一般財団法人材料科学技術振興財団　MST List of Products and Services

XRR measures the reflection intensity of X-rays incident on the sample surface at a very shallow angle. By comparing the reflection X-ray intensity profile obtained from this measurement with simulation results and optimizing the simulation parameters, this method determines the film thickness and density of the sample. - Evaluation of film thickness is possible (approximately 2 to 300 nm) - Evaluation of density is possible - Evaluation of surface roughness is possible (Rms ≤ 5 nm) - Non-destructive analysis is possible - Average information over a wide area of approximately 10×20 mm can be obtained

- Identification of crystalline substances is possible - Evaluation of crystal size (from a few nm to 100 nm) is possible - Evaluation of crystallinity is possible - Evaluation of orientation is possible - Evaluation of strain and stress is possible - Non-destructive analysis is possible Features of the equipment - Heating analysis is possible from room temperature to 1100°C - Micro-area measurement with a beam diameter of up to 100 μm is possible - Atmosphere control is possible with N2, He, Ar, and vacuum

SAXS is an analytical method that measures the X-rays scattered by a substance when X-rays are irradiated onto it, specifically in the low-angle region where 2θ < 10°. It is used to evaluate the structure of materials. Typically, it can assess structures ranging from a few nanometers to several tens of nanometers in size. - Enables evaluation of periodic structures and orientation at the nanoscale - Allows assessment of the distribution of voids in fine particles and materials - Capable of evaluating biological materials such as proteins - Allows for evaluation of samples under heating

Rietveld analysis is a method for analyzing measurement data from XRD (X-ray diffraction) and neutron diffraction. In addition to identifying lattice constants and space groups using existing methods, it is possible to obtain more detailed crystallographic information, such as atomic arrangements within the unit cell, if there is a crystal structure model (candidate) for the sample.

Antimicrobial coatings and coated everyday items aimed at infection prevention, mold prevention, and odor control have become widely popular. Among them, silver ions (Ag) are known to exhibit antibacterial and sterilizing effects against bacteria and viruses, while being almost harmless to the human body, making them widely used as inorganic antimicrobial agents. We will introduce a case study that focused on the presence of Ag as an antimicrobial component on the sample surface and evaluated the presence and durability of the antimicrobial coating film.

It is also referred to as HX-PES or HXPES. Due to high-energy X-ray excitation, it allows for bulk state evaluation up to approximately 50 nm deep, which is several to about 10 times deeper than conventional XPS, as well as damage-free evaluation of bonding states at interfaces. This device is a laboratory instrument equipped with a GaKα source (9.25 keV), which enables a reduction in the time lag from sample preparation to measurement. - Bulk-sensitive state evaluation (approximately up to 50 nm) - Non-destructive evaluation of buried interface bonding states - Evaluation using deep inner shell orbitals (avoiding overlapping Auger peaks in XPS, analysis using the non-split 1s orbital) It also includes options for measurements combined with sputtering using GCIB (Gas Cluster Ion Beam), angle-resolved measurements, Al source (1.49 keV), neutralization guns, and measurements under non-exposure to the atmosphere. - Damage-free sputter cleaning using GCIB (depth profiling is generally not possible) - Depth-direction comparison of bonding states using Al source and angle-resolved measurements - Evaluation under non-exposure to the atmosphere

Tensile Test It is possible to perform X-ray CT measurements while applying stress in the direction of pulling the sample. Compression Test It is possible to perform X-ray CT measurements while applying pressure in the direction of compressing the sample. Temperature Control It is possible to perform X-ray CT measurements while adjusting the temperature of the stage.

Soft X-ray emission spectroscopy (SXES) using synchrotron radiation is widely used as a method to evaluate the electronic states of materials, as it allows for the direct acquisition of the partial density of states (pDOS) near the Fermi level for each element constituting the material. Furthermore, the characteristics of this method include: 1. Information from the bulk can be obtained. 2. It can be evaluated without being affected by charging effects, even for insulators. 3. The detection limit is low (<1 atomic%). These features make it particularly effective for evaluating materials containing light elements (such as B, C, N, O). In this document, we will introduce the SXES spectrum of a GaN substrate as a measurement example.

CFRP (Carbon Fiber Reinforced Plastic) is a resin material that uses carbon fibers as a reinforcing material, characterized by its lightweight and high strength and rigidity. The internal fiber structure of CFRP was observed using X-ray CT. As a result, we were able to observe clusters of carbon fibers with a diameter of approximately 7 μm, and we also conducted an analysis of the fiber orientation.

This document presents a case study of Rietveld analysis applied to the powder X-ray diffraction data of Li(Ni, Mn, Co)O2, which is used as a positive electrode active material in lithium-ion secondary batteries. By seeking a crystal structure model that reproduces the measured powder X-ray diffraction data through simulation, it is possible to precisely calculate crystal structure parameters such as lattice constants, site occupancy rates, and the proportion of cation mixing, which can then be used to discuss the material properties.

Polyimide has very high heat resistance and excellent electrical insulation and mechanical properties, making it an essential material not only for electronic components but also for a wide range of fields such as precision machinery, automobiles, and aerospace. In its reliability evaluation, research on imide bonds is important. This document presents an example of XPS measurements conducted on polyimide before and after heating. Changes in the amount of oxygen and the chemical shifts of carbon, nitrogen, and oxygen confirmed that imidization progressed after heating. Additionally, by performing waveform analysis, it is also possible to determine the proportion of polyimide present.

Glass Fiber Reinforced Plastics (GFRP) are inexpensive, lightweight, and high-strength materials. Understanding their components, distribution, and internal structure is an important aspect of product design. This document presents case studies evaluating the components and structure of GF-reinforced PEEK (Poly Ether Ether Ketone) as GFRP material, as well as the degradation components of the resin after UV exposure.

The segregation of components and the formation of films on the surface of the positive electrode of lithium-ion secondary batteries are factors that influence the electric capacity. We will introduce a case study on Li(NiCoMn)O2 (NCM), which is used as a positive electrode, where micro-region mapping was conducted using AES, and qualitative analysis of organic components (binder) and active material surface films was performed using XPS and TOF-SIMS. These methods allow for analysis with a series of treatments conducted under an Ar atmosphere, which helps to suppress the alteration of the sample.

In lithium-ion secondary batteries, Li(NiCoMn)O2 (NCM) used as the positive electrode can achieve higher capacity by increasing the Ni ratio, and it also excels in high-temperature storage, making it suitable for mass production for automotive applications. On the other hand, cation mixing, where Ni ions occupy Li sites, is considered one of the factors contributing to the degradation of secondary batteries. This presentation will introduce a case where the metal content of the positive electrode active material was evaluated using ICP-MS, the crystal structure was assessed using XRD, and the results were used to perform Rietveld analysis to evaluate the proportion of cation mixing.

Next-generation all-solid-state batteries, which are lithium-ion batteries, are expected to have high safety, high energy density, high output, and a wide operating temperature range. In recent years, research and development aimed at practical application has been actively conducted, but there are various development challenges. At MST, we propose evaluation content suitable for solving development challenges based on comprehensive analysis and evaluation of structure, composition, and electrical properties. This document introduces specific examples of development challenges for all-solid-state batteries, their evaluation content, and representative evaluation methods for each component.

This document presents an example of evaluating organic contamination through bonding state mapping using XPS. This bonding state mapping is obtained by acquiring XPS spectra of the element of interest at several hundred points within the plane and plotting the distribution of peak intensities corresponding to the energy positions of specific bonding states. Depending on the size of the area of interest, evaluation areas can be set to arbitrary sizes ranging from approximately 1mm to 20mm square, making it particularly suitable for assessing contamination, discoloration, and surface treatments on the order of millimeters. Similar evaluations can also be conducted for metals and silicon, in addition to carbon.

The frequency of mask usage has increased to prevent infections caused by viruses, but there is a lack of structural data that serves as a basis for their usage methods and resistance. This document presents the results of an analysis of non-woven masks before and after use using X-ray CT. The analysis revealed that the thickness of the entire mask increased after use, and it was found that sparse areas in the fibers developed within the layers of the non-woven fabric. It is expected that after use, masks may become more susceptible to the infiltration of dust and that the capture of dust fibers may become less effective.

This is an example of wide-area quantitative mapping using XPS. We evaluated organic residue on silicon wafers using the following procedure. To graph the amount (atomic concentration) rather than peak intensity, it is less affected by sample roughness and allows for data acquisition over a wide area. It is suitable for investigating organic and inorganic contamination, discoloration, surface treatments, etc., as it enables an overview assessment of the compositional distribution on the sample surface.

The inner walls of metal pipes, such as SUS, used in various fields can discolor and corrode due to reactions with incoming gases and liquids, leading to a decline in equipment functionality. Understanding the locations prone to discoloration and corrosion, as well as their causes, is an important issue in equipment maintenance. At MST, we provide a comprehensive evaluation from sample cutting to analysis. This document presents a case study of XPS analysis conducted on the inner walls of SUS pipes used in vacuum equipment, highlighting both normal and discolored areas.

Tin (Sn), such as in solder, is used in many electronic components. In the XPS analysis of the Sn surface, by using the 4d orbitals in addition to the quantitative and state analysis typically performed with the 3d orbitals, it is possible to separate the oxidation states (divalent Sn2+ (SnO) and tetravalent Sn4+ (SnO2)) and calculate their ratios. Furthermore, by examining the valence band, it is possible to sensitively detect even a very small amount of the low oxidation state (divalent Sn2+ (SnO)). This document presents examples of evaluating Sn on the surface of solder using various orbitals.

The separator in lithium-ion secondary batteries not only serves the role of isolating the positive and negative electrodes to prevent internal short circuits, but in automotive batteries, it is also required to have heat resistance to prevent a decrease in strength or melting even in high-temperature environments. This report introduces a case study on separators used in overseas automotive batteries, where heat resistance and thermal decomposition behavior were investigated using TG-DTA, and structural and compositional evaluations were conducted using SEM-EDX, FT-IR, XPS, TOF-SIMS, and XRD. It was found that the separator used in the battery consists of a porous polyethylene and a layered structure of polygonal AlO(OH) aimed at heat resistance.

This article introduces a case study evaluating the surface morphology, cross-sectional structure, components, composition, crystal structure, and resistance value distribution of Li(NiCoMn)O2 (NCM), which is used as a positive electrode in lithium-ion secondary batteries. Based on a comprehensive evaluation of structure, composition, and electrical properties, MST proposes assessments suitable for solving development challenges aimed at improving characteristics and enhancing reliability.