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

TOF-SIMS and MALDI-MS, which are representative mass spectrometry methods for solid sample surfaces, both enable qualitative analysis and imaging analysis. TOF-SIMS, which utilizes hard ionization methods, can detect inorganic and organic components with masses up to several hundred with high sensitivity. On the other hand, MALDI-MS, which employs soft ionization methods, can detect polymers in the range of thousands to tens of thousands. Additionally, the spatial resolution of the images also varies depending on the diameter of the irradiation beam.

The electrolyte of lithium-ion secondary batteries can be qualitatively and quantitatively analyzed using GC/MS. In the example below, ethylene carbonate (EC) and ethyl methyl carbonate (EMC) were identified as organic solvents, and vinylene carbonate (VC) was identified as an additive. It is also possible to determine the composition ratio of the solvents and the content of the additives. Additionally, other additives such as fluoroethylene carbonate (FEC) and ethylene sulfite (ES) can also be evaluated.

The characteristics and reliability of lithium-ion secondary batteries are greatly influenced by materials, among which the impact of the electrolyte is said to be significant. Commercial products in various shapes, such as cylindrical and laminated types, can have their electrolytes extracted using appropriate methods, allowing for the identification of organic solvents and additives. The following case involves extracts from prismatic batteries, confirming the use of ethylene carbonate (EC), ethyl methyl carbonate (EMC), and diethyl carbonate (DEC) as organic solvents, and fluoroethylene carbonate (FEC) as an additive.

Adhesive tapes are used for a wide range of applications, including everyday household uses, as well as in medical, construction, and insulation purposes. The adhesives used for these tapes vary depending on their application, and various materials are employed. This case study introduces an example of structural analysis of the adhesives in commercially available adhesive tapes using thermal decomposition GC/MS method. Measurements of three types of tapes revealed that they each used different materials: acrylate-based, styrene/isoprene-based, and silicone-based.

The surface of the hair cuticle is covered with a lipid called 18-MEA (18-methyl eicosanoic acid). 18-MEA is said to be the source of hair shine and smoothness, and when it decreases due to UV rays or hair coloring, the cuticle becomes more susceptible to damage. In this case, we will present the results of evaluating the differences in 18-MEA on the surfaces of healthy hair (hair near the root that has not been treated with hair color) and damaged hair (hair that has been treated with hair color) using TOF-SIMS.

We created skin tissue samples and evaluated the distribution of biogenic components in freeze-dried samples using TOF-SIMS. Since TOF-SIMS identifies components based on the mass of molecular ions, it does not require labels such as fluorescent substances, allowing for the evaluation of distribution without the influence of labeled materials. The mapping results confirmed that arginine, a natural moisturizing factor (NMF), and cholesterol, which retains moisture as an intercellular lipid, are localized in the stratum corneum. This method is also effective for assessing the permeation state during drug application.

IGZO thin films, which are transparent oxide semiconductors, are being researched and developed as TFT materials for displays. IGZO is a material whose properties change based on the composition of the thin film and the amount of impurities within it, making it important to obtain information about the composition and impurities. This time, we will introduce a case where the main components and the amounts of metallic impurity elements in IGZO powder, the raw material for the thin film, were evaluated with high precision using ICP-MS. Analysis is possible not only for powders but also for bulk and thin films.

We analyzed the surface components of three types of commercially available food wrap films (A, B, C) using TOF-SIMS. In this document, we focused on the outermost surface of the wrap films, as shown in Figure 1.

Resveratrol is a type of polyphenol and a substance that has garnered attention as a natural antioxidant. Resveratrol, which is abundant in grape skins, is also present in red wine made from whole grape skins. This document presents an analytical case in which the amount of resveratrol in three types of commercially available red wine was measured and compared using the LC/MS/MS method.

UV-curable resins harden quickly when exposed to ultraviolet light and are widely used as coating materials and adhesives due to their ease of use. In acrylate resins, which are commonly used materials, the molecular ions of acrylate monomers are difficult to detect using the conventional ionization method of EI in GC/MS analysis, leading to insufficient structural estimation. Here, we introduce a case where, in addition to the partial structural information obtained from the conventional EI method, the use of the soft ionization method FI enabled the detection of molecular ions, allowing for the estimation of the structure of acrylate monomers.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.