一般財団法人材料科学技術振興財団　MST Product Lineup

In the manufacturing process of semiconductor devices, various adhesive sheets, such as dicing tape, are used. Adhesive sheets can be a source of foreign substances and contamination. Therefore, in this case study, we will present the results of a comprehensive evaluation using TOF-SIMS and SWA-GC/MS. With TOF-SIMS, by conducting qualitative analysis of each adhesive sheet material, it is possible to identify which adhesive sheet is responsible for foreign substances and contamination, as well as which layer of the adhesive sheet is the source. Additionally, SWA-GC/MS allows for quantitative confirmation of which adhesive sheet has the least contamination.

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Positive-type photoresists are widely used as photolithography materials in semiconductor device manufacturing. The materials used in the resist vary significantly depending on the exposure light source, but for g-line and i-line resists, phenolic novolak resin is generally used as the base resin, and naphthoquinone diazide compounds are used as the photosensitizer. This case study introduces an example where naphthoquinone diazide compounds were decomposed using thermal decomposition GC/MS method to estimate the structure of the parent nucleus.

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By using high-sensitivity LC-MS (Q-TOF type), qualitative analysis of low-concentration components such as metabolites in biological samples is possible. It allows for the search for components that have undergone metabolism such as addition or conjugation in the body, as well as inter-sample comparisons aimed at investigating temporal changes and individual differences. After consuming a high-concentration catechin beverage and collecting urine, both unchanged catechin and the metabolite catechin-glucuronide conjugate were confirmed. The amounts of catechin and metabolites in the urine of eight individuals were plotted for excretion over 0.5 to 8 hours post-consumption, and comparisons were made.

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XPS is a method for obtaining information about the composition and bonding state of the sample surface (to a depth of about several nanometers), but by combining it with ion irradiation for sputter etching, it is also possible to evaluate the internal structure of the sample and depth distribution. However, in evaluations involving sputter etching, due to the principles and measurement mechanisms of XPS, the amount of oxygen may be overestimated due to the influence of adsorbed oxygen, so caution is required. In the case of evaluating samples that easily adsorb oxygen (such as Ti, TiN, AlN, etc.) or focusing on trace amounts of oxygen, the influence of adsorbed oxygen becomes significant, so comparisons between samples and analyses using SIMS are recommended.

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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.

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Soft X-ray emission spectroscopy (SXES) using synchrotron radiation is widely used as a method to evaluate the electronic states of materials because it allows for the direct acquisition of the partial density of states (pDOS) near the Fermi level for each element constituting the material. Furthermore, the characteristics of this method include: 1. Information from the bulk can be obtained, 2. It can be evaluated without being affected by charging effects even for insulators, and 3. It has a low detection limit (less than 1 atomic %), making it particularly effective for evaluating materials containing light elements (such as B, C, N, O). In this document, we will introduce the SXES spectrum of a GaN substrate as a measurement example.

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Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. Since they are implanted in the body, evaluating the condition of the surface area that comes into direct contact with biological tissue is important. TOF-SIMS not only provides qualitative analysis of the top surface but also excels in depth resolution at the top surface, allowing for highly sensitive evaluation of the condition in the depth direction. This case summarizes the results of evaluating the state of titanium in dental implants in the depth direction.

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Sodium lauryl sulfate (and ammonium lauryl sulfate, etc.) is used as an emulsifier, foaming agent, and cleaning agent in everyday products, pharmaceuticals, and industrial goods. This document presents measurement examples of everyday products (toothpaste, shampoo) that list sodium lauryl sulfate as an ingredient and those that do not list lauryl sulfates. By measuring with LC/MS/MS, it is possible to investigate the content of lauryl sulfates in the products.

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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.

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Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. The materials used for implants are often titanium or titanium alloys, and various coatings are applied to the surface to promote the bonding between the implant and the bone. Since implants are embedded in living organisms, the safety assessment of the surface area that comes into direct contact with biological tissues is crucial. XPS can evaluate the composition and bonding state of the very surface (approximately 5 nm). This document presents examples of evaluations conducted using XPS.

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Plastic containers, such as PET bottles used in many food products, have features like being lightweight and unbreakable; however, a challenge has been their lower gas barrier properties compared to cans and bottles. In recent years, technologies have been developed to coat PET bottles with gas barrier films to prevent quality degradation due to oxygen intrusion and carbonation loss, and these technologies are now widely used. This document presents a case study on the measurement of commercially available PET bottles, along with an evaluation of the composition and chemical bonding state of the gas barrier films.

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The Karl Fischer titration method is a way to evaluate the moisture content, and the method of introducing the sample into the device varies depending on the properties of the sample. Here, we will introduce two sample introduction methods for titration.

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On April 2, 2018, MST will introduce the latest processing and analysis equipment and begin offering non-destructive analysis services. We will provide analysis services across a wide range of fields, including product development and quality control for electronic devices, pharmaceuticals, and food. Non-destructive analysis is a technology that visualizes the internal state of a product without destroying it. Until now, MST has primarily offered contract services based on destructive analysis methods such as electron microscopy and mass spectrometry. However, there has been an increasing customer demand for observing electronic devices without destruction in recent years. Additionally, there has been a growing need in other fields as well, such as confirming the shapes of pharmaceutical and medical device components, observing the distribution of constituent materials within food, and checking for the presence of cavities. With the introduction of the latest processing and analysis equipment, MST is now able to conduct non-destructive analysis. We will provide analysis services on a contract basis.

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• Composite Materials

Understanding the band structure, including valence bands, conduction bands, and gap states, is an extremely important evaluation criterion for controlling various properties of materials. However, there are limited analytical methods available for direct and detailed assessment of these aspects. Simultaneous measurements of X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) using synchrotron radiation allow for a comprehensive understanding of the band structure, as well as detailed information regarding the attribution of the elements and orbitals that compose it. This document presents the XAS and XES spectra of GaN substrates as an example of measurement.

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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.

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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.

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In Raman analysis, the component distribution in the depth direction can be confirmed through measurements from the surface. It is effective for materials that easily transmit light, allowing for non-destructive evaluation without the need for cross-section processing or ion sputter etching. This document presents an example of evaluating each layer of an organic multilayer film using Raman 3D mapping. The results indicated that the organic multilayer film is composed of four layers. Additionally, by comparing with library data, the components of each layer were identified.

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Dental implants are artificial devices that are embedded in the jawbone when teeth are lost due to cavities or periodontal disease. Since implants are directly embedded in the body, evaluating their safety is crucial. This document presents a case where the quantification of impurity elements was conducted using Dynamic-SIMS. The analysis results revealed that, in addition to the main component Ti, O and Fe were also present. Dynamic-SIMS can evaluate the elemental distribution in a depth of several micrometers at the order of ppm to ppb.

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Fucoidan is a high molecular weight polysaccharide found in seaweeds, and various functional properties, including anti-cancer effects, have been reported. The Japan Health and Nutrition Food Association (JHFA) announced the standards for fucoidan foods in July 2017, and MST was registered as a designated testing institution capable of conducting the necessary analyses. The JHFA standards specify fucoidan food regulations for three types: Okinawa mozuku, mekabu, and gagome kombu. The testing items include not only the fucoidan content in raw materials and products but also tests to confirm the safety of the products, such as arsenic and bacterial count tests.

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Lithium carbonate, widely used in the treatment of mania and bipolar disorder, must be administered while maintaining an appropriate blood concentration to prevent lithium toxicity. Therefore, regular measurement of blood concentration (therapeutic drug monitoring: TDM) is required. Analysis using ICP-MS (inductively coupled plasma mass spectrometry) allows for the quantification of lithium concentrations in the blood across a wide range, from subtherapeutic levels to toxic levels.

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In recent years, the market size for soft drinks has been expanding, and various studies are being conducted to further enhance their flavor. One report suggests that including an appropriate amount of dehydroascorbic acid in soft drinks can improve their taste. Dehydroascorbic acid is also produced by the oxidation of L-ascorbic acid, which is used as an antioxidant in beverages, so prompt analysis after opening the sample is necessary to obtain accurate values. This document measures the amount of dehydroascorbic acid over time after the sample has been opened.

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The SIMS analysis profile of the interface between different materials changes with a certain width in the depth direction. This is due to the characteristics of SIMS analysis, which are influenced by ion beam mixing and the roughness of the sputtered surface. The detected impurities represent averaged information up to the mixed depth, detecting ions from regions with a width in the depth direction. Therefore, the interface position is generally defined as the location where the ion intensity of the main constituent elements reaches 50%.

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There are materials in polymers that change shape depending on the environment. To observe the original shape of the sample, measurements in real environmental conditions are necessary. This document presents a case study that visualizes the surface shape of soft contact lenses in saline solution. By measuring under conditions close to the actual environment, it is possible to evaluate while maintaining the original shape of the sample.

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C-SAM is also known as SAT: Scanning Acoustic Tomography. - It is effective for confirming the "bonding state of electrodes" and "adhesion of bonded wafers," which are difficult to verify with X-ray CT observations. - In addition to reflected waves, transmission waves can also be acquired.

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• Other contract services
• Circuit board design and manufacturing

The TOC (Total Organic Carbon) measurement can evaluate the amount of organic matter contained in a sample. TOC measurement values are widely adopted as indicators for monitoring and managing water quality pollution in rivers and industrial water. This time, we will introduce an analysis case of seawater using the NPOC method (Non-Purgeable Organic Carbon). It can measure TOC with good reproducibility and is applicable to a wide range of fields, including solutions containing salt, plating solutions, and abrasives.

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• Water quality testing

TDS is a method for real-time detection of desorbed gases while heating the sample in high vacuum or maintaining a constant temperature. An example is shown where a SiN film on a Si substrate was held at 350°C to investigate the amount of H2 desorption. In simple heating, a desorption peak was observed around 500°C, but during the temperature hold at 350°C, the detection intensity of H2 decreased, and a desorption peak was observed upon re-heating.

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• Memory

In clean rooms where the manufacturing of semiconductors and liquid crystals takes place, it is important to monitor not only particles but also molecular-level chemical contamination (molecular contamination). Floating molecular contaminants include acidic and basic gases, cohesive organic substances, dopants, and metals, and the analysis methods vary depending on the components. Here, we will introduce details about cohesive organic substances and the representative collection methods, "adsorbent collection" and "wafer exposure collection."

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• Memory

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.

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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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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

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

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

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

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

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

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

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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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

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

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

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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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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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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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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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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