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

X-ray CT is a non-destructive analytical method that can measure the internal structure of samples, making it suitable for investigating abnormalities such as foreign substances, voids, and cracks within cosmetics, as well as for evaluating the dispersion of pearl agents and other components. In this case, foundation and lipstick were measured using X-ray CT to non-destructively assess their internal structures.

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MST offers a range of technologies suitable for evaluating the internal structures of electronic devices, and we propose analytical methods tailored to the observation field and objectives. This document presents case studies investigating specific areas of devices using X-ray CT and FIB-SEM. First, we observed the internal structure of the entire sample using X-ray CT to explore specific areas. Next, we used FIB-SEM to examine the detailed structures of the specific features identified on the vias.

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• Other electronic parts

By irradiating the sample with X-rays, a two-dimensional transmission image of the internal structure of the sample is obtained. Additionally, X-ray CT (Computed Tomography) images are constructed from continuous imaging data obtained by rotating the sample. - Non-destructive, allowing for the examination of the internal structure and defect shapes of the sample. - Capable of constructing 3D images and cross-sectional images at arbitrary locations. - The X-ray energy can be set between 30 kV and 160 kV, making it suitable for a wide range of materials from organic substances to electronic components. - With a dedicated stage, X-ray CT measurements of the sample can be performed under tensile/compressive or cooling/heating conditions. This document introduces application examples, principles, and data examples. For more details, please download the document or contact us.

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- It is possible to evaluate the chemical bonding states focusing on specific elements in the sample (especially light elements such as B, C, N, O). - The spectral shape reflects the partial density of states of the targeted elements in the valence band. - Evaluation of the band structure is also possible through simultaneous measurement with X-ray absorption spectroscopy (XAS). - Since information from the bulk is obtained, it is less affected by the influence of the surface region within a few nanometers. - Evaluation can be performed without being affected by charging effects, even for insulators. - The detection limit is low (<1 atomic%), allowing for the evaluation of trace components.

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Resins that excel in chemical resistance and electrical insulation are used as insulators, coatings, and adhesives for various electronic components. FT-IR analysis can investigate the causes of defects such as the degree of curing of the resin, making it effective for product development. As an example, we will introduce a case where the imidization rate was evaluated from the imide groups of polyimide. It is effective for process verification by comparing the imidization rate in the insulating film on the device with data on water resistance, heat resistance, and so on. Evaluation is possible in both chip and wafer states.

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• plastic

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.

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• Non-ferrous metals
• Solder

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.

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• plastic
• Other polymer materials

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.

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• Rubber

TDS (Thermal Desorption Gas Analysis) is a method that allows for the confirmation of desorbed components and desorption temperatures while heating a sample in a vacuum (1E-7 Pa). Furthermore, by combining the results of TDS with GC/MS (Gas Chromatography-Mass Spectrometry), which can identify organic substances, it is possible to evaluate the desorption temperatures of specific desorbed components in a vacuum. Below, we present an example of a combined analysis of TDS and GC/MS conducted on graphene.

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• Secondary Cells/Batteries
• LCD display

Lithium-ion secondary batteries are widely used in devices such as smartphones and digital cameras. These batteries degrade through repeated charging and discharging, which can lead to the phenomenon of battery swelling. When investigating a battery that has experienced this phenomenon, there are concerns about reactions caused by gases or electrolytes accumulated inside, and since processing can be dangerous, it is necessary to confirm the internal structure non-destructively. In this case, the internal structure of a lithium-ion secondary battery that has undergone repeated charging and discharging was observed using X-ray CT.

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• Secondary Cells/Batteries

Resins that excel in chemical resistance and electrical insulation are used as insulators, coatings, and adhesives for various electronic components. FT-IR analysis can investigate the causes of defects such as the degree of curing of resins, making it effective for product development. As an example, we will introduce a case where the degree of curing of epoxy resin was evaluated.

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• Other electronic parts

In order to investigate the causes of device failures that cannot be identified through visual inspection, non-destructive evaluation methods such as X-ray CT may be necessary. Using X-ray CT, we measured the faulty transistor and checked its internal condition. As a result, we confirmed a wire breakage, and it was also found that the mold resin surrounding the broken wire had deteriorated due to heat and other effects at the time of the breakage.

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• Other electronic parts
• Transistor

TOF-SIMS can identify components from the mass of molecular ions, allowing for imaging analysis without the need for labels such as fluorescent substances. Additionally, by measuring not only organic components but also inorganic components, it is possible to image not only the active ingredients of pesticides but also the minerals mixed into the formulations. In this study, we visualized the active ingredients of pesticides and inorganic components in two types of formulations with different mixing ratios. In formulation A (high mixing ratio), the active ingredient was widely distributed throughout the formulation, whereas in formulation B (low mixing ratio), the active ingredient was localized.

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• Chemicals

In scientifically evaluating the texture of food, internal voids serve as an indicator for assessing softness. To evaluate the internal voids of pancakes, we prepared pancakes made with a normal amount of eggs [1] and pancakes made with double the amount of eggs [2], and observed the internal voids using X-ray CT.

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A seamless capsule is a spherical capsule without seams that can contain powders or liquids and is used in pharmaceuticals, among other applications. In this case, the 3D structure of the seamless capsule was evaluated using X-ray CT. As a result, foreign substances were detected inside the membrane. Additionally, the membrane thickness distribution was visualized in 3D and represented as a histogram. By using X-ray CT in this way, it is possible to non-destructively evaluate the internal structure, investigate foreign substances, and assess membrane thickness distribution. Measurement method: X-ray CT Product field: Pharmaceuticals Analysis purpose: Structural evaluation, membrane thickness evaluation, product investigation For more details, please download the materials or contact us.

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The Scanning Ion Microscope (SIM) is a method that irradiates a solid sample with an ion beam and detects the secondary electrons generated. Since secondary electrons produce contrast according to the crystal orientation of each grain, it is possible to easily obtain insights into the size and distribution of crystal grains in polycrystalline metals such as Cu and Al using SIM. This document presents an example of measurements where the surface of Cu was observed using SIM.

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• Memory

Scanning Electron Microscopy (SEM) and Scanning Ion Microscopy (SIM) are both techniques used to evaluate the structure near the surface of a sample by obtaining secondary electron images. Differences in the primary probes lead to variations in contrast and spatial resolution, making it effective to choose between the two methods depending on the surface structure of interest. This document summarizes the comparison of the two methods and presents an example of measurements observing a Cu surface.

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• Memory

We will conduct a comprehensive analysis of DRAM, a representative memory, from product level to device microstructure analysis through TEM observation. By performing appearance observation, layer analysis, and Slice & View, we will grasp the overall structure, control the FIB processing position at the nanoscale, and observe the microstructure of the memory section through TEM imaging after thin section formation.

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• Memory

β-Ga2O3 has a wide band gap and is expected to be a promising material for next-generation power devices and oxide semiconductors in terms of excellent power transmission efficiency and cost reduction. In recent years, it has been reported that β-Ga2O3 can be n-doped with Si or Sn. In this study, we conducted structural optimization calculations for models of β-Ga2O3 doped with Si or Sn and evaluated which sites each dopant is more likely to occupy in the crystal. Subsequently, we calculated the density of states from the obtained structural models and investigated the changes in electronic states due to doping.

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• Other semiconductors

Amorphous SiNx (a-SiNx) films exhibit significant changes in physical properties from semiconductors to insulators due to compositional variations such as the N/Si ratio, making them suitable for a wide range of applications, including gate insulating films for transistors. On the other hand, experimental methods capable of atomic-level microscopic structural analysis for materials with non-crystalline amorphous structures are limited. Therefore, creating and analyzing amorphous structures with various compositions and densities through simulation becomes an effective tool. This document presents examples of structural analysis of a-SiNx films using molecular dynamics calculations.

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In recent years, SiC has attracted attention as a material for high-voltage devices. The trench MOSFET structure allows for high integration of the elements, and applications for SiC devices are also being advanced. On the other hand, there are challenges regarding the dopant activation rate of SiC devices, making performance evaluation important. In this instance, we will introduce a case where carrier polarity determination was conducted using SNDM (Scanning Nonlinear Dielectric Microscopy) and carrier concentration distribution was evaluated using SMM (Scanning Microwave Microscopy) for SiC trench MOSFETs.

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• Other electronic parts

By measuring the sample, it is possible to evaluate the crystal structure through the combination of results obtained and simulations. This document introduces a case study in which the crystal structure is discussed by comparing the results obtained from HAADF-STEM and EDX measurements on polycrystalline neodymium magnets with simulated images using the respective measurement conditions. The combination of measurement results and computational simulation results allows for a deeper understanding of the crystal structure.

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• magnet
• Memory

TOF-SIMS allows for simultaneous elemental analysis and molecular information analysis of organic and inorganic substances, and it also enables imaging analysis, making it an effective method for analyzing the distribution and penetration of target components in samples. By combining measurement methods and processing for hair, it is possible to evaluate the surface, cross-section, and depth distribution of hair from various perspectives, allowing for component comparison and permeability assessment in hair according to specific objectives.

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In recent years, SiC has been attracting attention as a material for high-voltage devices. The trench MOSFET structure is necessary for the high integration of devices, and the application development for SiC devices is progressing. Since the channel region of the trench MOSFET structure is the trench sidewall, the flatness of the trench sidewall is related to the reliability of the device. This document introduces an example of quantitatively evaluating the roughness of the trench sidewall of SiC trench MOSFETs using AFM (Atomic Force Microscopy).

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• Other semiconductors

In investigations of competitor products and inspections of defective items, an internal structural examination is necessary first. X-ray CT allows for non-destructive acquisition of transmission images from within the sample, enabling three-dimensional reconstruction. This document presents a case study where a discrete package equipped with SiC chips was observed using X-ray CT as part of a product investigation. After confirming the structure with X-ray CT, we propose conducting physical analysis (failure analysis) using MST.

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• Other semiconductors

Applications of carbon materials, such as graphene in electron emission devices and hydrogen storage in carbon nanotubes, are increasing in vacuum environments. Therefore, evaluating the outgassing from carbon materials in vacuum is an important point for the future applications of these materials. This case study introduces an example of outgassing analysis from graphene using TDS (Thermal Desorption Spectroscopy), which can evaluate outgassing from samples in a vacuum.

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• Secondary Cells/Batteries
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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.

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• Wafer
• Water quality testing

In SNDM (Scanning Nonlinear Dielectric Microscopy), it is possible to identify the p/n polarity of semiconductors and visualize the shape of the diffusion layer. This method encompasses the functions of the traditionally used SCM (Scanning Capacitance Microscopy), allowing for sufficient evaluation of next-generation power devices, such as SiC, which are difficult to assess with SCM, from low to high concentrations. It is characterized by high sensitivity and can be applied to all compound semiconductor devices. As an example, we will introduce a case where a cross-section of a SiC Planer Power MOS was fabricated and analyzed using SNDM.

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• Transistor

In the semiconductor manufacturing process, ion irradiation is sometimes performed for the purpose of surface modification. It is known that irradiating the surface of single-crystal Si with ions of inert elements can cause structural damage and lead to the formation of an amorphous layer. Utilizing the fact that high-resolution XPS spectra detect c (single-crystal) Si and a (amorphous) Si with different peak shapes, we will introduce a case where this damage-derived a-Si was separated from c-Si and quantitatively evaluated.

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We will introduce a compilation of basic explanations and analysis examples that will be helpful for your consideration of surface analysis. Please keep it on hand and make use of it for your consideration of analysis services. ★Free gift for all who wish to receive it★ Please check "Request for catalog" in the [Contact Us] section to apply. *You can view the digest version from [PDF Download].

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Angle-resolved X-ray photoelectron spectroscopy (ARXPS) is a technique that detects photoelectrons emitted by X-ray irradiation at different take-off angles, using spectra with varying detection depths to evaluate the depth profile near the sample surface. Compared to traditional methods using Ar ion sputtering, it offers improved depth resolution and advantages such as the absence of compositional changes due to selective sputtering or mixing, making it effective for evaluating the depth profiles of ultra-thin films (on the order of a few nanometers) on substrates. This document presents a case study on the evaluation of compositional distribution within a SiN film on a Si substrate.

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XPS is a method for evaluating the composition and bonding state of a material based on the photoelectron spectrum from inner shell levels. On the other hand, the valence band spectrum, which reflects the states of the outer shell electrons, appears near the Fermi level. This document presents a case study that verifies the reduction treatment of Sn oxides by comparing and discussing the density of states calculated through first-principles calculations with the valence band spectrum obtained by XPS. Utilizing computational simulations allows for a deeper understanding of the XPS spectrum obtained.

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Knowing how administered drugs distribute within the body is important information for drug development. In this case, the drug was directly administered into the vitreous body of fish eyes, and the distribution of the drug components was evaluated in cross-sections of the eyeball. As a result, the drug components were strongly detected near the administration site, showing their distribution within the eye. By using a mass microscope called TOF-SIMS, it is possible to apply this to the pharmacokinetics of various biological organs, including the eyeball.

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The penetration rate of smartphones is increasing year by year, and along with that, the protective films applied to their surfaces are diversifying in functionality. In this instance, we will introduce a case where two types of films (A and B) with fingerprint prevention and anti-reflection features were quantitatively evaluated in terms of roughness, simulating the sensation of touch through AFM analysis.

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• LCD display

Polyurethane is a resin material characterized by high resilience. Rigid polyurethane foam, a type of polyurethane product, is used as insulation material for homes. In this case study, we observed the shape of the internal voids in sheet-like rigid polyurethane foam using X-ray CT. As a result, we were able to confirm the shapes of the numerous individual voids present inside. Furthermore, we conducted a quantitative evaluation of the void ratio using the obtained data. Measurement method: X-ray CT method Product field: Daily necessities and resin materials Analysis purpose: Shape evaluation, structural evaluation, product investigation For more details, please download the materials or contact us.

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• plastic

We will introduce a case where lenses and CMOS sensor chips were extracted from commercially available smartphones and evaluated. Depending on the purpose, we created flat and cross-sectional surfaces through polishing and FIB processing, and confirmed the layered structure and layers using TEM and SEM. Furthermore, we identified the types of films using EDX. At MST, we can handle everything from disassembly to analysis in a consistent manner.

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• lens

Diacetyl, which has a buttery smell, is known as an off-flavor (off-odor) in beverages and significantly affects the flavor of products. In particular, in the brewing industry, even minor differences in concentration at the ppb level can influence the aroma of the product, making it useful to sensitively quantify diacetyl concentration for quality assessment and product development. This document presents a case where trace amounts of diacetyl in beverages, which could not be evaluated by standard GC/MS measurements, were quantifiable through derivatization treatment.

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Graphene, a monolayer form of graphite, is expected to be applied in a wide range of fields such as batteries, transparent electrodes, and sensors due to its excellent properties, including toughness, high electrical conductivity, and high thermal stability. It is also said that the types and amounts of functional groups present on the surface vary depending on the manufacturing method, and clarifying its structure is an important point for improving performance. This case study introduces a comparison of the functional groups of two types of graphene using thermal decomposition GC/MS method.

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• Transistor
• Power storage device

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.

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• Solder

AFM is a method that scans the surface of a sample with a fine probe and measures nano-scale surface topography in three dimensions. It can measure a wide range of materials, not only for the evaluation of metals, semiconductors, and oxides, but also for soft materials such as hair and contact lenses. This document presents various AFM images of different materials.

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• Wafer

This document presents case studies evaluating the diffusion layer of image sensors in smartphones. Using a scanning capacitance microscope (SCM) capable of determining the p/n type of semiconductors, we assessed the distribution of the diffusion layer. By combining the results from cross-sectional and planar SCM, we obtained complementary and extensive information. SCM is one of the effective tools for evaluating the quality of image sensor diffusion layers and for failure analysis.

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• lens

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.

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• Other metal materials
• Steel

When designing and controlling the properties of various materials, it is very important to clarify the types and amounts of elements present in trace amounts in the base material, as well as their states of existence. The types and amounts of elements can be evaluated using methods such as SIMS (Secondary Ion Mass Spectrometry) and ICP-MS (Inductively Coupled Plasma Mass Spectrometry), but the evaluation of states of existence, such as valence and chemical bonding states, is effectively conducted using XAFS (X-ray Absorption Fine Structure) measurements with synchrotron radiation. This document introduces a case study where the valence of trace amounts of Ce in ceramic materials was evaluated as a measurement example.

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• Ceramics
• Wafer

The peaks in the Raman spectrum of single crystal Si shift to higher wavenumbers when compressive stress is applied to the sample and shift to lower wavenumbers when tensile stress is applied. This allows us to gain insights into the stress in Si. An example is shown where the distribution of stress in the cross-section of an IGBT (Insulated Gate Bipolar Transistor) was confirmed using Raman mapping.

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• Wafer

Organic acids are a general term for acidic organic compounds. In addition to components found in food, such as citric acid, which contributes to sourness, and inosine acid, which contributes to umami, they are used as raw materials and additives in cosmetics, pharmaceuticals, and industrial fields, with a wide range of applications. This document introduces simultaneous analysis of 12 organic acid components using HPLC and case studies of soft drink analysis. After separating each component in the column, selective analysis can be performed without being affected by interfering components by reacting with a color reagent (BTB solution) for detection. It is possible to simultaneously qualitatively and quantitatively analyze organic acids in liquid samples as well as in extracts from solids.

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