X-ray topography is a powerful method for analyzing crystal defects and strain in crystalline materials non-destructively. However, conventional X-ray topography uses simple X-ray diffraction images, which means depth information on defects and dislocations cannot be obtained. We have therefor developed a novel three-dimensional micro-X-ray topography technique (3D μ-XRT) that combines Bragg-case section topography with focused sheet-shaped X-rays.
View Article and Find Full Text PDFAlthough various spectroscopic methods have been developed to capture ion-concentration profile changes, it is still difficult to visualize the ion-concentration profile and surface topographical changes simultaneously during the charging/discharging of lithium-ion batteries (LIBs). To tackle this issue, we have developed an scanning ion conductance microscopy (SICM) method that can directly visualize an ion-concentration profile and surface topography using a SICM nanopipette while controlling the sample potential or current with a potentiostat for characterizing the polarization state during charging/discharging. Using SICM on the negative electrode (anode) of LIBs, we have characterized ion-concentration profile changes and the reversible volume changes related to the phase transition during cyclic voltammetry (CV) and charge/discharge of the graphite anode.
View Article and Find Full Text PDFThe SAGA Light Source provides X-ray imaging resources based on high-intensity synchrotron radiation (SR) emitted from the superconducting wiggler at beamline 07 (BL07). By combining quasi-monochromatic SR obtained by the newly installed water-cooled metal filter and monochromatic SR selected by a Ge double-crystal monochromator (DCM) with high-resolution lens-coupled X-ray imagers, fast and low-dose micro-computed tomography (CT), fast phase-contrast CT using grating-based X-ray interferometry, and 2D micro-X-ray absorption fine structure analysis can be performed. In addition, by combining monochromatic SR obtained by a Si DCM with large-area fiber-coupled X-ray imagers, high-sensitivity phase-contrast CT using crystal-based X-ray interferometry can be performed.
View Article and Find Full Text PDFAn understanding of electrolyte stratification behaviours in lead-acid battery electrolytes during battery operation is important for optimal operation and design of lead-acid batteries for vehicle applications. In this paper, we present an in operando phase-contrast X-ray imaging technique for quantitatively visualizing electrolyte stratification dynamics that arise in electrolytes during battery operation.
View Article and Find Full Text PDFTo visualize the electrochemical reactivity and obtain the diffusion coefficient of the anode of lithium-ion batteries, we used scanning electrochemical cell microscopy (SECCM) in a glovebox. SECCM provided the facet-dependent diffusion coefficient on a LiTiO (LTO) thin-film electrode and detected the metastable crystal phase of LiFePO.
View Article and Find Full Text PDFUnderstanding the structure-property relationship of glass material is still challenging due to a lack of periodicity in disordered materials. Here, we report the properties and atomic structure of vanadium phosphate glasses characterized by reverse Monte Carlo modelling based on neutron/synchrotron X-ray diffraction and EXAFS data, supplemented by Raman and NMR spectroscopy. In vanadium-rich glass, the water durability, thermal stability and hardness improve as the amount of PO increases, and the network former of the glass changes from VO polyhedra to the interplay between VO polyhedra and PO tetrahedra.
View Article and Find Full Text PDFA fundamental understanding of concentrations of salts in lithium-ion battery electrolytes during battery operation is important for optimal operation and design of lithium-ion batteries. However, there are few techniques that can be used to quantitatively characterize salt concentration distributions in the electrolytes during battery operation. In this paper, we demonstrate that in operando X-ray phase imaging can quantitatively visualize the salt concentration distributions that arise in electrolytes during battery operation.
View Article and Find Full Text PDFJ Synchrotron Radiat
November 2011
Quick-scanning X-ray absorption fine structure (XAFS) measurements were performed in transmission mode using a PILATUS 100K pixel array detector (PAD). The method can display a two-dimensional image for a large area of the order of a centimetre with a spatial resolution of 0.2 mm at each energy point in the XAFS spectrum.
View Article and Find Full Text PDFTripodal molecules consisting of a tetrasubstituted adamantane with three phenylacetylene legs and a reversibly photoswitching apex were designed as "single molecular tips" for both chemical and topographical characterization of the substrate surface. By covalent attachment onto gold-coated AFM tips through three S-Au bonds, these rigid tripodal molecules are expected to act as sharp, robust, and stationary molecular tips whose configuration can be reversibly changed upon irradiation with UV or visible light. In this report, the full account of the syntheses of two photoswitching tripodal molecular tips, their immobilization onto Au(111) surfaces, and the detection of photoinduced configurational change on Au(111) surface by SPM measurements are documented.
View Article and Find Full Text PDFA tripod molecule with an azobenzene arm was designed as a single molecular tip for noncontact atomic force microscopy (NC-AFM). The azobenzene moiety showed photoisomerization that enabled measurements of the same position of the sample by different tip apexes with different interactions. Photoswitching behavior of the molecule synthesized and adsorbed on Au surfaces was examined and reversible switching between the trans- and cis forms was successfully confirmed by NC-AFM measurements.
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