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

The electrolyte used in lithium-ion batteries is generally composed of a solvent and an electrolyte salt, and is considered a homogeneous system on a macroscopic scale. However, from a microscopic perspective, phenomena such as solvation occur. Understanding the local structure of lithium-ion solvation and the reactions that occur when inserting into the positive and negative electrodes is important for the design of high-performance battery materials. This document presents a case study that evaluates the microscopic structure of lithium-ion solvation in the electrolyte of lithium-ion batteries using molecular dynamics simulations.

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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.

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The electrical, optical, and magnetic properties of semiconductors are strongly influenced by defects and impurities present in the system. Therefore, to achieve the desired material properties, it is necessary to understand and control the behavior of defects and impurities. However, evaluating atomic-level microscopic behavior through experimental methods is challenging, making approaches using computational simulations effective. This document presents a case study using first-principles calculations with the NEB (Nudged Elastic Band) method to evaluate the diffusion pathways and barriers of metal impurities (Fe) in silicon crystals.

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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.

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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.

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Thermally stable α-alumina is used in a wide range of applications, including heat-resistant materials, semiconductor packages, and components of semiconductor manufacturing equipment. Among these, dense α-alumina is also used as a material for vacuum devices. However, the gases generated when such materials are heated can adversely affect products and equipment, making it important to understand the outgassing from these materials. In this report, we present a case study comparing the outgassing amounts of porous and dense α-alumina using TDS analysis (temperature-programmed desorption gas analysis).

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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.

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High-resolution HAADF-STEM images reflect the atomic arrangement of crystals, and by simulating STEM images corresponding to various crystal orientations, they help in accurately understanding the relative orientations between crystal grains and the observed images in polycrystalline materials. This document presents a case where STEM images were simulated from the crystal orientation information obtained by the EBSD method for the crystal grains in a polycrystalline neodymium magnet, and compares them with actual high-resolution HAADF-STEM images.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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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.

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The separator, which is a key component material of batteries, influences the characteristics and safety of the battery due to its porosity, shape, and other factors. Currently, mainstream polymer materials such as polyethylene (PE), polypropylene (PP), or their composite materials have low softening points, with PE being around 125°C and PP around 155°C. We will introduce a case where the structure of a PP separator with a low softening point was observed, and cooling was performed during cross-section processing to suppress degradation for evaluation.

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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.

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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.

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NMR is typically performed using the resonance signals of deuterium (2H or D) nuclei in deuterated solvents for reasons such as ensuring the stability of the magnetic field. However, by using the resonance signals of proton (1H) nuclei, measurements can also be conducted with light solvents (i.e., regular solvents) (No-D measurement method). The effective measurements for the No-D method are as follows: - Measurements to evaluate interactions with light solvents (e.g., degradation studies in light solvents) - Measurements of samples that cannot use deuterated solvents (e.g., samples in the biochemical field such as proteins) - Measurements of samples containing volatile components - Measurements of samples for which no dissolvable deuterated solvents are available.

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- Phosphorescence has a longer lifespan compared to fluorescence, and it often becomes thermally deactivated due to quenching by oxygen or the motion and collisions of solvents, making it difficult to measure at room temperature in most cases. Therefore, phosphorescence measurements are generally conducted at low temperatures. The fluorescence spectrometer owned by MST can cool samples to liquid nitrogen temperatures, allowing for phosphorescence measurements. - To perform phosphorescence measurements, it is necessary to measure the emission lifetime of phosphorescence and appropriately set the opening and closing time of the shutter integrated into the device based on the results. By establishing suitable measurement conditions, it is possible to distinguish and observe phosphorescence from fluorescence. This document explains the measurement of phosphorescence emission lifetime and phosphorescence measurements.

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In HAXPES, hard X-rays (Ga radiation) are used for excitation, which results in different positions of the Auger peaks compared to the Al and Mg radiation typically used in standard XPS measurements. Therefore, even in samples where the photoelectron peaks and Auger peaks overlap in Al and Mg measurements, this overlap can be avoided in Ga measurements, allowing for a detailed evaluation of the bonding states. This document presents the spectra of Kovar (an alloy of Fe, Ni, and Co) and GaN measured using Ga radiation (equipped with HAXPES) and Al and Mg radiation (equipped with XPS).

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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.

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Environmental Testing Evaluates the resistance of electronic components and devices when subjected to environmental stress. Reliability Evaluation Testing Assesses items related to the reliability and safety of the product.

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The probe tip made of SiO2 is coated with Pd, and the probe itself acts as a resistive element. Therefore, when current flows through the probe tip, a temperature rise occurs, and when it comes into contact with the sample surface, the sample absorbs the heat from the probe. To maintain a constant probe temperature, the amount of electricity supplied to the probe is adjusted, and by plotting the changes in the supplied electricity at each measurement point, the thermal conductivity of the measurement locations (for each material) is visualized as a distribution.

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The Corona Charged Aerosol Detector (CAD) shows almost identical area values for different components if they are at the same concentration under the same analytical conditions. In gradient separation, the organic solvent composition when each component reaches the detector differs, leading to changes in sensitivity; however, this can be corrected using a reverse gradient system. Semi-quantification can be performed using calibration curves created from different components, allowing for the estimation of the quantity of components without standard samples.

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The Corona Charged Aerosol Detector (CAD) detects components after they have been separated by HPLC and nebulized, followed by solvent removal. Therefore, volatile substances cannot be detected, but everything else is subject to detection. In CAD, particles are given a charge, and by measuring the amount of that charge, an area value corresponding to the amount of the component is obtained. In the case of a UV detector, the area value can vary significantly depending on the component, even at the same concentration, but in CAD, the difference in area values is about 10%. 1. Non-volatile and semi-volatile substances can be detected even if they do not have UV absorption. 2. Consistent responsiveness is obtained depending on the weight of the substance, allowing for semi-quantitative analysis even without standard samples. 3. High sensitivity detection is possible regardless of chemical structure (detection limits are around several hundred pg to several ng). 4. Gradient analysis is possible.

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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.

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Analysis targets (Information such as composition and crystal structure is required for calculations) ? The main analysis targets are systems with periodicity, such as crystals. ? Calculations for systems with amorphous structures, surfaces, and interfaces are also possible. Obtained physical property information ? Crystal structure parameters (lattice constants, atomic arrangements, etc.) ? Electronic structure and spin states (charge distribution, band structure, Fermi surface, magnetic moments, etc.) ? Chemical bonding states such as covalent bonds and ionic bonds ? Stable structures and defect formation energies when lattice defects such as atomic substitutions and vacancies are present ? Formation energies and atomic arrangements of surfaces and interfaces ? Information related to chemical reactions, such as activation energies and structures of intermediates ? Electronic response characteristics such as dielectric functions, electrical resistivity, and Seebeck coefficients ? Thermodynamic quantities of solids, such as specific heat ? Various spectroscopic spectra (XPS, XAFS, etc.)

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It achieves high positional accuracy and wide-area cross-section production, making it usable as a new large-capacity analysis application. Even small structures within a large area can be targeted for processing, enabling wide-area structural analysis.

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Among the various forms of medication, tablets are widely used, but not much is known about the state of each component within them. To gain insights into the distribution of active ingredients within tablets, we conducted TOF-SIMS analysis on the cross-section of commercially available cold medicine tablets. In the outer layer of the tablet, SiO2, presumed to be derived from lubricant components, was detected almost uniformly, while inside, the active ingredients acetaminophen, anhydrous caffeine, dl-methyl ephedrine, and noscapine were found to be dispersed in different areas.

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The gas chromatography time-of-flight mass spectrometer (GC-TOF MS) allows for the acquisition of precise mass information by using a time-of-flight mass spectrometer to detect components separated by GC. Compared to the integer mass information obtained from a typical quadrupole mass spectrometer, the accuracy of qualitative analysis is improved. Additionally, it is equipped with various ionization methods; the hard ionization method, EI, provides partial structural information, while the soft ionization method, FI, yields molecular weight information. By combining different ionization methods, the range of analytes that can be qualitatively analyzed is expanded. Furthermore, it is also possible to directly introduce samples into the ionization chamber, allowing for the evaluation of samples that are difficult to introduce via GC, such as thermally unstable substances and non-volatile compounds.

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EI method: It is capable of detecting both inorganic and organic compounds, making it suitable for initial qualitative analysis. PI method: It allows detection while maintaining the molecular structure through soft ionization.

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In molecular dynamics simulations, the motion of particles (atoms and molecules) is simulated by applying Newton's equations of motion to individual particles, and the physical properties of the system are calculated based on statistical thermodynamics, along with evaluating the response and dynamics to external fields such as temperature and pressure. The results obtained are effective for predicting the structure and properties of materials and contribute to solving problems in research and development involving materials engineering and molecular biology.

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? High-speed sample processing is possible with pico-second pulse lasers. ? Light-transmitting samples such as glass can also be processed.

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- Possible to identify high resistance abnormal areas - The current flowing through the wiring is weak (pA) - Measurement is possible even with a surface protective film present - Measurement is possible even with multilayered wiring - Measurement is possible under conditions almost identical to SEM observation

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There are mainly three types of dyes, which are used according to the observation target. - Osmium tetroxide (OsO4) It selectively reacts with the unsaturated polymer material's ?CH=CH- (double bond). - Ruthenium tetroxide (RuO4) It cross-links with the amorphous parts of saturated polymer materials such as polyolefins. - Phosphotungstic acid (H3[P(W3O10)4]·xH2O, abbreviated as PTA) It reacts with polyamides and other materials containing the -CONH functional group.

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The IP method utilizes the sputtering phenomenon, where sample atoms are ejected from the sample surface when an ion beam with aligned energy and direction is irradiated onto the sample. It is also referred to as the CP method (Cross-section Polish). The ion species used is typically a noble gas (Ar in MST) that does not pose concerns for chemical reactions with the sample. In the AES analysis of the processed surface, the components of the shielding plate (Ni, P) were below the detection limit. ■Features - Wide-area cross-section processing is possible (approximately 500μm to 1mm) - No impact from mechanical polishing damage - Minimal surface contamination - Non-exposure to the atmosphere, cooling processing is possible

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In secondary ion mass spectrometry (SIMS), due to phenomena such as surface roughness, the knock-on effect where atoms present on the surface are pushed inward by ion irradiation, and crater bottom roughness, it may not be possible to obtain sharp elemental distributions. To address this issue, the SSDP method (Back-Side SIMS) involves performing SIMS analysis from the substrate side (the back side) after thinning the sample. This technique allows for a more accurate evaluation of elemental distribution without being affected by the sample shape or measurement conditions.

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TG-DTA-MS continuously evaluates not only TG and DTA but also the volatile components (MS). - TG allows for the detection of weight changes on the order of percentage. - DTA provides insights into reactions such as pyrolysis, melting, sublimation, oxidation, combustion, and phase transitions. - MS enables the structural estimation of volatile components and decomposition products.

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Fitting is performed using various computational models on the force curve, which is an AFM measurement technique, to obtain elastic and viscoelastic data. ? Data can be measured in micro-regions that are consistent with DMA testing machines and nanoindenters. ? Applicable to materials with various hardness ranging from 10 kPa to 100 GPa. ? Fitting is possible using elastic models (DMT, Hertz, JKR) and viscoelastic models. ? Elastic modulus and viscoelastic modulus mapping can be performed using the above models. ? Frequency dependence (0.1 to 20 kHz) can be evaluated at each analysis point. ? Measurements can be conducted with temperature changes (room temperature to 250°C).

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O-PTIR has the following features: - It allows for spectral and image measurements in small areas due to its spatial resolution (maximum spatial resolution: less than 1μm). - No need for thin sectioning (effective for samples that are difficult to thin section, such as foreign materials). - Measurements can generally be performed non-destructively. - Similar analyses can be performed using the FT-IR library.

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This method allows for simultaneous measurement of the sample's surface roughness and mechanical property distribution, as well as infrared absorption images (functional group distribution) at selected absorption bands, by conducting measurements in conjunction with the AFM system. AFM-IR has the following features: - It enables evaluation with very high spatial resolution (on the nanoscale), allowing for spectral and imaging measurements in small areas. - Similar analyses can be performed by using the FT-IR library.

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Rubber products contain various additives such as vulcanization accelerators, antioxidants, plasticizers, and lubricants. This document presents case studies of the analysis of additives found in commercially available rubber products. After immersing the rubber in an organic solvent, the resulting solution was analyzed using LC/MS/MS, revealing the presence of several additive components, including N-(1,3-dimethylbutyl)-N'-phenyl-1,4-phenylenediamine, which is commonly used as an antioxidant. By conducting LC/MS/MS analysis, comprehensive qualitative analysis is possible.

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- MM (Machine Model) test: A test that simulates damage caused by the discharge of static electricity accumulated in metals and other materials. - HBM (Human Body Model) test: A test that simulates damage caused by the discharge of static electricity accumulated in the human body. - CDM (Charged Device Model) test: A test that simulates damage caused by the discharge of static electricity occurring when a charged conductor comes into contact with terminals of different potentials. - Latch-up test*: Evaluates the resistance to the phenomenon of latch-up, where excessive current continues to flow in devices with a parasitic thyristor structure. *Corresponds to pulse current injection method and power supply overvoltage method.

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