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

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).

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.

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.

Polymers are known to exhibit diverse functions by altering their composition and structure, and they are utilized in various products. In the evaluation of polymers, assessment in real environments is crucial. This time, we will introduce a case where the shape of polymers on a substrate was visualized in the atmosphere and in aqueous solution using an environmental control atomic force microscope (AFM). Additionally, by combining data analysis, we quantified the dispersion of polymer particles.

The gas generation concentration device is an apparatus that traps gases generated from samples placed inside a chamber into a collection tube. By trapping in the collection tube, trace amounts of desorbed components can be concentrated and measured with high sensitivity using GC/MS. Depending on the type of sample, a suitable size of chamber can be selected, and it can accommodate heating up to 350°C. - Compatible with relatively large samples (on the order of several centimeters) - Allows for measurements with 2 to 3 orders of magnitude higher sensitivity compared to the headspace method - Enables evaluation of organic contamination from both sides of a wafer - Allows for evaluation of organic contamination on photomasks (reticles) - Quantitative analysis using hexadecane, decamethylcyclopentasiloxane, etc., is possible.

Foreign substances attached to manufacturing equipment or parts can affect product defects and equipment operation issues. By appropriately analyzing and evaluating these foreign substances, it is possible to investigate the causes of their occurrence and improve the defects. This document presents the results of evaluating the components of foreign substances attached to metal materials using Raman analysis. Raman can measure micro-regions of about 1μm, allowing for the acquisition of information regarding the molecular or crystal structure of targeted areas, making it effective for qualitative analysis of sparsely present foreign substances.

Foreign substances attached to manufacturing equipment or parts can affect product defects and equipment operation issues. By properly analyzing and evaluating these foreign substances, we can investigate the causes of their occurrence and improve the defects. This document presents a case study of the complex analysis of contamination attached to the surface of Si wafers using ICP-MS and SWA-GC/MS. SWA (Silicon Wafer Analyzer) -GC/MS is a method that heats the wafer in an electric furnace to gasify organic substances, which are then measured using GC/MS.

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).

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.

XPS is a surface-sensitive technique widely used for evaluating sample surfaces, but when combined with ion etching, it allows for depth analysis. In addition to the compositional distribution in the depth direction, XPS also enables the assessment of bonding states, making it suitable for investigating the causes of discoloration on the surfaces of device components. This document presents a case study evaluated by XPS regarding the discoloration of the blades of a turbo molecular pump.

Many metallic materials, such as steel, are known to deteriorate (hydrogen embrittlement) due to diffusible hydrogen that diffuses within the crystal lattice at room temperature. This time, we present an example of evaluating the amount of hydrogen desorption from stainless steel plates (SUS316L) with added hydrogen using TDS. A desorption peak, thought to be diffusible hydrogen, was observed in the low-temperature range around 150°C.

In AES analysis, the SEM observation function is included, allowing for the measurement of specific areas on the sample surface. Additionally, since measurements can be taken in sub-micrometer micro-regions, it is possible to target specific areas for measurement not only on flat samples like substrates but also on samples with spherical or curved shapes, which are less affected by curvature. Below is an example of evaluating the oxide film thickness on solder ball surfaces with different surface shapes.

ICP-MS can sensitively analyze the metal content in solutions, such as the metal amounts in the cleaning solution used in the wafer cleaning process and the metal amounts in the pure water flowing through the pipes installed in the equipment and buildings. It can accommodate various types of solutions, including pure water, acids, and alkalis, and can analyze metal element concentrations ranging from ppt levels to major component levels. This document presents case studies investigating the metal content in commercially available solutions.

It is possible to conduct internal structure analysis using X-ray CT while applying stress (tensile or compressive) to the sample. In this document, we used foamed rubber as an example to perform in situ X-ray CT measurements in both the normal state and the stretched state, and analyzed the volume changes of the bubbles from the obtained CT images. By combining in situ X-ray CT measurements with image analysis techniques, it is possible to evaluate under actual usage conditions, which was previously difficult, as well as assess the impact of stress on the product.

Epoxy resin is used as a semiconductor encapsulant, as well as an adhesive and for vacuum leak prevention both inside and outside vacuum devices. However, even after curing, heating may cause outgassing, which can negatively affect products and equipment. TDS (Thermal Desorption Gas Analysis) allows for monitoring outgassing components by heating the sample in high vacuum (1E-7 Pa) or while maintaining a constant temperature. Below, we present a case study investigating the outgassing behavior of epoxy resin using TDS with temperature maintenance.

Soldering of metals is one of the essential processes in the field of electronics. It is known that the outgassing that occurs when metal and solder are heated in contact can lead to voids. Below, we introduce a case where TDS analysis (Thermal Desorption Spectroscopy) was performed with solder placed on a copper plate. TDS can evaluate the outgassing associated with the heating of materials. By bringing the copper plate and solder into contact and heating them simultaneously within the TDS apparatus, we were able to capture outgassing in an environment close to the actual process.

In HAXPES, it is possible to obtain information from deep positions (up to about 50 nm) from the sample surface. Furthermore, by using a two-dimensional detector for angle-resolved measurements, data obtained at a wide range of photoelectron emission angles can be divided into information corresponding to different angles, that is, varying detection depths. This allows for a comparison of depth-resolved bonding states to greater depths than XPS in a non-destructive manner. It is effective for evaluating materials where state changes extend not only to the surface but also into the bulk.

To investigate the causes of defects such as poor adhesion, it is important to gain insights into the surfaces of wafers and devices. In this instance, hydrophobic areas were observed on a silicon wafer, prompting wide-area imaging using TOF-SIMS. As a result, components estimated to be silicone oil, CF-based grease, and paraffin oil were identified from the hydrophobic areas. TOF-SIMS typically has a measurement field of view up to 500μm square, but by moving the stage during measurement, it is possible to evaluate wide-area distributions. Measurement method: TOF-SIMS Product fields: Devices, Displays, Electronic Components, Manufacturing Equipment Analysis objectives: Qualitative, Imaging, Composition Distribution Evaluation For more details, please download the materials or contact us.

X-ray CT analysis allows for the non-destructive comparison and investigation of the structure and dimensions of components. This document presents a measurement case of a rubber O-ring used in vacuum equipment. To investigate a long-used item that is leaking gas, X-ray CT analysis and three-dimensional image analysis were conducted, comparing it with data from a new item. As a result, it was found that the long-used item had localized areas where the thickness of the ring was reduced, suggesting that leaks were occurring from those points. Measurement method: X-ray CT Product fields: Manufacturing equipment and parts, polymer materials, daily necessities Analysis purposes: Shape evaluation, film thickness evaluation, structural evaluation, failure analysis, defect analysis, degradation investigation, reliability evaluation, product investigation For more details, please download the document or contact us.

TOF-SIMS (Time-of-Flight Secondary Ion Mass Spectrometry) is a method that can sensitively evaluate organic and inorganic substances on the very surface, and it can be used as an analytical tool for various quality control processes of products. For example, it can be used for regular checks of surface contaminants during product storage, investigating the causes when defects such as peeling or discoloration occur in products, and analyzing changes in key components before and after altering manufacturing conditions. This document presents an example of comparing the surfaces of silicon wafers stored under different environments, focusing on the representative contaminant polydimethylsiloxane (PDMS). Measurement method: TOF-SIMS Product fields: Electronic components, manufacturing equipment, parts, and others (general electronics) Analysis purposes: Surface analysis, evaluation of chemical bonding states, failure analysis, defect analysis, and others (contamination assessment, quality control) For more details, please download the document or contact us.

Impurities contained in semiconductor materials can affect product quality, leading to issues such as leakage current and early device failure. Therefore, understanding the amount of impurities in the materials is crucial for improving product quality. This document presents a case study on SiC substrates, which are gaining attention as power device materials, analyzing impurities adhered to the substrate surface using ICP-MS and impurities within the substrate using GDMS. Measurement methods: ICP-MS, GDMS Product fields: Power devices, manufacturing equipment, components Analysis purpose: Trace concentration evaluation For more details, please download the document or contact us.

Ceramics are inorganic compound materials widely used in everyday goods and electronic components. For evaluating the discoloration of ceramics caused by impurities and adherents, TOF-SIMS analysis, which allows for imaging analysis of trace components regardless of organic or inorganic substances at the focus area, is effective. This document presents a case study where the discoloration of aluminum oxide ceramics was analyzed using TOF-SIMS, demonstrating the cause of discoloration through ion images and line profiles. Measurement method: TOF-SIMS Product field: Manufacturing equipment and components Analysis purpose: Composition distribution evaluation For more details, please download the document or contact us.

Ceramics are inorganic compound materials widely used in everyday items and electronic components. Their surface condition significantly affects the properties and performance of materials such as everyday items and electronic components. Therefore, it is important to properly evaluate the surface condition when assessing the functionality of ceramics. This document introduces a case study evaluating the cleaning components that contribute to the wettability of ceramic surfaces made of zirconium oxide, using TOF-SIMS to assess surface distribution and depth distribution. Measurement method: TOF-SIMS Product field: Manufacturing equipment and components Analysis purpose: Qualitative and distribution evaluation For more details, please download the document or contact us.

Ceramics are inorganic compound materials widely used in everyday items and electronic components. They possess characteristics such as heat resistance and chemical resistance, and evaluating the surface condition is important for utilizing the functions of ceramics. This document introduces a case where the cause of decreased hydrophobicity in Zr oxide ceramic materials with hydrophobic surface treatment was evaluated using TOF-SIMS. Measurement method: TOF-SIMS Product field: Manufacturing equipment and components Analysis purpose: Composition evaluation and identification For more details, please download the document or contact us.

When impurities are mixed into metallic materials, depending on the combination of elements, it can affect the reduction of toughness and corrosion resistance. Therefore, it is important to understand the amount of impurities in metallic materials for quality control. GDMS can simultaneously analyze 77 elements without standard samples, making it effective for impurity analysis of samples with unknown contained elements, regardless of the matrix. This document presents a case study of impurity analysis of FeCoNi alloys using GDMS. Measurement method: GDMS Product field: Manufacturing equipment and parts Analysis purpose: Trace concentration evaluation For more details, please download the document or contact us.

In precision machinery, vacuum devices, and semiconductor manufacturing equipment, contamination of the materials used can adversely affect product quality and the stable operation of the equipment. In this case, we handled glass components with disposable gloves of different types and analyzed the organic contamination adhered to the glass components using GC/MS analysis with a gas concentration device. By evaluating the contamination of the materials, it is possible to identify the components causing defects, eliminate the sources of material contamination, and consider changes to the materials.

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.

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.

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.

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.

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).

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).

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.

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.

This document presents an example of evaluating organic contamination through bonding state mapping using XPS. This bonding state mapping is obtained by acquiring XPS spectra of the element of interest at several hundred points within the plane and plotting the distribution of peak intensities corresponding to the energy positions of specific bonding states. Depending on the size of the area of interest, evaluation areas can be set to arbitrary sizes ranging from approximately 1mm to 20mm square, making it particularly suitable for assessing contamination, discoloration, and surface treatments on the order of millimeters. Similar evaluations can also be conducted for metals and silicon, in addition to carbon.

This is an example of wide-area quantitative mapping using XPS. We evaluated organic residue on silicon wafers using the following procedure. To graph the amount (atomic concentration) rather than peak intensity, it is less affected by sample roughness and allows for data acquisition over a wide area. It is suitable for investigating organic and inorganic contamination, discoloration, surface treatments, etc., as it enables an overview assessment of the compositional distribution on the sample surface.

The inner walls of metal pipes, such as SUS, used in various fields can discolor and corrode due to reactions with incoming gases and liquids, leading to a decline in equipment functionality. Understanding the locations prone to discoloration and corrosion, as well as their causes, is an important issue in equipment maintenance. At MST, we provide a comprehensive evaluation from sample cutting to analysis. This document presents a case study of XPS analysis conducted on the inner walls of SUS pipes used in vacuum equipment, highlighting both normal and discolored areas.

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.

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.

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

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