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

SiC power devices are expected to reduce power loss and handle high power in a compact form as power conversion elements. The quality evaluation of SiC substrates, which is necessary for manufacturing these devices, has become a challenge. We propose a method to evaluate and quantify the crystal orientation, in-plane defect distribution, surface roughness, and impurities of SiC substrates, as well as to visualize these factors. Measurement methods: XRD, AFM, PL, SIMS Product fields: Power devices, lighting Analysis purposes: Trace concentration evaluation, structural evaluation, shape evaluation, failure analysis, defect analysis For more details, please download the materials or contact us.

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Imaging SIMS measurements were conducted on a 50μm square area on the emitter side of the NPT-IGBT. Figure 1 shows the ion images of 11B and As obtained from the analysis. It can be seen that 11B and As are injected into the same area. Additionally, while conventional analysis calculates the average concentration of each element over the entire detection area, imaging SIMS measurements allow for the extraction of partial depth profiles, enabling the evaluation of the concentration distribution of dopants localized in the plane (Figure 2).

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We will introduce a case where the depth concentration distribution of dopant elements such as Mg and Si in GaN-based LED structures was evaluated using multiple analysis modes. By selecting the optimal analysis mode according to the purpose in SIMS analysis, more precise evaluations can be achieved, so please feel free to consult with us.

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GaN-based LEDs have become widely used for lighting applications. To enhance the light extraction efficiency, textured surfaces may be created; however, these textures can lead to a degradation in depth resolution during depth analysis. We will present cases where flattening processing was applied to textured surfaces to mitigate the degradation of depth resolution and evaluate the depth concentration distribution, as well as cases where analysis was conducted from the backside (substrate side).

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From the perspective of cost reduction, the use of high-resistance Si substrates for power devices made of GaN is expected. However, it is said that if Al and Ga diffuse to the surface of the Si substrate during high-temperature film formation, a low-resistance layer is formed, leading to leakage. Therefore, we will introduce a case where SIMS analysis was conducted to evaluate the presence or absence of Al and Ga diffusion into the Si substrate. To accurately assess trace diffusion, measurements were conducted from the Si substrate side towards the GaN layer.

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Typically, SIMS measurements are conducted using chips with a flat surface of a few millimeters in size, but analysis can also be performed on small chips or samples with special shapes, typically less than 1 mm in size, by applying a fixed pre-treatment. Some samples that require investigation of trace components may have shapes that are not suitable for analysis under normal conditions, such as tiny chips or wire-like samples (Figure 1). In such cases, analysis is performed after fixation (Figure 2). Additionally, analysis may be possible for cross-sections, side surfaces, or samples with special shapes by applying pre-treatment.

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We will introduce a case where the thickness of extremely thin films, such as natural oxide films on silicon wafers and silicon nitride thin films, which are less than a few nanometers thick, was calculated using XPS analysis. By measuring the Si2p spectrum of the surface of the Si wafer and performing waveform analysis on the obtained spectrum, we can determine the ratio of the presence of each bonding state, and from this result, it is possible to estimate the film thickness based on the average free path of photoelectrons (Equation 1). XPS allows for non-destructive and simple calculation of thin film thickness on substrates as broad average information.

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SIMS analysis can be applied to various shapes of samples beyond wafers and substrates. In this case study, we will introduce an example of evaluating the distribution of impurities in a wire. The results of evaluating the impurity distribution in the depth direction from the side of the wire (Figure 2) indicate that the impurity profiles of H, O, F, S, and Cl vary in intensity with depth, suggesting that they are localized within the wire. The elemental mapping of the wire cross-section (Figure 3) confirmed the localization of impurities within the wire.

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SiC has been actively researched and utilized in recent years for applications such as power devices. Due to the various polytypes of SiC, there is a problem where stacking defects, which can lead to disordered stacking arrangements, easily occur. One method for detecting these defects is photoluminescence (PL), which analyzes the light emitted when a sample is stimulated with light. We will introduce a case where mapping measurements were conducted to detect light emission caused by defects.

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Stainless steel (SUS) is excellent in corrosion resistance and is used in various industrial products and components. Although it is a material resistant to corrosion, changes in the composition of the surface passive film due to aging or processing can lead to issues. In this instance, we introduce a case study analyzing the state of the metal oxide film on the surface of stainless steel using TOF-SIMS. TOF-SIMS allows for the high-sensitivity acquisition of molecular information in the oxide state, enabling the distribution of oxides ranging from a few nanometers to several tens of nanometers on the surface to be obtained, and spatial distribution can be evaluated through image analysis. Measurement method: TOF-SIMS Product field: Manufacturing equipment and components Analysis purpose: Evaluation of chemical bonding state, composition distribution, and thickness of corrosion layers For more details, please download the materials or contact us.

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The presence of OH and fluoride on the surface of aluminum electrodes is one of the causes of electrode corrosion, and investigating the state of the aluminum surface is essential for identifying the causes of defects. TOF-SIMS excels in depth resolution at the very surface and can measure depth distribution with high sensitivity while monitoring the state of inorganic substances. By evaluating the depth distribution along with OH, we discovered a phenomenon where OH increased without a change in the thickness of the oxide film. In this way, TOF-SIMS enables the evaluation of depth distribution of molecular information of inorganic substances that cannot be obtained through elemental analysis.

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In depth-direction analysis of molecular information obtained by TOF-SIMS, (1) the depth resolution is good, (2) it is possible to distinguish the chemical states of inorganic materials such as oxides, nitrides, fluorides, carbides, alloys, and metals, (3) evaluation of trace states is possible, (4) monitoring of OH is possible, (5) relative comparisons between samples (film thickness, composition) are possible, and (6) image analysis allows for a visual capture of the distribution of states at the surface level of a few nanometers. We will summarize the results of natural oxide films and oxide films. Measurement method: TOF-SIMS Product field: LSI, memory Analysis purpose: evaluation of chemical bonding states, evaluation of composition distribution, thickness of corrosion layers For more details, please download the materials or contact us.

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The electrodes of lithium-ion secondary batteries are very significant constituent materials that greatly influence the performance and reliability of the battery, such as its capacity. By performing ion polishing (IP) processing on the electrode materials after charge-discharge cycle testing under controlled atmospheric conditions, we can accurately observe them while minimizing degradation due to atmospheric exposure. In this instance, we will present a case that verifies the effect of atmospheric control on the positive electrode materials of lithium-ion secondary batteries after charge-discharge cycles by comparing the results of SEM observations after IP processing.

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The separator, which is a key component material of batteries, significantly influences the characteristics and safety of the battery due to its porosity, shape, and other factors. Currently, mainstream polymer materials such as polyethylene (PE), polypropylene (PP), or their composites have low softening points, with PE around 125°C and PP around 155°C. This report presents a case study where the cooling of a low softening point PP separator was conducted to suppress degradation and evaluate its structure.

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Si is one of the candidates for high-capacity negative electrode active materials, but it is said to suffer from severe cycle degradation due to very large volume changes during charge and discharge. In this study, to confirm the state of the Si negative electrode after charging, we disassembled it under a controlled atmosphere environment and performed cooling FIB processing, followed by observing the cross-sectional shape using SEM. When observing the cross-section at room temperature, significant damage such as film contraction, roughness of the observation surface, and pore formation was observed. In contrast, by conducting the observation while cooling, we were able to suppress the alteration of the Si negative electrode and evaluate the original shape of the sample.

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Lithium-ion secondary batteries have excellent characteristics among secondary batteries, but there are various challenges in their development, such as increasing output, capacity, and lifespan. This time, we will introduce a case where the composition of sheet-like active materials for the positive electrode was evaluated with high precision using ICP-MS analysis.

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PET bottles allow a small amount of air (oxygen) to permeate, making the beverages inside susceptible to the effects of oxygen intrusion from the outside, which leads to a deterioration in quality. To address this, various innovations have been made in PET bottles. For example, by inserting an oxygen-absorbing layer between the PET layers, as shown in Figure 1, the deterioration of beverages is prevented, preserving their taste. This document presents the results of analyses conducted using TOF-SIMS to confirm what the oxygen-absorbing layer is composed of.

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We disassembled a commercially available SiC Schottky diode and conducted imaging SIMS measurements to evaluate the concentration distribution of the dopant element Al in a 40μm square area to a depth of 0.5μm. From the data processing after the imaging SIMS measurements, we extracted the depth-wise concentration distribution of Al localized within the sample surface and present a case study comparing the concentration distributions for each pattern.

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We disassembled a commercially available SiC power MOSFET and conducted imaging SIMS measurements to evaluate the concentration distribution of the dopant elements Al, N, and P in a 20 µm square area to a depth of 0.5 µm. We will present a case where we extracted the depth profile concentration distribution of Al, N, and P localized within the sample surface from the data processing after the imaging SIMS measurements.

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SiC is used as a power device material due to its physical properties, but unlike Si, the diffusion of dopants after thermal treatment following ion implantation is difficult. Therefore, it is necessary to control the distribution in the depth direction through multi-step ion implantation. SIMS analysis can evaluate impurity concentrations in the depth direction with high sensitivity (below ppm), making it suitable for assessing the distribution of dopant elements in SiC. It is also possible to evaluate the distribution of light elements (such as H, C, O, F, etc.). Please contact us regarding any elements you would like to evaluate.

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The way makeup is removed varies depending on the type of cleansing oil, even with the same washing method. To investigate the cleansing effect, we evaluated the remaining components after washing lipstick with oil using TOF-SIMS. This report introduces a case where the differences in cleansing effects due to the type of cleansing oil were assessed by conducting relative comparisons of the components of the lipstick (such as pigments and oils) between samples.

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XRF is an analytical method used to evaluate the composition and distribution of constituent elements. A notable feature is that it does not require any special pretreatment for measurements, and it can be performed non-destructively over a wide range from 1.2 mm to several centimeters. As an example of elemental analysis using XRF, we will introduce a case where measurements were conducted focusing on the metal components contained in polymer materials of chemical storage containers, investigating metal contamination that adhered to the container surface during the storage period.

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White LEDs have a long lifespan and are energy-efficient, leading to a rapid increase in demand in recent years, particularly for lighting applications. White LEDs emit light through a blue semiconductor chip, which then excites surrounding phosphors (mainly yellow) to produce white light. Therefore, in investigating the improvement of luminous characteristics and the causes of degradation, it is necessary to confirm the luminous characteristics of both the semiconductor chip and the phosphor. A micro photoluminescence (PL) device can confirm the luminous characteristics by targeting small areas.

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In SCM, it is possible to identify the p/n polarity of semiconductors and visualize the shape of the diffusion layer. This method has been utilized for Si devices, but it can also be applied to SiC devices in areas where the carrier concentration is sufficiently high. This document presents the results of SCM analysis conducted on a cross-section of a SiC Planar Power MOS.

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In the development aimed at achieving flexibility and cost reduction for CIGS thin-film solar cells, low-temperature formation processes for the light-absorbing layer and non-vacuum processes are required, making the optimization of the film formation method for CIGS composition and the control of metal contamination levels crucial. This time, we will introduce a case where the composition and impurity concentration of the raw CIGS powder were evaluated with high precision using ICP-MS.

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In the development aimed at enhancing the performance of CIGS thin-film solar cells, the optimization of the film formation process conditions for the light-absorbing layer is necessary, and controlling the compositional distribution of the CIGS composition has become important. This document presents cases where the composition of the deposited CIGS thin film was quantitatively analyzed with high precision using ICP-MS, evaluated for depth concentration distribution using SIMS, and assessed for in-plane concentration distribution on the substrate using XRF. Measurement methods: SIMS, ICP-MS, XRF, etching Product field: Solar cells Analysis objectives: Composition evaluation, identification, compositional distribution assessment, film thickness evaluation, product investigation For more details, please download the materials or contact us.

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Epoxy resin is widely used in electronic component applications such as printed circuit boards and IC encapsulants due to its excellent mechanical properties, chemical resistance, and electrical insulation. Data measured by TOF-SIMS was obtained regarding the reagents of bisphenols, which are commonly used as raw materials for epoxy resin. By comparing the sample measurement data with standard data at MST, it is possible to investigate the origin of the detected fragment ions and estimate the materials used in the epoxy resin.

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To observe and analyze the internal structure of organic materials and liquid samples that are sensitive to heat, it is necessary to suppress temperature increases caused by processing or electron beam irradiation and to conduct a series of analyses while maintaining the original structure of the sample. In this case study, we will introduce an example where a cosmetic was used as an evaluation sample, and structural analysis was performed from cross-section FIB processing to SEM observation and EDX analysis while maintaining a cooling environment.

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We will introduce a case where XRD measurements were conducted by narrowing the X-ray beam to Φ400μm, allowing us to obtain crystal information targeting a specific area rather than the entire surface. In the XRD measurement results of the printed circuit board sample, Cu and BaSO4 were detected at all measurement points (1) to (3), and a peak from Au was detected at the measurement point (1), which is the electrode. This aligns well with the results from XRF measurements. Thus, it is possible to identify crystal structures by targeting regions of several hundred micrometers with different compositions and crystallinities. Measurement methods: XRD, XRF Product fields: LSI, memory, electronic components Analysis purposes: Composition evaluation, identification, structural evaluation For more details, please download the materials or contact us.

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Plastic consists of a crystalline portion where polymer chains are arranged in an orderly manner and an amorphous portion where polymer chains are randomly present. The mechanical strength, density, and thermal properties of crystalline plastics are greatly influenced by the degree of crystallinity, making it important to understand this degree. In this study, we investigated the changes in crystallinity of polypropylene films, which are crystalline plastics, by conducting XRD measurements while increasing the temperature.

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When materials undergo chemical reactions and phase changes with increasing temperature, performing XRD measurements while heating is effective. We present a case where high-temperature XRD measurements were used to identify the decomposition products of copper(II) sulfate pentahydrate. The results showed that the diffraction peaks changed at the temperature where decomposition occurred, clearly confirming the changes in the crystal structure. In MST, it is possible to conduct Out-of-plane XRD measurements and In-plane XRD measurements while heating.

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In semiconductor device manufacturing, it is necessary to remove metals remaining on the backside of the wafer from the perspective of improving yield, and it is important to quantitatively understand the amount of metal components remaining. To investigate the concentration distribution of metals remaining on the backside within a range of 500 µm from the bevel area, we conducted evaluations using TOF-SIMS. TOF-SIMS has the spatial resolution to detect metal components only near the bevel area, and by using standard samples with known concentrations, it is possible to quantitatively calculate the concentrations.

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It is possible to non-destructively determine the interstitial oxygen and carbon atom concentrations in silicon single crystals using FT-IR analysis. The concentrations are calculated from the peak heights of the absorption due to interstitial oxygen or carbon in the spectra measured by the transmission method. The calculation method is standardized by the Japan Electronics and Information Technology Industries Association (JEITA). Below are examples of calculated interstitial oxygen atom concentrations.

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On the surface of cell culture dishes, treatments are performed to convert hydrophobic plastic surfaces to hydrophilic ones in order to enhance cell adhesion. In this study, the surfaces of dishes that underwent hydrophilic treatment were evaluated using XPS and TOF-SIMS, revealing an increase in OH and CHO groups. By conducting quantitative evaluations with XPS and qualitative evaluations with TOF-SIMS, it is possible to capture how the surface has changed.

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Polyimide is a material that is used in various fields, including electronic components, due to its high heat resistance and excellent electrical insulation properties. Since surface modification can enhance adhesion to other materials, it is important to understand the state of the modified layer. In this study, TOF-SIMS measurements were conducted under sputtering conditions that minimize the degradation of organic components, allowing for the evaluation of polyimide components in the depth direction. Using GCIB (Ar cluster) for sputtering enables the measurement of the targeted organic components in the depth direction. *GCIB: Gas Cluster Ion Beam

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This paper presents a case study analyzing the degradation components of organic materials that deteriorate due to atmospheric exposure, using GCIB (Ar cluster). The experiment utilized the organic EL material, Rubrene. Measurements of the atmosphere-exposed samples using TOF-SIMS revealed the presence of a mass (m/z 564) estimated to be Rubrene peroxide, as well as low molecular weight benzene-related masses (m/z 77, 105). It was confirmed that these degradation-related components exist at depths of approximately 1μm or more from the surface. *GCIB: Gas Cluster Ion Beam

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Chitosan is used in a wide range of fields such as medicine, food, cosmetics, and clothing due to its antibacterial and moisturizing properties. Some cotton swabs, which are everyday items, contain chitosan to provide antibacterial effects. Therefore, we evaluated the chitosan contained in cotton swabs using TOF-SIMS, which allows for visualization through mapping and component assessment through spectral measurement.

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We will introduce a case where the concentration distribution of dopants in a-Si (amorphous silicon) was quantitatively evaluated in flexible thin-film Si solar cells. The sample, sealed with resin, was disassembled, and SIMS analysis was conducted. In the analysis of B (Figure 3), measurements were performed with enhanced depth resolution because it exists in shallow areas on the surface side. In the analysis of P (Figure 4), a large amount of H exists in a-Si, causing mass interference; therefore, measurements were conducted under conditions that separated H from Si using high mass resolution methods to detect only P.

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In SIMS analysis, it is essential to use standard samples with a composition close to that of the measurement sample in order to obtain more reliable concentration quantification values. By offering a wide range of AlGaN standard samples with varying Al content, we have been able to more accurately determine the impurity concentration in AlGaN, which is used in UV LEDs and UV sensors. We will present a case study where SIMS analysis of a UV sensor was conducted to quantify the concentration of the dopant, Si.

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We will introduce a case where the permeability of water (H2O) in a thin film with a thickness of less than 1 µm was evaluated by measuring the distribution of deuterium (D) in the film. When hydrogen (H) is originally present in the thin film, 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 naturally occurring isotope deuterium was measured in the depth direction using SIMS. By examining the depth distribution of deuterium, it is possible to estimate how deep the water has penetrated.

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We conducted qualitative analysis of the components by measuring the surface under controlled conditions, minimizing alterations due to processing, on a commercially available digital audio player equipped with an organic EL display.

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A comparison of the electrolyte of lithium-ion secondary batteries composed of organic solvents and supporting salts containing Li before and after degradation was conducted using LC/MS analysis. As a result, components believed to be reaction products of LiPF6 and the electrolyte were detected. Furthermore, by analyzing characteristic components after degradation using LC/MS/MS, it was possible to estimate the components that are thought to have been generated by the degradation test.

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The development of lithium-ion secondary batteries faces challenges such as improving performance, extending lifespan, and enhancing reliability. To address these challenges, it is important to understand the degradation mechanisms of the batteries. In this study, we conducted a heating degradation test to evaluate the degradation mechanisms caused by temperature. After the heating degradation test, we assessed samples that showed significant capacity reduction using LC/MS/MS for the electrolyte, TOF-SIMS for the anode surface, and FIB-TEM+EDX for the cross-section of the anode.

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Silicon (Si) is one of the candidates for high-capacity anode active materials, but it is said to suffer from severe cycle degradation due to the very large volume changes during charge and discharge. We dismantled and observed the Si anode before and after charging under controlled atmospheric conditions. Furthermore, we created cross-sectional observation samples using the FIB micro-sampling method and conducted shape observation and EELS measurements with a Cs-corrected STEM device to evaluate the condition of the Si electrode and the distribution of Li within the electrode.

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It is possible to measure the resistance of electrode materials in lithium-ion batteries using SSRM (Scanning Spreading Resistance Microscopy). In electrode composites made up of components with different resistance values, it may be possible to confirm the mixing ratio of various materials as well as the presence of electrically active and inactive active materials. Additionally, by combining shape measurements such as AFM and elemental analysis, a comprehensive evaluation can be achieved.

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