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At least 469 records · Page 26

Microscopic assessment of ASR-affected concrete under confinement conditions

The Damage Rating Index (DRI), a semi-quantitative microscopic procedure, has been successfully used to describe alkali-silica reaction (ASR) damage development of concrete under “free expansion” conditions. Yet, the confinement impact on ASR-induced cracks' generation and propagation has not been fully investigated. This work aims to understand the influence of confinement on ASR development through the DRI. Eighteen concrete blocks incorporating a highly reactive coarse aggregate and distinct reinforcement configurations were manufactured, stored in conditions enabling ASR development, and monitored over time. Two expansion levels were selected for analysis (0.08% and 0.15%) and once reached, cores were extracted from three different directions (longitudinal, transverse and vertical) and the DRI conducted on those. Results demonstrate that ASR-induced expansion and deterioration change according to the direction and confinement configuration. Moreover, distinct crack features and orientations are generated in confined concrete, which attests that ASR displays different damage mechanisms under free and confinement conditions.

36 MATERIALS SCIENCE↗

Quantification of grain boundary effects on the geometrically necessary dislocation density evolution and strain hardening of polycrystalline Mg 4Al using in situ tensile testing in scanning electron microscope and HR-EBSD

In situ tensile testing in a scanning electron microscope (SEM) in conjunction with high-resolution electron backscatter diffraction (HR-EBSD) under load was used to characterize the evolution of geometrically necessary dislocation (GND) densities at individual grain boundaries as a function of applied strain in a polycrystalline Mg—4Al alloy. The increase in GND density was investigated at plastic strains of 0 %, 0.6 %, 2.2 %, 3.3 % from the area including 76 grains and correlated with (i) geometric compatibility between slip systems across grain boundaries, and (ii) plastic incompatibility. We develop expressions for the grain boundary GND density evolution as a function of plastic strain and plastic incompatibility, from which uniaxial tensile stress-strain response of polycrystalline Mg—4Al are computed and compared with experimental measurement. The findings in this study contribute to understanding the mechanisms governing the strain hardening response of single-phase polycrystalline alloys and more reliable prediction of mechanical behaviors in diverse microstructures.

Geometrically necessary dislocations↗

A microscopic continuum model for defect dynamics in metallic glasses

Motivated by results of the topological theory of glasses accounting for geometric frustration, here we develop the simplest possible continuum mechanical model of defect dynamics in metallic glasses that accounts for topological, energetic, and kinetic ideas. A geometrical description of ingredients of the structure of metallic glasses using the concept of local order based on Frank–Kasper phases and the notion of disclinations as topological defects in these structures is proposed. This novel kinematics is incorporated in a continuum mechanical framework capable of describing the interactions of disclinations and also of dislocations (interpreted as pairs of opposite disclinations). The model is aimed towards the development of a microscopic understanding of the plasticity of such materials. We discuss the expected predictive capabilities of the model vis-a-vis some observed physical behaviors of metallic glasses.

36 MATERIALS SCIENCE↗

Learning macroscopic internal variables and history dependence from microscopic models

This paper concerns the study of history dependent phenomena in heterogeneous materials in a two-scale setting where the material is specified at a fine microscopic scale of heterogeneities that is much smaller than the coarse macroscopic scale of application. Here, we specifically study a polycrystalline medium where each grain is governed by crystal plasticity while the solid is subjected to macroscopic dynamic loads. The theory of homogenization allows us to solve the macroscale problem directly with a constitutive relation that is defined implicitly by the solution of the microscale problem. However, the homogenization leads to a highly complex history dependence at the macroscale, one that can be quite different from that at the microscale. In this paper, we examine the use of machine-learning, and especially deep neural networks, to harness data generated by repeatedly solving the finer scale model to: (i) gain insights into the history dependence and the macroscopic internal variables that govern the overall response; and (ii) to create a computationally efficient surrogate of its solution operator, that can directly be used at the coarser scale with no further modeling. We do so by introducing a recurrent neural operator (RNO), and show that: (i) the architecture and the learned internal variables can provide insight into the physics of the macroscopic problem; and (ii) that the RNO can provide multiscale, specifically FE 2 , accuracy at a cost comparable to a conventional empirical constitutive relation.

36 MATERIALS SCIENCE↗

Multiaxial ratcheting of 20 carbon steel: Macroscopic experiments and microscopic observations

The multiaxial ratcheting behaviors of polycrystalline 20 ordinary carbon steel were investigated at room temperature. The macroscopic experimental results showed that the studied multiaxial ratcheting depends greatly on the mean stress, stress amplitude and loading path. The axial ratcheting strain increased with the increase of applied mean stress and stress amplitude. Apparent additional hardening was observed in the non-proportionally multiaxial cyclic loading. The multiaxial ratcheting of 20 carbon steel was lower than the corresponding uniaxial one and varies with different loading paths. Dislocation patterns and their evolutions of the multiaxial ratcheting of different loading paths were then investigated using transmission electron microscopy. The obtained images showed that, with the increasing number of loading cycles, the dislocation patterns evolved from dislocation lines and networks to dislocation tangles, walls and cells. After certain cycles, sub-grains were formed because of the re-arrangement of dislocations in the walls of cells and inside the cells since the cross slip of dislocations can be easily activated for the 20 carbon steel, a kind of body-centered cubic metal. The dislocation evolution of the multiaxial ratcheting is much quicker than that of the uniaxial one. With the reference to the uniaxial one of 20 carbon steel, the macroscopic multiaxial ratcheting behaviors can be qualitatively correlated with the microscopic observation of the dislocation patterns and their evolution. - Highlights: • Multiaxial loading hardly changes the cyclic stable feature of 20 carbon steel. • Multiaxial ratcheting of 20 carbon steel depends greatly on the load path. • Dislocation patterns evolve quicker in the multiaxial case. • The stabilized dislocation pattern is sub-grain, rather than the dislocation cell. • Sub-grains formed after certain cycles make the stable ratcheting strain rate large.

36 MATERIALS SCIENCE↗

Determining the sputter yields of molybdenum in low-index crystal planes via electron backscattered diffraction, focused ion beam and atomic force microscope

Previous literature has used several monocrystalline sputtering targets with various crystalline planes, respectively, to investigate the variations of the sputter yield of materials in different crystalline orientations. This study presents a method to measure the sputtered yields of Mo for the three low-index planes (100), (110), and (111), through using an easily made polycrystalline target. The procedure was firstly to use electron backscattered diffraction to identify the grain positions of the three crystalline planes, and then use a focused ion beam to perform the micro-milling of each identified grain, and finally the sputter yields were calculated from the removed volumes, which were measured by atomic force microscope. Experimental results showed that the sputter yield of the primary orientations for Mo varied as Y{sub (110)} > Y{sub (100)} > Y{sub (111)}, coincidental with the ranking of their planar atomic packing densities. The concept of transparency of ion in the crystalline substance was applied to elucidate these results. In addition, the result of (110) orientation exhibiting higher sputter yield is helpful for us to develop a Mo target with a higher deposition rate for use in industry. By changing the deformation process from straight rolling to cross rolling, the (110) texture intensity of the Mo target was significantly improved, and thus enhanced the deposition rate. - Highlights: • We used EBSD, FIB and AFM to measure the sputter yields of Mo in low-index planes. • The sputter yield of the primary orientations for Mo varied as Y{sub (110)} > Y{sub (100)} > Y{sub (111)}. • The transparency of ion was used to elucidate the differences in the sputter yield. • We improved the sputter rate of polycrystalline Mo target by adjusting its texture.

36 MATERIALS SCIENCE↗

A simple and inclusive method to determine the habit plane in transmission electron microscope based on accurate measurement of foil thickness

A simple and inclusive method is proposed for accurate determination of the habit plane between bicrystals in transmission electron microscope. Whilst this method can be regarded as a variant of surface trace analysis, the major innovation lies in the improved accuracy and efficiency of foil thickness measurement, which involves a simple tilt of the thin foil about a permanent tilting axis of the specimen holder, rather than cumbersome tilt about the surface trace of the habit plane. Experimental study has been done to validate this proposed method in determining the habit plane between lamellar α{sub 2} plates and γ matrix in a Ti–Al–Nb alloy. Both high accuracy (± 1°) and high precision (± 1°) have been achieved by using the new method. The source of the experimental errors as well as the applicability of this method is discussed. Some tips to minimise the experimental errors are also suggested. - Highlights: • An improved algorithm is formulated to measure the foil thickness. • Habit plane can be determined with a single tilt holder based on the new algorithm. • Better accuracy and precision within ± 1° are achievable using the proposed method. • The data for multi-facet determination can be collected simultaneously.

36 MATERIALS SCIENCE↗

Microscopic deformation compatibility during monotonic loading in a Mg-Gd-Y alloy

Microscopic deformation compatibility is a key in achieving high ductility in polycrystalline magnesium alloys. This paper presents a grain-level compatibility investigation of Mg-Gd-Y alloy using in-situ tension in scanning electron microscopy (SEM) combined with electron back scattered diffraction (EBSD) and digital image correlation (DIC) techniques. The results show that strain amplitudes are not always higher in grains with high Schmid factors of basal slip. Thus, the Schmid law can hardly predict the strain amplitudes at grain level. In addition, the average intergranular strains are higher than the average intragranular strain and a strong surrounding effect grain-to-grain was found. A slip-transfer parameter m′, describing the surrounding effect, was used to evaluate the deformation compatibility. It is found that a high m′ value and a high Schmid factor of certain slip system in the adjacent grains would result in a good compatibility around grain boundaries and could accommodate higher local strains, which would improve the ductility of magnesium alloys. - Highlights: •Microstructure based DIC analyses have been performed on a Mg-Gd-Y alloy. •Strain amplitudes are higher at grain boundary areas than grain interiors. •Schmid Law is not applicable for predicting the strain amplitudes. •A geometric parameter m′ can effectively evaluate strain.

36 MATERIALS SCIENCE↗

Elucidating the microscopic origin of electrochemical corrosion and electrical conductivity by lattice response to severe plastic deformation in Al-Mn-Si alloy

Highlights: • Al-Mn-Si specimens were underwent severe plastic deformation by CGP and cold-rolling and their combined routes. • Microscopical observations depicted particles' fragmentation and non-preferential distribution under heavy straining. • XRD analysis revealed dislocations annihilation and lattice swelling (d-spacing increase) due to dynamic recrystallization. • Polarization outputs disclosed direct correlation of corrosion behavior with dislocations density. • Four-point probe test proved that electrical conductivity was a function of lattice d-spacing. - Abstract: Al-Mn-Si specimens were underwent SPD by CGP, cold-rolling and their combined paths. Acquired OM and SEM micrographs revealed that random distribution of intermetallic precipitates beside their fragmentation under heavy imposed strains deteriorated particles’ influence on the electrochemical corrosion and inhibited pitting. Analysis of XRD patterns pointed out that post-rolling of CGPed sheets resulted in dynamic annihilation of dislocations and accordingly crystal lattice swelling (d-spacing increase) due to dynamic recrystallization. From polarization results, crystallites’ refinement along with density increment of sub-grain boundaries within structure as a consequence of SPD beside dislocation density enhancement accelerated corrosion. Outputs of four-point probe electrical conductivity examination indicated that apart from the employed processing, lattice compaction and atomic layers approach would limit the electrons’ mobility space and hence reduce the conductivity of material. In this regard, combined effects of CGP and rolling as employed dual-straining route on Al-Mn-Si alloy enhanced the electrical conductivity by d-spacing growth.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

The roles of interfaces and other microstructural features in Cu/Nb nanolayers as revealed by in situ beam bending experiments inside an scanning electron microscope (SEM)

Interfaces and their interactions with other microstructural features, such as grain boundaries or twin structures, have been widely viewed as parameters for designing metallic nanolayers. These interfaces could play a role in hindering cracks from propagating across the nanolayers while in operation. To date, many studies have focused on the roles of interfaces in affecting the plasticity mechanisms and thus the deformability of nanolayers. However, no studies have investigated on the subsequent mechanisms of fracture leading to the final failure. In this study, in situ microfracture bending tests inside a scanning electron microscope (SEM) were performed on the notched clamped beams of Cu/Nb nanolayers with a similar layer thickness using two different fabrication processes: physical vapor deposition (PVD) and accumulative roll bonding (ARB). Due to the columnar grains of the Cu/Nb PVD beams, a sudden catastrophic linear elastic, brittle fracture phenomenon was observed; in the Cu/Nb ARB beams, fracture events of notch widening phase and crack initiation and fracture along the shear instability were observed. Detailed examinations showed the presence of competing mechanisms between the multilayered interface, columnar grain boundary, and experimental factors of beam geometry and the position of the tip. With this newfound knowledge, new types of metallic nanolayers can be designed with enhanced strength and fracture resistant properties.

36 MATERIALS SCIENCE↗

Microscopic analysis of copper current collectors and mechanisms of fragmentation under compressive forces

Extensive fragmentation of copper current collectors was observed after spherical indentation on prismatic and large-format pouch Li-ion cells by 3D X-ray computed tomography (XCT). Microscopic analysis including scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) and x-ray photoelectron microscopy (XPS) was carried out on copper current collectors from used commercial cells and pristine anodes. The copper-graphite cross-section images showed rough interface areas affected by reactions and diffusion in the used cell. Electron probe micro-analyzer (EPMA) element mapping showed the interface area was rich in oxygen and phosphorus. A detectable amount of phosphorus was also uniformly distributed inside the current collector. The same oxygen and phosphorus distributions were confirmed by STEM/EDS analysis. XPS depth profiles on multiple elements revealed the interface area of the aged anode was rich in Li, F, P, O and C and diffused at least 50 nm into the copper. In comparison, the pristine anode showed a very smooth C/Cu interface. No other elements were detected. For commercial cells, the reactions in the interface area and diffusion of multiple elements into the lattice and grain boundaries were responsible for the embrittlement of the copper current collectors. Finally, permanent cell capacity loss was observed in electrochemical performance of the indented cells.

36 MATERIALS SCIENCE↗

Microscopic vertical orientation of nano-interspaced graphene architectures in deposit films as electrodes for enhanced supercapacitor performance

This paper reported a novel two-step process to fabricate high-performance supercapacitor films that contain microscale domains of nano-interspaced, re-stacked graphene sheets oriented perpendicular to the surface of current collector substrate, i.e., carbon fiber paper. In the two-step process, we first used ligand molecules to modify the surface of graphene oxide (GO) sheets and manipulate the interspacing between the re-stacked GO sheets. The ligand-modified GOs, i.e., m-GOs, were then reduced to obtain more conductive graphene (m-rGO), where X-ray diffraction measurement results indicated well-controlled interlayer spacing between the restacked m-rGO sheets up to 1 nm. The typical lateral dimension of the restacked m-rGO sheets were ~40 µm. Then, electrical field was introduced during m-rGO slurry deposition process to induce the vertical orientation of the m-rGO sheets/stacks in the film deposit. The direct current electrical field induced the orientation of the domains of m-rGO stacks along the direction perpendicular to the surface of deposit film, i.e., direction of electric field. Also, the applied electric field increased the interlayer spacing further, which should enhance the diffusion and accessibility of electrolyte ions. As compared with the traditionally deposited “control” films, the field-processed film deposits that contain oriented structure of graphene sheets/stacks have shown up to ~1.6 times higher values in capacitance (430 F/g at 0.5 A/g) and ~67% reduction in equivalent series resistance. Finally, the approach of using electric field to tailor the microscopic architecture of graphene-based deposit films is effective to fabricate film electrodes for high performance supercapacitors.

36 MATERIALS SCIENCE↗

Enhancement of effective linear RF surface resistance of superconducting surfaces by microscopic topography

Minimization of Radio-Frequency (RF) dissipation on superconducting surfaces is of interest for many applications. A prominent one is the use of Superconducting RF (SRF) cavities for charged particle acceleration. In addition to our previous investigation which characterized the occurrence of high-field non-linear losses by microscopic surface topography, the topic of increased linear losses as a function of surface topographic character merits consideration. Surfaces with isotropic homogeneous surface topography may be well characterized by power spectral density (PSD) derived from systematic height measurements. PSD characterizations of representative niobium cavity surface treatments have been developed: Electro-Polishing (EP), Nano-Mechanical Polishing (NMP) and Centrifugal Barrel Polishing (CBP) A perturbation model based on PSD statistical analysis is used to calculate additional RF loss on these surfaces when superconducting. The model assesses the penetration depth effects for a superconductor. We thus estimate the RF power dissipation ratio between these rough surfaces and an ideal smooth surface.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Polarization control at the microscopic and electronic structure observatory

The new Microscopic and Electronic Structure Observatory (MAESTRO) at the Advanced Light Source (ALS) in Berkeley provides X-rays of variable polarization, produced by an elliptically polarized undulator (EPU), for angle resolved photoemission (ARPES) and photoemission electron microscopy (PEEM) experiments. The interpretation of photoemission data, in particular of dichroism effects in ARPES, requires the precise knowledge of the exact polarization state. Numerical simulations show that the first harmonics of the EPU at MAESTRO provides soft X-rays of almost 100% on axis polarization. However, the higher harmonics as well as the downstream optical elements of the beamline, have a considerable impact on the polarization of the light delivered to the experimental end-station. Finally, employing a simple reflective polarimeter, the polarization is characterized for variable EPU and beamline settings and the overall degree of polarization in the MAESTRO end-stations is estimated to be on the order of 83%.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Electron Microscopic Evaluation and Fission Product Identification of Irradiated TRISO Coated Particles from the AGR-1 Experiment: A Preliminary Review

Post-irradiation examination of coated particle fuel from the AGR-1 experiment is in progress at Idaho National Laboratory and Oak Ridge National Laboratory. In this paper a brief summary of results from characterization of microstructures in the coating layers of selected irradiated fuel particles with burnup of 11.3% and 19.3% FIMA will be given. The main objectives of the characterization were to study irradiation effects, fuel kernel porosity, layer debonding, layer degradation or corrosion, fission-product precipitation, grain sizes, and transport of fission products from the kernels across the TRISO layers. Characterization techniques such as scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, and wavelength dispersive spectroscopy were used. A new approach to microscopic quantification of fission-product precipitates is also briefly demonstrated. Microstructural characterization focused on fission-product precipitates in the SiC-IPyC interface, the SiC layer and the fuel-buffer interlayer. The results provide significant new insights into mechanisms of fission-product transport. Although Pd-rich precipitates were identified at the SiC-IPyC interlayer, no significant SiC-layer thinning was observed for the particles investigated. Characterization of these precipitates highlighted the difficulty of measuring low concentrations of Ag in precipitates with significantly higher concentrations of Pd and U. Different approaches to resolving this problem are discussed. An initial hypothesis is provided to explain fission-product precipitate compositions and locations. No SiC phase transformations were observed and no debonding of the SiC-IPyC interlayer as a result of irradiation was observed for the samples investigated. Lessons learned from the post-irradiation examination are described and future actions are recommended.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The microscopic model of BiFeO 3

Many years and great effort have been spent constructing the microscopic model for the room temperature multiferroic BiFeO 3 . However, earlier models implicitly assumed that the cycloidal wavevector q was confined to one of the three-fold symmetric axes in the hexagonal plane normal to the electric polarization. Because recent measurements indicate that q can be rotated by a magnetic field, it is essential to properly treat the anisotropy that confines q at low fields. Here, we propose that the anisotropy energy $–K_3S^6$ sin$^6θ$ cos $6ϕ$ confines the wavevectors q to the three-fold axis $ϕ=0$ and $±2π/3$ within the hexagonal plane with $θ=π/2$.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Microscopic Self-consistent Study of Neon Halos with Resonant Contributions

Recent reaction measurements have been interpreted as evidence of a halo structure in the exotic neutron-rich isotopes 29,31Ne. While theoretical studies of 31Ne generally agree on its halo nature, they differ significantly in their predictions of its properties and underlying cause (e.g., that 31Ne lies in an "island of inversion'"). We have made a systematic theoretical analysis of possible Neon halo signatures -- the first using a fully microscopic, relativistic mean field approach that properly treats positive energy orbitals (such as the valence neutron in 31Ne) self-consistently with bound levels, and that includes the pairing effect that keeps the nucleus loosely bound with negative Fermi energy. Our model is the analytical continuation of the coupling constant (ACCC) method based on a relativistic mean field (RMF) theory with Bardeen-Cooper-Schrieffer (BCS) pairing approximation. We calculate neutron- and matter-radii, one-neutron separation energies, p- and f-orbital energies and occupation probabilities, and neutron densities for single-particle resonant orbitals in 27-31Ne. We analyze these results for evidence of neutron halo formation in 29,31Ne. Our model predicts a p-orbit 1n halo structure for 31Ne, based on a radius increase from 30Ne that is 7 - 8 times larger than the increase from 29Ne to 30Ne, as well as a decrease in the neutron separation energy by a factor of ~ 10 compared to that of 27-30Ne. In contrast to other studies, our inclusion of resonances yields an inverted ordering of p and f orbitals for small deformations. Furthermore, we find no evidence of an s-orbit 1n halo in 29Ne as recently claimed in the literature.

exotic nuclei↗

Enhanced phase contrast transfer using ptychography combined with a pre-specimen phase plate in a scanning transmission electron microscope

We report the ability to image light elements in both crystalline and noncrystalline materials at near atomic resolution with an enhanced contrast is highly advantageous to understand the structure and properties of a wide range of beam sensitive materials including biological specimens and molecular hetero-structures. This requires the imaging system to have an efficient phase contrast transfer at both low and high spatial frequencies. Here, we introduce a new phase contrast imaging method in a scanning transmission electron microscope (STEM) using a pre-specimen phase plate in the probe forming aperture, combined with a fast pixelated detector to record diffraction patterns at every probe position, and phase reconstruction using ptychography. The phase plate significantly enhances the contrast transfer of low spatial frequency information, and ptychography maximizes the extraction of the phase information at all spatial frequencies. In addition, the STEM probe with the presence of the phase plate retains its atomic resolution, allowing simultaneous incoherent Z-contrast imaging to be obtained along with the ptychographic phase image. An experimental image of Au nanoparticles on a carbon support shows high contrast for both materials. Multislice image simulations of a DNA molecule shows the capability of imaging soft matter at low dose conditions, which implies potential applications of low dose imaging of a wide range of beam sensitive materials.

36 MATERIALS SCIENCE↗