一般財団法人材料科学技術振興財団　MST Product Lineup

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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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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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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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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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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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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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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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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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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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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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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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 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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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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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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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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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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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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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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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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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 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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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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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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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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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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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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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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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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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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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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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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- 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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- 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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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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To improve the reliability of organic EL, which is expected to expand in demand in the future, detailed structural analysis, state analysis, and identification of degradation causes will become increasingly important. We will introduce examples of evaluating layer structures and materials using TOF-SIMS and LC/MS. With TOF-SIMS, we were able to evaluate the layer structure and the component information of each layer. We conducted analyses of the components revealed by TOF-SIMS using LC/MS and a fluorescence detector, allowing us to assess the emission wavelength and understand the structure of the components. Thus, the combination of TOF-SIMS and LC/MS enables detailed evaluations.

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Glucosylceramide is one of the glycosphingolipids found in food, and due to its moisturizing effects and improvement effects on atopic dermatitis, it has gained attention in recent years. Not only in cosmetics applied directly to the skin, but also in health foods and general foods, as well as beverages that contain glucosylceramide, many processed products are being sold. By using HPLC, it is possible to analyze the amount of glucosylceramide contained in raw crops and processed foods with high precision. Here, we will introduce an analysis case of konjac.

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The metal processing surfaces of injection needles are generally rough, but it is known that using injection needles with rough surfaces can cause discomfort to patients. Therefore, to reduce surface friction caused by rough surfaces, biologically inert silicone lubricants are used on injection needles. This document presents a case study evaluating roughness using AFM (Atomic Force Microscopy) based on the presence or absence of surface processing with silicone lubricants.

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In PL (photoluminescence) mapping, it is possible to identify the positions of crystal defects from the luminescent areas. Furthermore, by performing high-resolution STEM observation (HAADF-STEM images) at the same locations, we can capture stacking defects. In this case study, we investigated commercially available SiC power devices using PL mapping and STEM. After identifying the positions of stacking defects through PL mapping, we conducted μ-sampling at the defect edge and performed cross-sectional STEM observation.

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In recent years, the development of alternative methods to animal testing for the efficacy and safety testing of pharmaceuticals and cosmetics has been progressing, with particular attention being paid to testing methods using three-dimensional cultured skin. In this case study, a percutaneous absorption test of a cosmetic (lotion) was conducted using three-dimensional cultured human skin, which was measured using AFM (Atomic Force Microscopy). This allows for a visual evaluation of the microstructure of the skin surface, and it is also possible to quantitatively assess the roughness of any specific area. By measuring under atmospheric conditions, it is possible to observe the samples while minimizing alterations that would occur under vacuum conditions.

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In recent years, the development of alternative methods to animal testing has progressed in the efficacy and safety testing of pharmaceuticals and cosmetics, with particular attention being paid to testing methods using three-dimensional cultured human skin. In this case study, a permeation test of indomethacin was conducted using a Franz cell, and TOF-SIMS and LC/MS/MS measurements were performed on the same skin sample. LC/MS/MS was used to quantify skin concentration and skin permeation, while TOF-SIMS was used to evaluate the component distribution within the skin. Measurement methods: TOF-SIMS, LC/MS, cryo-processing, cutting Product fields: Biotechnology, pharmaceuticals, cosmetics Analysis objectives: Composition distribution evaluation, safety testing For more details, please download the materials or contact us.

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TDS can evaluate the temperature dependence of the desorption of inorganic and organic gases that are released with increasing temperature. Therefore, it is effective for assessing the degassing of samples based on the baking temperature. The results of TDS analysis after baking the resist film at 50°C and 200°C are shown. It was confirmed that the degassing peaks detected up to 200°C after "baking at 50°C" were not detected after "baking at 200°C."

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TDS is a method that heats samples in high vacuum (1E-7 Pa) and investigates the gases released from the samples using a mass spectrometer. Since it is a vacuum system, it is not suitable for the large release of organic substances, but it can be evaluated by adjusting the sample amount. Below is an example of TDS analysis conducted on a resist film. Desorption gases originating from the resist film, such as organic substances, water, H2S, and SO2, were detected. It was also found that the desorption temperatures varied depending on the components.

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We will introduce a case where a sheet coated with graphite negative electrode particles used in lithium-ion secondary batteries was analyzed using TOF-SIMS. It was confirmed that graphite and PVDF are distributed on the surface of a single powder particle. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a method suitable for qualitative analysis and imaging of organic and inorganic substances on surfaces from the mass spectrum of secondary ions. It is effective for evaluating the distribution of minute foreign substances and stains due to its high resolution. Measurement method: TOF-SIMS Product field: Secondary batteries Analysis purpose: Composition distribution evaluation For more details, please download the materials or contact us.

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Corrosive gases such as etching gases have a significant impact on the degradation of semiconductors, electronic components, and devices. Below, we present an example of capturing corrosive gases using TDS (Temperature-Programmed Desorption Gas Analysis). It was confirmed that HCl, a corrosive gas, desorbs with the increase in temperature of the sample. Since TDS can capture desorption in the m/z range of 2 to 199 while heating, it is effective for investigating the types and amounts of corrosive gases as well as their temperature dependence of desorption.

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