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

We offer composition distribution evaluation of ultra-thin films using ARXPS (Angle-Resolved X-ray Photoelectron Spectroscopy) (C0550). Photoelectrons emitted by X-ray irradiation are detected at different take-off angles, and spectra with varying detection depths are used to evaluate the depth profile very close to the sample surface. This method improves depth resolution and has the advantage of no compositional changes due to selective sputtering or mixing, making it effective for evaluating the depth profiles of ultra-thin films (on the order of a few nanometers) on substrates. [Measurement Method / Processing Method] ■ [XPS] X-ray Photoelectron Spectroscopy *For more details, please download the PDF or feel free to contact us.

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We offer quantitative analysis of glucosylceramide in konjac (C0491). Glucosylceramide is a type of glycosphingolipid found in food. It is included not only in cosmetics that are applied directly to the skin but also in health foods and general foods, such as supplements containing glucosylceramide, as well as various processed products and beverages. By using HPLC, it is possible to analyze the amount of glucosylceramide contained in raw crops and processed foods with high precision. [Measurement Method/Processing Method] ■ [HPLC] High-Performance Liquid Chromatography *For more details, please download the PDF or feel free to contact us.

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We offer the evaluation of the chemical state of RuO2 catalysts using in-situ XAFS (C0456). Under controlled conditions with gas atmospheres and temperatures tailored to the sample environment, it is possible to assess the chemical bonding state and local atomic structure of the sample. Therefore, it is suitable for cases where state evaluation is required in special environments, such as catalysts. In a case where RuO2 powder was heated from room temperature to 400°C under a reducing atmosphere using in-situ XAFS, it was confirmed from the shape of the spectrum that RuO2 is reduced to Ru between 100°C and 200°C. [Measurement Method / Processing Method] ■ [XAFS] X-ray Absorption Fine Structure *For more details, please download the PDF or feel free to contact us.

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We would like to introduce our spectral separation technology using the DOSY method. In NMR, when performing structural analysis of each component in a mixed sample, each component is typically isolated and purified before measurement. The DOSY method allows for the separation of spectra for each component by utilizing the differences in diffusion rates, enabling structural analysis of each component in a mixed sample without the need for isolation and purification. 【Features】 - Effective for measuring samples where physical separation by molecular weight is difficult - Effective for measuring samples that undergo structural changes during pretreatment (e.g., samples in the biochemical field such as proteins) - Facilitates structural analysis of each component by separating mixed spectra of multiple components - Provides insights into the mobility of molecules of each component in the mixture *For more details, please download the PDF or feel free to contact us.

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We will introduce a technique that emphasizes the signals of polymers or small molecules using a measurement method that utilizes the differences in relaxation times or diffusion coefficients of each component in a mixed sample. When electromagnetic waves are irradiated onto atomic nuclei in a static magnetic field, they absorb energy corresponding to the energy difference ΔE and enter an excited state (nuclear magnetic resonance). When the irradiation of electromagnetic waves is stopped, the process of returning to the original state is called relaxation, and the relaxation time is the time required for this process. The relaxation time is closely related to the mobility of the molecules. [Measurement Method / Processing Method] ■ [NMR] Nuclear Magnetic Resonance Analysis *For more details, please download the PDF or feel free to contact us.

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We offer NMR (Nuclear Magnetic Resonance Analysis) services. Since NMR directly observes nuclear spins, the area of the peaks of the measured nuclides obtained from the measurement is proportional to the number and concentration of the nuclides contained in the solution or solid being measured. Based on this principle, NMR allows for quantitative analysis without the need for a calibration curve. For example, using the integral value of the peak of the 31P nucleus, it is possible to determine the concentration of one component of a two-component mixture from the known concentration of the other component according to a relationship. [Measurement Method / Processing Method] ■ [NMR] Nuclear Magnetic Resonance Analysis *For more details, please download the PDF or feel free to contact us.

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We offer metal contamination analysis of Si wafers (B0233). The purpose of metal contamination analysis of Si wafer surfaces using ICP-MS includes not only the contamination assessment of the Si wafer itself but also the evaluation of contamination within semiconductor devices and the assessment of the working environment due to Si wafer exposure. Therefore, the analysis of Si wafer surfaces is conducted for various purposes. ICP-MS analysis allows for the highly sensitive measurement of metal contamination on Si wafer surfaces, and it is also possible to specify the evaluation area according to the purpose. [Measurement Method] ■ [ICP-MS] Inductively Coupled Plasma Mass Spectrometry *For more details, please download the PDF or feel free to contact us.

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Our organization has established a system that suppresses atmospheric exposure through atmosphere control, and further cools the samples for processing, observation, and analysis. We can produce TEM thin samples while maintaining the original structure of the specimen, allowing for observation and analysis. Even with unstable materials, we can perform thinning processing while cooling, and by maintaining a vacuum during the transfer between processing and observation devices, we enable cross-sectional TEM/SEM observation that minimizes atmospheric exposure and thermal alteration. 【Measurement and Processing Methods】 ■ [(S)TEM] Scanning Transmission Electron Microscopy ■ Processing under atmosphere control ■ Cryo-processing *For more details, please download the PDF or feel free to contact us.

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Control of particles in the semiconductor wafer manufacturing process is extremely important for ensuring wafer quality. In this case study, we estimated what the particles were on a Si wafer through SEM observation, EDX analysis, and simple quantification. The SEM equipment, which has high spatial resolution in the submicron range and can scan areas of several centimeters, allows for rapid inference of what the particles on the wafer are based on shape and composition information, enabling quick identification of the generation process. Analysis linked to coordinate data from defect inspection equipment is also possible.

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• Wafer
• Other semiconductor manufacturing equipment

Freon gases are utilized in various applications such as refrigerants, foaming agents, semiconductors, and cleaning agents for precision parts due to their chemically stable nature and minimal impact on human health. On the other hand, they are substances that contribute to ozone layer depletion and global warming, which is why they are regulated by law. In this case, Freon gases were analyzed using GC/MS, and the separation analysis of CF4, which has low polarity and is difficult to separate among PFCs, was conducted. By using GC/MS, it is possible to qualitatively analyze specific Freons such as CFCs, HCFCs, and alternative Freons like HFCs and PFCs.

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• Environmental Analysis

In situ X-ray CT measurements allow for internal structure analysis under conditions where a load (tension or compression) is applied to the sample. In this document, in situ X-ray CT measurements were conducted using an aluminum plate as the sample, both in its normal state and in an extended state. We calculated the tensile stress applied to the sample and monitored the internal structural changes under each stress condition. By combining in situ X-ray CT measurements with image analysis technology, it is possible to evaluate under actual usage conditions, which was previously difficult, and assess the impact of stress on the product.

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Impurities from components of the film formation device, target materials, and plating solutions can contaminate the device and have adverse effects, making the qualitative assessment of impurities on surfaces, within films, and at interfaces important. TOF-SIMS can sensitively evaluate unknown elements present on surfaces, within films, and at interfaces in a single measurement due to the following three characteristics: 1. For metallic elements, ions from m/z 1 to 800 can be detected simultaneously in one measurement. 2. Detection sensitivity of a few ppm can be achieved (varies depending on materials and ions). 3. The use of a sputter gun allows for the evaluation of depth distribution.

• Wafer
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• Other semiconductors

We have launched a new service using XPS/HAXPES starting in June! For increasingly complex materials and fine structure samples, we can evaluate the composition and chemical bonding states from the surface to the interior of the material (up to ~30nm) at the same location and in a non-destructive manner. - Depending on the elements of interest and the analysis area and depth, we can select the appropriate X-ray source (Al Kα/Mg Kα/Ga Kα/Cr Kα) to achieve evaluation under suitable measurement conditions. - Non-exposure measurements to the atmosphere, Ar monomer/GCIB sputter etching, and heating pretreatment can be combined. - It is possible to evaluate the electronic states of semiconductor samples using UPS/LEIPS (ionization potential/electron affinity/band gap).

• Secondary Cells/Batteries

- AI Model Development Based on collected data that includes the target object and publicly available open data, we will develop an AI model suitable for the conditions. By utilizing this AI model, it is expected that daily operations can be replaced by AI, promoting automation and efficiency in business processes and stabilizing accuracy. - Image/Data Analysis We analyze and evaluate images and other data. The evaluation content will be discussed with the client, and proposals will be made in line with the challenges. If the target is a product or material, analysis data can be obtained using MST.

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• Image Processing Software

Porous ceramics are lightweight and have low thermal conductivity due to their numerous pores, making them useful as insulation materials and filters. The structure of the pores directly affects the fluids passing through the porous ceramics, so capturing three-dimensional images and understanding numerical values such as porosity and specific surface area is important. This document presents a case study comparing the differences in porosity, specific surface area, and pore size distribution by conducting 3D structural observations using X-ray CT on two types of samples and analyzing the images.

• Ceramics
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• X-ray inspection equipment

TOF-SIMS has features such as simultaneous evaluation of organic and inorganic materials, capability for micro-area analysis, and high sensitivity for analyzing the very surface, making it effective for residue investigation in cleaning processes. An example is presented where pure water was dried on a silicon wafer. Optical microscopy only reveals slight point-like foreign substances and cloudiness. However, the results measured by TOF-SIMS showed that in the contaminated areas, organic components such as hydrocarbons, PDMS, and amides, which tend to adsorb naturally, were aggregated.

• Contract measurement
• Wafer
• Memory

There are various colored products made from paper used as wrapping paper, which contain diverse components. Since these coloring components can affect adhesion to contact materials and cause contamination, it is important to understand the components of the paper surface. This document presents a case study investigating the components of paper surfaces with different colors using TOF-SIMS.

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• Paper and pulp

MALDI-MS (Matrix-Assisted Laser Desorption Ionization Mass Spectrometry) is a method that allows for the detection and imaging of organic components in their molecular ion form. In particular, MALDI imaging is effective for evaluating the distribution of biological components and substances administered to living organisms in pharmacokinetic studies and pharmaceutical research and development. MST can provide a consistent process from sample preparation to measurement. This document presents an example of analysis where lipids were imaged using MALDI-MS, starting from the preparation of mouse brain slices.

• Contract measurement
• Animal cells
• Imaging and image analysis equipment

Perovskite solar cells are expected to be the next generation of solar cells due to their lightweight and flexible characteristics. They contain organic structures, halogens, and metals, and the variations in their composition and crystallinity lead to changes in their properties, which is considered one of the challenges in the research and development of perovskite solar cells. In this study, we evaluated the differences in photoluminescence (PL) spectra and luminescence lifetimes between the normal and abnormal areas of perovskite solar cells subjected to high-temperature and high-humidity testing using PL measurement and fluorescence lifetime measurement devices.

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The main components of wood biomass consist of cellulose, hemicellulose, and lignin, and their composition ratios vary depending on the plant species from which they originate. The composition ratios of these three components can be evaluated by applying specific chemical treatments such as the Klason method or the Wise method to the samples and measuring their weights. At MST, the proportion of the main components in wood biomass is calculated according to the following analysis flow.

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• wood

The SiON film used as the gate oxide film for Si transistors is formed by introducing nitrogen into the Si oxide film to suppress leakage current. To ensure a good interface characteristic with the substrate while maintaining the dielectric constant, it is necessary to strictly control the distribution of nitrogen in the SiON film. We will present a case study evaluating the distribution of silicon oxide and nitride in a 1nm thick SiON film using TOF-SIMS. TOF-SIMS has high depth resolution on the surface and can obtain molecular information with good sensitivity, allowing for a clear understanding of the compositional distribution in the ultra-thin SiON film.

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• Transistor
• Memory

Hyaluronic acid is a high molecular compound widely used in cosmetics and supplements. The characteristics, such as permeability to tissues, vary depending on the molecular weight, and there is a growing demand for low molecular weight hyaluronic acid in addition to high molecular weight hyaluronic acid. In electrophoresis, which is used for the analysis of polysaccharides, DNA, proteins, etc., the molecular weight distribution of hyaluronic acid can be visualized and evaluated by using a hyaluronic acid molecular weight marker with a known molecular weight. Here, we present analytical examples where high molecular weight hyaluronic acid is depolymerized by various methods and its molecular weight distribution is evaluated.

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Carbon nanotubes (CNTs) are lightweight and possess excellent mechanical properties (high strength and high elasticity), making them suitable for various applications and environments. In particular, the deformation behavior of CNTs is related to flexibility and energy absorption characteristics, which are important in sensor and nano-device design. This document presents a case study that simulates the bending and recovery deformation of single-walled CNTs using molecular dynamics calculations. The simulation allows for the observation of structural changes at the atomic level due to environmental changes (pressure and temperature), enabling the analysis of deformation behavior based on the changes in strain energy associated with these structural changes.

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Bacteria have various growth environments depending on their species, and there are many bacteria that are difficult to isolate and culture. Therefore, by extracting and analyzing DNA, which is the blueprint of life that all bacteria possess, it becomes possible to investigate the existing bacteria without isolation or culture. Here, we will introduce examples of analysis methods for sequencing bacterial DNA to infer the existing bacteria through microbiome analysis, as well as investigating bacterial numbers using real-time PCR methods.

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When heated, resin can emit organic substances, which may cause contamination depending on the usage environment. The GC/MS method using a gas concentration device is effective for the high-sensitivity analysis of organic outgassing. Here, we will introduce a case study of outgassing evaluation for resin used in 3D printers. Different types of resin are used for 3D printer materials depending on the intended use of the printed objects, varying in strength, color, heat resistance, and other properties. By conducting analysis using a gas concentration device, it is possible to compare trace amounts of outgassing components and quantities for resins with different properties.

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Multilayer ceramic capacitors (MLCCs) are capacitors designed to increase capacitance by layering ceramic dielectric and electrodes. The electrical properties of MLCCs are significantly affected by impurities, making the evaluation of impurities in the ceramic layers and the diffusion of electrode components important. With the miniaturization of MLCCs, the ceramic layers have become thinner, making it difficult to evaluate impurities. This document introduces the results of evaluating impurities in the ceramic layers by innovating the pretreatment process.

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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.

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The charge and discharge characteristics of lithium-ion secondary batteries are influenced by electronic conductivity. I will introduce a case where the decreased conductivity of active materials, due to degradation or blockage of conduction paths, was visualized as a resistance value distribution using SSRM. By comparing the results obtained from SSRM with the elemental distribution of Li and other elements measured by TOF-SIMS, it is possible to confirm the correlation between resistance values and elemental distribution. Additionally, it is feasible to classify conductive additives and binders based on resistance values, perform statistical processing, and quantify the mixing degree for each material.

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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.

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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.

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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.

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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.

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Due to the increased demand for disinfectant alcohol to prevent infections caused by viruses, it is important that the products do not contain methanol during handling. It is known that the components other than the main agent, ethanol, differ depending on the type of product. This document introduces cases where components other than ethanol were analyzed using chromatography. The analysis of four types of disinfectant alcohol products revealed that the components contained in the products varied.

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In anticipation of future demand for antimicrobial agents due to viral infections, this document presents the results of imaging antimicrobial agents and other components in antimicrobial coatings using TOF-SIMS. The antimicrobial coating was formed by spraying an antimicrobial spray containing Ag ions as the antimicrobial component onto a substrate. The analysis revealed that the amount of the antimicrobial component, Ag, did not change even after wiping or rinsing. It was also found that other components besides the antimicrobial agents were present.

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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.

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In the electrolyte of lithium-ion secondary batteries, a combination of high dielectric constant solvents and low viscosity solvents is used to improve electrical conductivity. Additionally, additives and electrolytes (supporting salts) not only facilitate the transport of Li ions but also have the function of forming a film on the electrode surface, requiring various performance characteristics. This paper presents examples of qualitative and quantitative analysis of various components such as solvents, electrolytes, and additives by evaluating the electrolyte itself using ICP-MS, volatile components during electrolyte heating using GC/MS, and the dry residue of the electrolyte using TOF-SIMS.

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The binder for lithium-ion secondary batteries not only serves as an adhesive between active materials but also needs to be insoluble in the electrolyte. Therefore, the selection of suitable materials for both the positive and negative electrodes is crucial. This document presents cases where the components of the binders used in each electrode sheet were identified by measuring the positive electrode binder using TOF-SIMS and the negative electrode binder using GC/MS, and then comparing the results with a materials library database.

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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.

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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.

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Resin materials such as adhesives may release gas components when heated, even after curing. If resin is present in manufacturing equipment, the released gas components can adversely affect the equipment or products, making it important to understand the outgassing components at the actual temperature and atmosphere in which the materials will be used. This case presents the results of analyzing the gas generated by heating epoxy-based adhesive after curing using headspace-GC/MS.

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Resins that excel in chemical resistance and electrical insulation are used as insulators, coatings, and adhesives for various electronic components. FT-IR (Fourier Transform Infrared Spectroscopy) can investigate the causes of defects such as the degree of curing of resins, making it effective for product development. As an example, we will introduce a case where the degree of curing of UV-curable resins was evaluated. It is effective for examining the UV exposure time in adhesives and assessing the curing state when delamination occurs in products.

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Resins (synthetic polymers) are polymers of monomers and have characteristic functional groups depending on their type. Due to their structure, they exhibit properties such as heat resistance, toughness, and electrical insulation, making them widely used in packaging materials, adhesives, paints, and more. Structural analysis is important for understanding the properties of resins, and common analytical methods include FT-IR and thermogravimetric GC/MS. FT-IR allows for the evaluation of functional groups, while thermogravimetric GC/MS enables the assessment of monomers and partial structures, so by combining these two methods, structural analysis of a wide variety of resins becomes possible.

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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.

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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.

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Many organic materials (resins) may discolor due to aging and other factors. The causes include the formation of conjugated double bonds within the polymer, the degradation of additives contained in the resin, and the transfer of surrounding substances, among others. When the degradation of additives is the cause, the responsible substances can be analyzed by elution using methods such as LC or GC. Here, we provide an overview of the causes of resin discoloration and analysis methods, and introduce a case where the coloring substances responsible for yellowing in polyurethane were separated by LC and qualitatively identified using a combination of PDA and MS.

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