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

Carbon materials, widely used in industrial components and medical devices, have different properties depending on their structure and crystallinity, making it important to evaluate their state. This document presents evaluation examples using high-sensitivity and high-spatial-resolution Raman spectroscopy. The distribution of the crystalline state of graphite, a carbon material, was visualized through mapping. It allows for a visual capture of the quantity of defects, whether high or low.

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- It is possible to quantify water in the range of several ppm to several percent. - Solid samples that do not dissolve in the electrolyte can also be quantified.

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- Compounds that are relatively low molecular weight and highly polar, such as organic acids, can also be analyzed. - Low polarity compounds, such as lipids, can also be analyzed. - By using the post-column method, it is possible to eliminate the effects of interfering components that could not be completely separated. - Quantification of polymers and measurement of molecular weight distribution are possible.

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Absolute PL quantum yield measurement is a method to determine the luminescence efficiency of a material, specifically how efficiently light (energy) absorbed by the material is converted into emitted light. - Since an excitation light source with a spectrometer is used, excitation at various wavelengths (approximately 350 to 800 nm) is possible. ■ Features of MST - The equipment is managed under controlled atmospheric conditions, allowing measurements of thin film samples without the influence of oxygen.

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Fluorescent dyes are used in commercial clothing, detergents, paints, etc., due to their effect of increasing apparent whiteness by absorbing ultraviolet light and emitting visible light (fluorescence). In this case study, we attempted to qualitatively analyze the fluorescent whitening agents contained in laundry detergents by connecting a fluorescence detector (FL) and a mass spectrometer (MS) to the liquid chromatography (LC). As a result, we were able to identify peaks that emit fluorescence from the numerous peaks detected by MS, and further estimation of the components was possible through the analysis of the MS spectra. By connecting FL and MS, it is possible to determine the presence of fluorescent components and estimate the components in a single measurement.

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GPC (Gel Permeation Chromatography) is one of the separation modes of HPLC and is a method for evaluating the molecular weight of polymer compounds. It can determine several average molecular weights (Mn), weight average molecular weight (Mw), and polydispersity (Mw/Mn) in a single analysis, and it is also possible to compare the distribution profiles. It is also referred to as SEC (Size Exclusion Chromatography).

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To understand the pharmacokinetics of drugs, it is important to know the concentration of drugs in body fluids. While blood is generally used for quantitative analysis of drugs absorbed into the body, recent years have seen a growing interest in the analysis of body fluids such as tears and saliva, which are less burdensome to collect than blood. At MST, it is possible to quantitatively analyze components contained in not only blood and urine but also tears and saliva with high sensitivity using LC/MS/MS. Below are examples of glucose analysis in tears and 5-fluorouracil analysis in saliva.

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AES analysis is a method for obtaining compositional information and elemental distribution at the very surface (to a depth of a few nanometers). By combining it with cross-sectional processing, similar information can also be obtained within layered structures and at structural interfaces. This allows for the evaluation of alloy layers, elemental diffusion, and segregation, making it effective for failure analysis and defect investigation of devices. Below, we present a case where a cross-section was prepared using IP processing to evaluate the state near the bonding interface of wire bonding, followed by assessment through AES analysis.

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IGBT (Insulated Gate Bipolar Transistor) is used in various products as a power semiconductor module, ranging from home appliances to industrial equipment. Lifetime control is implemented for performance improvement in IGBTs, but this control is achieved by creating defects (lifetime killers) in the drift layer. By conducting low-temperature micro-PL analysis from the cross-section, it is possible to gain insights into lifetime killers.

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When ions or electron beams are irradiated onto Si, a portion of the "substitutional carbon" that is slightly contained in Si changes into "interstitial carbon." This interstitial carbon is believed to influence the electrical properties of the device. The behavior related to interstitial carbon can be observed very sensitively through low-temperature PL analysis, allowing insights into trace amounts of carbon below the detection limit of SIMS analysis. This document presents examples of low-temperature PL analysis and SIMS analysis conducted on Si substrates subjected to ion implantation.

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TDS is a method that heats the sample, ionizes the released gases, and performs mass analysis. It can analyze the mass-to-charge ratio (m/z) from 2 to 199 in high vacuum (1E-7 Pa). In this case, we will introduce an example of TDS analysis conducted on a Si chip treated with hydrogen termination. The TDS was able to capture the desorption of hydrogen from the hydrogen-terminated surface.

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Fucoidan is a type of high molecular weight polysaccharide that is said to have effects such as boosting immunity, anti-cancer properties, and lowering cholesterol, and it has gained attention in recent years. It is considered a type of soluble dietary fiber and is found in seaweeds such as kelp and wakame. In this method, fucoidan in supplements and drinks is analyzed by breaking it down into monosaccharides. In addition to the main component, fucose, xylose, mannose, galactose, rhamnose, and glucuronic acid are simultaneously measured to calculate the quantitative values of each sugar.

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Carbon materials with nitrogen (N) atoms introduced as substitutes for platinum (Pt), the electrode catalyst in fuel cells, are attracting attention, and the catalytic activity is significantly related to the substitution positions of N within the carbon materials. XPS analysis allows for the evaluation of the N1s spectrum, where chemical shifts occur due to differences in bonding states and substitution positions of N, enabling the identification and quantitative separation of which C positions have been substituted by N.

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In fluorescent X-ray analysis (XRF), it is possible to easily evaluate element distribution and film thickness. In this case study, we will introduce an example of evaluating the thickness distribution of an Au film on a 4-inch Si wafer through multi-point mapping measurements. By performing multi-point mapping, we can calculate the Au film thickness using the FP (Fundamental Parameter) method from the XRF spectra at each point, allowing for the evaluation of thickness distribution based on the measurement coordinates.

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In fluorescent X-ray analysis (XRF), a simple evaluation of elemental distribution is possible. In this case study, we used a deposition device to create films of arbitrary amounts of Au on 4-inch Si wafers A and B as samples, and compared the distribution and total amount of Au. The results of the surface analysis confirmed the distribution state of Au (Figures 1-4). Additionally, by comparing the adhesion amounts based on the Au intensity from the XRF spectra obtained from each pixel, we confirmed that wafer B had more Au than wafer A (Figure 5).

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Aluminum oxide is used in various industrial machinery and manufacturing equipment parts due to its excellent wear resistance and heat resistance. Additionally, its chemical stability and high insulation properties make its thin films suitable for applications such as catalyst supports and insulating layers in magnetic tunnel junctions. The evaluation of the fine structure of aluminum oxide films, which can take on amorphous structures or various crystalline structures depending on the film formation conditions, is effectively conducted using XAFS. This document presents a case study of the quantitative separation of coordination structures (AlO4, AlO6) in amorphous aluminum oxide thin films.

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In MST, atomic-level TEM analysis is possible under atmosphere control (and cooling). This document presents a case where LiCoO2 particles, extracted from a lithium-ion secondary battery without exposure to the atmosphere, were processed using FIB and analyzed with TEM under atmosphere control and cooling. STEM observation and EDX analysis were conducted while cooling to -174°C, allowing for a visual confirmation of the atomic arrangement. This method can be applied to materials with low thermal stability and crystalline materials that undergo changes in the atmosphere for high-resolution analysis.

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This case study introduces an analysis of the condition of the cuticle on the hair surface using AFM. AFM is a method for three-dimensional measurement of nanoscale surface roughness. Since the analysis is conducted in the atmosphere, it does not cause degradation or gas release of organic materials, allowing for an evaluation of the sample's original shape. In this case study, we assessed the degree of cuticle opening, the distribution of adhered substances, and the roughness evaluation of different areas through images, as well as quantitatively evaluated the surface roughness through numerical processing. This method is effective for evaluating the condition of hair after shampooing and the application state after applying styling products.

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The majority of pharmaceuticals are crystalline and are known to have multiple crystal forms. Even for the same substance, the physical and chemical properties, such as solubility, can differ depending on the crystal form, which can also affect the efficacy and safety of the drug. Therefore, the identification of crystal forms is extremely important. In this case, XRD analysis was conducted to evaluate the crystal forms of the active pharmaceutical ingredient in question, both for the pure active pharmaceutical powder and for the commercial products.

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Gallium nitride (GaN) is used as a material for LEDs and power devices due to its high thermal conductivity and high breakdown voltage characteristics. In its manufacturing process, the production of high-quality GaN crystals without crystal defects is required, making the assessment of damage from ion implantation and the degree of recovery an important evaluation criterion. This document presents a case study evaluating the damage caused by ion implantation into GaN substrates using XAFS. It is possible to detect disturbances in the crystal structure near the GaN surface, as well as N2 and interstitial N within the film, with high precision.

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Nonylphenol ethoxylate (NPnEO) is used in industrial cleaning agents, but in January 2016, a restriction on the use of NPnEO in textile products was added to the European REACH regulation (Regulation on the Registration, Evaluation, Authorization, and Restriction of Chemicals). From February 3, 2021, the sale of specific textile products containing NPnEO (at 0.01 weight% or more) will be prohibited. This document presents the measurement results of NPnEO in various textile products.

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Organic fluorinated compounds are used in various applications such as surfactants and metal plating agents. Among them, perfluorooctanesulfonic acid (PFOS) is a substance regulated under the Stockholm Convention on Persistent Organic Pollutants (POPs), which restricts its manufacture, use, and import/export. Furthermore, the addition of perfluorooctanoic acid (PFOA) to the list of regulated substances is also being considered. In addition to PFOA and PFOS, perfluoroalkyl carboxylic acids (PFCA) and perfluoroalkyl sulfonic acids (PFAS) with different carbon chain lengths can also be analyzed simultaneously.

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Medical injection needles reduce puncture resistance and lessen the physical burden on patients by coating the surface of the metal tube with silicone. To maintain the performance of the needle, it is important that the entire surface is covered with a coating film. This report introduces a case where imaging analysis of the opening at the tip of the injection needle was conducted using TOF-SIMS to evaluate whether the coating film was applied. Since TOF-SIMS detects information from the very surface, it can assess the condition of the coating film without detecting the underlying elements.

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In protein composition analysis, there are methods to examine only the target protein after electrophoresis, but this document introduces "shotgun analysis," which comprehensively investigates proteins. In shotgun analysis, after separating proteins and obtaining mass information using LC/MS/MS measurements, a database search is conducted to comprehensively analyze the proteins present in the solution.

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TOF-SIMS identifies components from the mass of molecular ions, eliminating the need for labels such as fluorescent substances, allowing for imaging without their influence. Additionally, cross-sectional imaging enables the evaluation of distribution in the depth direction. In this study, a gel formulation of indomethacin was applied to three-dimensional cultured human skin, visualizing the distribution of the permeated active ingredient. As a result, it was found that indomethacin is concentrated on the surface side of the stratum corneum. Furthermore, depth profile analysis observed a gradual penetration towards the cell layers.

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In the solution that dissolves the SiN film (Si3N4) on the Si wafer, there is a Si matrix derived from the film in addition to the target impurity metal elements. Therefore, accurate and highly sensitive analysis cannot be performed directly on the dissolved solution itself. Thus, after dissolving the SiN film on the Si wafer, we enabled the analysis of impurity metal elements in the SiN film without the influence of the Si matrix by applying additional treatment. An example of conducting high-sensitivity analysis using ICP-MS with commercially available Si wafers with SiN films is provided.

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The purpose of evaluating metal contamination on the surface of Si wafers using ICP-MS includes not only the contamination assessment of the Si wafers themselves 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 the Si wafer surface is conducted for various purposes. ICP-MS analysis can sensitively obtain the amount of metal contamination on the surface of Si wafers, and it is also possible to specify the evaluation area according to the purpose.

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When peptides are measured using LC/MS/MS, characteristic fragment ions are obtained, allowing for the analysis of the amino acid sequence that makes up the peptide. Additionally, because peptides are separated and analyzed by LC, it is possible to analyze the sequences even in samples containing multiple peptides or impurities. Here, we present a case study where low molecular weight peptides were analyzed using LC/MS/MS, and the amino acid sequences were estimated.

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If the plating film contains gas, it may cause defects such as peeling, blistering, and bubbles within the film. To investigate the gas contained in the plating film, TDS, which can measure the gas released by heating the sample in a high vacuum, is effective. The results of TDS analysis on a sample with Ni/Au plating on SUS material are presented. The release of H2, HCN, H2S, and HCl from the plating film was confirmed. Additionally, quantitative values were calculated.

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TDS is a method that heats samples in high vacuum (1E-7 Pa) and detects the gases that are released. By heating the sample at a constant rate in high vacuum, it is possible to confirm the temperature dependence of even trace amounts of desorption (at the monolayer level). Additionally, for some components, it is also possible to calculate the number of molecules of the desorbed gas. We will introduce examples of TDS applied to representative materials.

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The band gap of thin film samples has been measured using analytical methods such as UV-Vis, PL, and XPS, but the cases that could be evaluated were limited due to constraints related to the sample structure, such as materials, film thickness, and substrates. This time, through the combined analysis of XAFS and XPS, it has become possible to reduce the constraints of the sample structure and achieve a higher precision band gap evaluation than before. This method is particularly effective for the evaluation of various oxide and nitride films. This document presents a case study on the band gap evaluation of silicon nitride (SiN) films. Measurement methods: XAFS, XPS. Product fields: solar cells, lighting, oxide semiconductors, power devices. Analysis purpose: evaluation of electronic states. For more details, please download the document or contact us.

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It is known that the adsorption of organic substances on the wafer surface can lead to various issues, such as the degradation of gate oxide film breakdown voltage. Therefore, as the miniaturization and high integration of semiconductor devices progress, it has become increasingly important to monitor not only inorganic substances but also trace amounts of organic substances. Here, we present a case where silicon wafers were stored in two types of wafer cases, and the organic contamination components adhered to the entire wafer surface were concentrated using a wafer analyzer and evaluated using GC/MS.

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Metal elements suspended in environments such as clean rooms and production lines can adhere to or contaminate products, potentially leading to a deterioration in product performance. With ICP-MS, exposure tests can be conducted on clean Si wafers, allowing for the measurement of the amount of metal elements adhered to the surface at ppt levels. Additionally, we also offer the loan of Si wafers that have been pre-cleaned.

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We will introduce a case where the permeability of water (H2O) in glass materials was evaluated by measuring the distribution of deuterium (D). When hydrogen (H) is already present, it is difficult to distinguish whether the hydrogen is due to the influence of water. Therefore, treatment with heavy water (D2O) was performed, and the distribution of the stable isotope deuterium was measured in depth using SIMS. By examining the depth distribution of deuterium, it is possible to estimate how deep the water has penetrated.

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Sn is used as the main raw material for solder, which is also used in semiconductor manufacturing. The gases in the solder can cause void formation, so it is important to control the amount of encapsulated gas in the solder and its main raw material, Sn. The results of investigating the gases released by heating Sn to a temperature above its melting point using TDS analysis are shown below. By heating the sample above its melting point, it is possible to evaluate the surface-adsorbed components and the components of the encapsulated gas in the sample.

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Titanium tetraalkoxide is an essential reagent for the Katsuki-Sharpless asymmetric epoxidation and is affected by oxidation in the atmosphere. In this case, we present an investigation using TOF-SIMS on how titanium tetraalkoxide (titanium tetra-isopropoxide) changes under controlled atmosphere and after exposure to air. In MST, the evaluation of the complex can be performed without the influence of atmospheric oxidation due to atmosphere control. Measurement method: TOF-SIMS Product fields: Biotechnology, Pharmaceuticals, Cosmetics, Daily necessities Analysis purpose: Deterioration investigation, Reliability assessment For more details, please download the materials or contact us.

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Carbon-supported PtRu (PtRu/C) catalysts are used as anode (fuel electrode) catalysts in fuel cells. There is a demand for reducing the amount of Pt used in order to lower costs, and active research and development is underway. To evaluate the state of the catalyst under fuel cell operating conditions, in-situ XAFS, which allows for observation in the same environment while controlling the gas atmosphere and temperature of the sample, is effective. This document presents a case study where the valence states of Pt and Ru in PtRu/C catalysts were evaluated using in-situ XAFS in an environment controlled to the gas atmosphere and temperature actually used in fuel cells.

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In-situ XAFS allows for the evaluation of the chemical bonding state and local atomic structure of a sample under controlled conditions, focusing on the gas atmosphere and temperature surrounding the sample. Therefore, it is suitable for cases where state evaluation in special environments, such as catalysts, is necessary. This document presents a case where RuO2 powder was heated from room temperature to 400°C under a reducing atmosphere using in-situ XAFS, capturing the changes in the state of RuO2. From the shape of the spectrum, it was confirmed that RuO2 is reduced to Ru between 100°C and 200°C.

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With the miniaturization of circuits, the design and development of micro vias for interlayer connections require an understanding of the quality of filling. TOF-SIMS is an effective method for evaluating the results, as it can simultaneously perform elemental analysis and analyze molecular information of organic and inorganic substances, as well as enable image analysis. This document presents a case study analyzing a sample with Cu filled in vias of approximately 0.5μm in diameter on a Si substrate. The analysis of positive ion results confirmed the distribution of Cu and Si. Measurement method: TOF-SIMS Product fields: LSI, memory, electronic components Analysis objectives: Composition distribution evaluation, failure analysis, defect analysis For more details, please download the document or contact us.

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SRA can analyze the depth profile of carrier concentration distribution over a wide range from shallow regions (a few hundred nm) to deep regions (a few hundred μm). It is also possible to evaluate the in-plane distribution of resistance values at the sample surface or at specified depths. As an example, we will introduce a case where the depth profile of carrier concentration distribution for a commercially available Si-IGBT chip was evaluated, including the entire chip, the field stop layer, and the lifetime killer, as well as the in-plane distribution of resistance values at the irradiation depth of the lifetime killer using SRA.

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SEM-EDX analysis and AES analysis are suitable for simple investigations of discoloration and foreign substances on metal surfaces. However, when the discoloration or foreign substances are thin or small, AES analysis, which provides information from very shallow areas of the surface (about 4-5 nm), is effective. The AES equipment owned by MST can acquire SEM images, allowing AES analysis to be conducted while confirming the areas of interest using SEM images. In this case study, we will present data comparing the evaluation of discoloration on the Cu surface using AES analysis and SEM-EDX analysis. Additionally, we will also present the results of AES depth direction analysis.

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One method for qualitative analysis of gases generated during sample heating is the pyrolysis GC/MS method, but the EGA*-MS method is effective for investigating the temperature at which each component detected here is generated. This method involves directly introducing the gases generated from the sample during temperature ramping into the mass spectrometer without passing through the GC column. This case presents an example of measuring the temperature profile of gases generated during the heating of polyvinyl acetate. * EGA: Evolved Gas Analysis

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The WA (Wafer Analyzer) is a device that heats wafers with a diameter of φ76 to 300mm to elevate their temperature, gasifying organic contaminants adhered to the wafer surface and trapping them in a collection tube. As a result, it can concentrate compounds such as phthalate esters and cyclic siloxanes, which are considered causes of device characteristic impacts and manufacturing troubles, allowing for high-sensitivity measurement using GC/MS. Quantification using hexadecane is also possible. - Evaluation of organic contaminants on one side of the wafer is possible. - Detection of easily volatile components is possible since vacuum pumping is not required. - Organic components can be detected with high sensitivity (for 300mm wafers, on the order of 0.01ng/cm²). - Quantification using hexadecane conversion is possible.

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TDS is a method that heats samples in a vacuum environment and monitors the gases that are released. When measuring organic substances, it can be difficult to obtain accurate measurements due to contamination of the equipment from large amounts of gas release. However, by adjusting the sample amount and analysis conditions in advance to control the amount of gas released, analysis becomes possible. Below are the results of TDS analysis conducted on organic films. We were able to capture the phenomenon where surface-adsorbed water is released at low temperatures, and the intensity of gas release increases with rising temperature.

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The analysis results of TDS may show multiple components detected for a single mass-to-charge ratio (m/z). Even in such cases, it is possible to estimate the components desorbed by heating by measuring multiple masses and comparing the desorption patterns. Using the TDS analysis results of W films on Si substrates as an example, I will explain the estimation methods for water and ammonia (m/z=17), as well as organic substances and argon (m/z=40).

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