Volume 38(1) - Winter 2022

X-ray emission spectroscopy (XES) is a chemical state analysis method. It is possible to show the change in a compound’s bonding state profile by measuring fluorescent X-rays with high energy resolution. Recently, the XES method has been evaluated in the field of advanced materials such as battery materials and catalysts, and the need for laboratory spectrometers is increasing. We are evaluating the applicability of Si-based negative electrode materials and next-generation battery materials for lithium-ion batteries using double-crystal spectroscopy with high-energy resolution. Quantitative analysis results of Li–Si alloy composition and side reaction products were reported based on changes in the Si Kβ spectral profile during electrochemical charging and discharging. It is known that the X-ray emission spectrum changes depending on the chemical state of the material, but the technique is not actively applied to chemical state analysis currently. In this paper, as the basis for describing the X-ray emission analysis method, we explain the optical system required to obtain high resolution, describe the interpretation of the X-ray emission spectrum and spectral changes due to the chemical state, and introduce application examples.

An essential feature of the qualitative analysis of the powder X-ray diffraction (PXRD) method is that this provides information on the sample’s crystal structure, which often affects the properties and functions of the material. The qualitative analysis by the PXRD method is a phase identification method based on the matching of known patterns (Card) in with measurement patterns. Tips in the phase identification procedure are the quality of the measurement data, the presence of trace phases, and the selection of card. In recent years, the performance of analysis software has been improved, and phase identification can now be done quickly and easily by a computer search. Since the results of computer searches are not always correct, analysts need to evaluate the validity of the analysis results themselves.

For the past 70 years, since the founding of our company in 1951, our management philosophy has been to “contribute to the enhancement of humanity through scientific and technological development.” By aligning ourselves with the enterprises and institutes pushing the boundaries of possibility over these seven decades, we have continuously expanded our portfolio of original technologies. These, in turn, help us in our efforts to contribute to the research and development of materials as well as the improvement of their performance and functionality.

I would like to express my sincere gratitude to our users and researchers for their guidance and support, which have enabled us to come this far as a manufacturer specializing in X-ray and thermal analysis in the fields of steel, nonferrous metals, cement, automobiles, and more recently, composite materials and lithium batteries.

In recent years, many countries have become increasingly concerned about environmental issues, and are accelerating their efforts to reduce their environmental impact by reducing dependence on fossil fuels (coal and oil) to achieve the carbon neutral. Developed countries and manufacturers are creating social policies and manufacturing strategies for low environmental load. Thus, the demand for advanced polymer materials has increased annually for use in products related to energy conservation, such as electric vehicles, fuel cells and biodegradable plastics. Structural control at the crystal structure scale (nanoscale) is one of the most important issues in their development and manufacturing of functional polymer materials for polymer electrolyte membranes for fuel cells, battery separators, biodegradable polymers, and bulk reinforced plastics, as well as films and fibers.

Wide-Angle X-ray Scattering (WAXS) / Wide Angle X-ray Diffraction (WAXD) is widely used for structural analysis of functional polymer materials. In particular, 2D-WAXS measurements using a two-dimensional (2D) detector are widely used for the identification of crystal structures, evaluation of selected orientations, and measurement of crystallinity of polymers. In general, the periodic structure of polymers has a spacing size of 0.2 nm to 1.8 nm, and diffraction peaks are observed in a scattering angle 2θ range between 5° and 45° when using Cu Kα radiation (λ=0.15418 nm). Therefore it is necessary to measure a wide region with a large scattering angle.

In this paper, we introduce the latest wide-angle X-ray scattering measurement system NANOPIX-WE. While NANOPIX is designed for advanced small-angle X-ray scattering measurements (SAXS), NANOPIX-WE is optimized for WAXS measurements, with a scattering angle of 2θ between 3° and 65°. Its high-intensity X-rays enable not only static measurements but also in situ measurements with controlled temperature and external fields, and high-speed time-resolved measurements. This new product has been developed to allow structural evaluation of polymeric materials such as films, fibers and bulk materials in various environments, but it can also perform 2D-WAXS measurements on inorganic materials such as powders and metallic materials.

3D electron diffraction (3D ED)/Micro electron diffraction (MicroED) is a technique that can provide measurers with three-dimensional molecular structures from crystals of submicron order. However, 3D ED/Micro ED requires expertise in both electron microscopy and crystallography. Here, we introduce the newly developed electron diffractometer XtaLAB Synergy-ED specialized for 3D ED/MicroED experiments, its instrument configuration, measurement flow, and measurement examples.