite is concluded to be the dominant mechanism in improving cross tension strength of 3GAHSS welds following paint baking.

36 MATERIALS SCIENCE↗

Controlling mechanical properties of laser powder bed fused AlSi10Mg through manipulation of laser scan rotation

The microstructure and mechanical properties of laser powder bed fused (LPBF) AlSi10Mg alloys can be controlled by many processing parameters. This study focuses on the scan rotation angle, α, between adjacent layers, and establishes the relationship between α and tensile behavior of the as-built LPBF-processed AlSi10Mg alloy. Near-full density cubic coupons were manufactured using the same processing parameters but with systematic variation of α from 0° to 90°. Microscopic observations and X-ray diffraction analysis showed that differences among various coupons mainly include orientations of the melt pools with respect to the build direction and development of the crystallographic texture. The α=0° coupon and α=30° coupon showed the highest and lowest texture index, although the overall crystallographic texture was mild. Tensile specimens were manufactured horizontally and vertically using either α=0° or α=30°, but with various first layer laser direction with respect to the build plate. Notably, the α=0° specimen that was tested along the laser scan direction showed the largest yield strength (283 MPa) and highest tensile ductility (10.1 %). Quantitative image analysis and fractography were performed on all specimens. Results showed that the melt pool orientation with respect to the tensile direction affected the tensile behavior across the different specimens. This was closely related to the localized strain distribution within the melt pool and along the melt pool boundary for the different melt pool orientations observed. Further, these results demonstrate that the laser scan rotation angle between layers can be used to fine tune the mechanical properties of LPBF AlSi10Mg alloy.

36 MATERIALS SCIENCE↗

Report of the panel on plate motion and deformation, section 2

Given here is a panel report on the goals and objectives, requirements and recommendations for the investigation of plate motion and deformation. The goals are to refine our knowledge of plate motions, study regional and local deformation, and contribute to the solution of important societal problems. The requirements include basic space-positioning measurements, the use of global and regional data sets obtained with space-based techniques, topographic and geoid data to help characterize the internal processes that shape the planet, gravity data to study the density structure at depth and help determine the driving mechanisms for plate tectonics, and satellite images to map lithology, structure and morphology. The most important recommendation of the panel is for the implementation of a world-wide space-geodetic fiducial network to provide a systematic and uniform measure of global strain.

Bock, Yehuda↗

Mechanisms of compressive failure in 3D composites

The present study of angle-interlock woven polymer matrix composite behavior under uniaxial monotonic compression notes these materials to be macroscopically ductile, with compressive strains in failure that can exceed 15 percent. Some of the tests conducted on stitched laminates indicated brittle behavior. Woven composite failure mechanisms have been studied by a combination of optical microscopy, moire interferometry, stereoscopy, and digital image comparisons; the critical failure event was in all cases a kink band formation in the primary load-bearing axial rows.

Cox, B. N.↗

Enhanced Raman Microprobe Imaging of Single-Wall Carbon Nanotubes

We explore Raman microprobe capabilities to visualize single wall carbon nanotubes (SWCNTs). Although this technique is limited to a micron scale, we demonstrate that images of individual SWCNTs, bundles or their agglomerates can be generated by mapping Raman active elementary excitations. We measured the Raman response from carbon vibrations in SWCNTs excited by confocal scanning of a focused laser beam. Carbon vibrations reveal key characteristics of SWCNTs as nanotube diameter distribution (radial breathing modes, RBM, 100-300 cm(exp -1)), presence of defects and functional groups (D-mode, 1300-1350 cm(exp -1)), strain and oxidation states of SWCNTs, as well as metallic or semiconducting character of the tubes encoded in the lineshape of the G-modes at 1520-1600 cm(exp - 1). In addition, SWCNTs are highly anisotropic scatterers. The Raman response from a SWCNT is maximal for incident light polarization parallel to the tube axis and vanishing for perpendicular directions. We show that the SWCNT bundle shape or direction can be determined, with some limitations, from a set of Raman images taken at two orthogonal directions of the incident light polarization.

Hadjiev, V. G.↗

The effects of microstructure on deformation twinning in Mg WE43

The interplay between microstructure and deformation twinning in a WE43-T6 Mg alloy under uniaxial compression was investigated using a combination of scanning electron microscopy with digital image correlation (SEM-DIC) and crystal plasticity finite element (CPFE) simulation. To improve understanding of the statistical characteristics of deformation twin formation, microstructural effects were characterized in over 1000 grains through metrics including the nominal Schmid Factor, grain size, geometric compatibility factor (m'), residual Burgers vector, and the strain accommodated by neighboring grains. There was a strong correlation between the nominal Schmid Factor and both twin activation and variant selection, but this was not fully deterministic. Deformation twinning also exhibited a strong dependence on existing slip and twinning in the neighboring grain and on the m' value. Within the range of grain sizes present in this condition, grain size was determined to have minimal effect on deformation twinning. Finally, statistical analysis of CPFE simulations was used to further investigate microstructural effects on twinning, and qualitatively captured the effect of the nominal Schmid Factor.

36 MATERIALS SCIENCE↗