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

IGZO films are materials that are being researched and developed as TFT materials for displays. There are concerns that the diffusion of metal elements into the IGZO film may degrade the TFT characteristics, so it is necessary to accurately measure the metal concentration within the film for evaluating the device characteristics and reliability using IGZO films. We will introduce a case where the Ti concentration in the IGZO film was evaluated from the opposite side of the metal electrode using SSDP-SIMS.

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IGZO films are materials that are being researched and developed as TFT materials for displays. The carrier concentration changes according to the hydrogen concentration in the IGZO film, leading to variations in electrical characteristics. Therefore, it is necessary to accurately measure the hydrogen concentration in the film for evaluating the device characteristics and reliability of devices using IGZO films. We will introduce a case study that evaluated the hydrogen concentration in IGZO films under different heating conditions using SIMS.

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The IGZO thin film, a transparent oxide semiconductor, is being researched and developed as a TFT material for displays; however, there are still challenges regarding the stability of TFT characteristics for practical use. To address this issue, it is important to elucidate the IGZO film formation mechanism. By clarifying the electronic states of metal elements and their local structures in IGZO thin films through XAFS analysis using synchrotron radiation, it is possible to gain insights into the IGZO film formation mechanism. This paper presents a case study of local structure analysis of IGZO thin films using Zn-K edge XAFS spectra.

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It has been announced that nonylphenol (NP) will be newly added to the environmental standards concerning the conservation of aquatic organisms, as part of the environmental standards related to the preservation of living environments affected by water quality pollution (August 22, 2012). NP is considered a substance of concern due to its impact on living organisms, and the standard values are set between 0.0006 to 0.002 mg/L, depending on the water area and type. We will introduce a case study that evaluated NP concentrations within this concentration range. MST provides a comprehensive service that includes the lending of specialized containers and measurement.

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Odors are commonly expressed in various ways, such as "fragrance" that gives pleasure and "stench" that causes discomfort. Odors rarely exist as a single type of odor component; instead, they are typically a mixture of various odor components. To visualize these complex odors, instrumental analysis using gas chromatography-mass spectrometry (GC/MS) is effective. This document introduces the flow of odor component analysis and presents a case study of simultaneous analysis of unpleasant odors.

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In lock-in thermal analysis, it is desirable to increase the frequency to narrow down the hotspots; however, there is a problem that the sensitivity decreases. Therefore, it is important to shift the measurement conditions from the high-frequency side to the low-frequency side and identify the frequency at which the heating signal begins to be obtained. In this case, we will introduce an example where the heating location associated with leakage current was identified non-destructively in a cylindrical package. Thus, it is possible to identify heating locations even in samples with complex three-dimensional structures, which are difficult to analyze using the liquid crystal method.

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We will introduce an analysis case of commercially available SiC power MOSFET devices. In SiC materials, it is essential to control the materials in a system that includes not only Si but also C, which differs from the conventional manufacturing methods of Si semiconductors. In the process of forming ohmic junctions between the contact electrodes and the SiC layer, we evaluated the elemental distribution and crystal phases, including C, using EDX/EELS analysis with TEM and electron diffraction.

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We will introduce a case study evaluating the distribution of the diffusion layer in commercially available SiC power MOSFET devices. In the SiC MOSFET manufacturing process, the channel is formed through ion implantation, activation heat treatment, and epitaxial layer formation. During the active layer formation process, we understood the device structure through TEM observation and evaluated the diffusion layer distribution of the p-type/n-type cross-section and the epitaxial layer from SCM measurements, as well as the depth concentration distribution of dopant elements (N, Al, P) from SIMS measurements. Measurement methods: SIMS, SCM, TEM Product field: Power devices Analysis purpose: Trace concentration evaluation, shape evaluation, product investigation For more details, please download the materials or contact us.

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We will introduce two measurement examples of effective failure analysis methods for GaN-based LEDs and high-frequency devices. By conducting lock-in thermal analysis on LED elements, it is possible to visualize the presence and timing of heat generation associated with light emission, allowing for the identification of specific areas that exhibit unique behaviors or characteristics. By performing emission microscopy observation on high-voltage, high-frequency devices, it is possible to capture the light emission associated with breakdown and identify areas with issues related to voltage resistance.

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Linear alkylbenzene sulfonic acid and its salts (LAS) are used as anionic surfactants in household laundry detergents and were newly added as environmental standards for the conservation of aquatic organisms in public water bodies on March 27, 2013. Due to the low concentration of the environmental standard set at 6-50 μg/L, the high-performance liquid chromatography-tandem mass spectrometry (LC/MS/MS) method was designated for measurement as the first measurement method for the environmental standard. MST provides a comprehensive service from the loan of specialized containers to measurement.

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TBHQ (tert-Butylhydroquinone) is a compound used as an antioxidant in foods in countries such as the United States and China. However, in Japan, the import and sale of foods containing TBHQ is not permitted. As a result, imported foods may contain TBHQ, and if detected domestically, measures such as voluntary recalls are taken. This document presents examples of adding 0.1 ppm of TBHQ to various foods and measuring it using LC/MS/MS. In all cases, TBHQ was analyzed with a recovery rate of over 80%. We hope this will help ensure the safety and security of imported foods and raw materials.

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In MST, qualitative and quantitative analysis of tea catechins can be performed using LC/MS/MS. This document observed the changes in EGCG concentration based on the temperature and time of brewing tea (Figure 1). It was found that the higher the temperature, the greater the extraction efficiency of EGCG, with a significant amount extracted up to 5 minutes. Additionally, a comparison of the catechin content in six commercially available tea products confirmed that green tea contains more catechins than black tea or oolong tea (Figure 2). Benifuki green tea contains a high amount of methylated catechin (ECCG3"Me), which has strong anti-allergic effects against conditions such as hay fever.

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The main component of green tea, catechins, is known to have functions such as antioxidant effects, promoting fat burning, and lowering blood cholesterol levels, and it is designated as a specific health use food (Tokuho). Natural green tea contains four types of catechins (EC, EGC, ECG, EGCG), but commercially available tea also contains a significant amount of heat-isomerized catechins (C, GC, CG, GCG) produced during the heating sterilization process. This document presents a case study of analyzing commercially available green tea using LC/MS/MS to separate and identify eight types of catechins, including heat-isomerized forms.

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Glucosylceramide (plant ceramide), one of the glycosphingolipids, has been reported to have moisturizing effects and improvements for atopic dermatitis, making it a component of interest in the beauty field. Although the main structural components of glucosylceramide vary among plants, qualitative analysis can be performed using LC/MS. Additionally, since glucosylceramide has multiple molecular species even from the same plant source, quantitative analysis can be conducted with high precision using an evaporative light scattering detector (ELSD).

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Diosgenin is a component that has recently been reported to have not only nourishing and strengthening effects but also improvements in Alzheimer's disease and enhancements in motor function, making it a focus of attention. Natural diosgenin primarily exists as glycosides, and is abundantly found in foods such as yam. In this case, qualitative analysis of yam extract was performed using LC/MS, confirming multiple diosgenin glycosides. Additionally, by hydrolyzing the glycosides to unify them into aglycones (non-glycosides), quantitative analysis of diosgenin also becomes possible.

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The main component of Korean ginseng, which is widely used as a herbal medicine, is a saponin called ginsenoside. Ginsenosides are classified based on the way sugars are attached, and currently, about 30 types have been discovered. In this case, we will introduce an example of analyzing ginsenosides using LC/MS/MS. With LC/MS/MS, we confirmed that the double filtering effect of MRM allows for the separation of peaks from six structurally similar compounds, enabling simultaneous qualitative and quantitative analysis.

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Using data from Slice&View (a method that repeatedly performs FIB processing and SEM observation to obtain dozens of continuous images), it is possible to calculate the volume of particles and other micron-sized objects. This allows us to obtain information such as the presence ratio and average volume of each substance within a certain volume. In this case study, we will introduce an example where the volume of active material was calculated from the Slice&View analysis results of a lithium-ion secondary battery cathode, and the presence ratio was determined.

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Regarding the positive electrode of lithium-ion secondary batteries, it is possible to visualize the distribution of crystal grains insulated from the surroundings and the active materials whose conductivity has decreased due to degradation by mapping their shape and conductivity. In this case study, we present the results of estimating the material distribution through SSRM measurements conducted on a cross-section of the positive electrode of a lithium-ion secondary battery prepared by mechanical polishing, along with statistical processing. Measurement method: SSRM Product field: Secondary batteries Analysis purpose: Composition distribution evaluation, shape evaluation, degradation investigation For more details, please download the materials or contact us.

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In the pursuit of improving the efficiency of CIGS thin-film solar cells, various buffer layer materials have been investigated for controlling the band structure and crystallinity from the light absorption layer to the transparent electrode. This presents a case study of various evaluations conducted using X-rays on Zn-based buffer layers deposited on a flattened substrate. Comparisons can be made between different levels based on deposition conditions and various processes after deposition.

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For the sample where Pt was sputter-deposited on a Si substrate, Out-of-plane XRD and In-plane XRD measurements were conducted while increasing the temperature. In both measurements, it was observed that the peak intensity of Pt(111) increased and the full width at half maximum decreased at temperatures above 500°C, indicating that crystallization was progressing. Additionally, it was confirmed that as the temperature rose, thermal expansion caused the peaks to shift towards lower angles (the direction of increased lattice spacing).

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It is possible to determine the concentrations of Si-H and N-H in SiN films through FT-IR analysis. Although it is also possible to determine hydrogen concentration using analyses such as SIMS, this provides the total hydrogen concentration and does not allow for the separate determination of hydrogen bonded to Si and hydrogen bonded to N. In FT-IR, the Si-H stretching vibration and N-H stretching vibration have peaks at different positions, allowing us to use these peaks to determine the respective hydrogen concentrations. Below are examples of analyses that determined the concentrations of Si-H and N-H in SiN films on Si substrates.

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Transmission electron microscopy (TEM) allows for morphological observation and elemental analysis on the order of μm to nm. Since eyeshadows are aggregates of solid particles, we conducted the analysis directly using TEM. After TEM observation, we performed EDX analysis on specific areas within the field of view to estimate the materials based on the constituent elements. Furthermore, it is possible to distinguish crystal types through EELS analysis.

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Emulsification technology is a fundamental technology in cosmetic development and is utilized across various cosmetics. Changes in the structure of emulsifiers are closely related to the balance of water and oil in the product, the permeability of encapsulated active ingredients, cleansing power, and changes in user experience, making its analysis very important.

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This paper presents examples of evaluating the depth concentration distribution of the dopant elements N, Al, and P in commercially available SiC power MOSFETs using multiple analysis modes. Depending on the analysis objectives, it is possible to measure multiple elements simultaneously without measuring each element separately under optimal conditions. Examples are provided for cases of simultaneous multi-element measurement and measurements focused on each individual element.

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The functionality of films is known to be determined by factors such as material, thickness, and layer structure. In this study, we evaluated the layer structure of polyethylene-based multilayer films commonly used as food wrap. By confirming that the film is primarily composed of polyethylene using FT-IR, and employing GCIB (Ar cluster) for sputtering, we were able to clearly visualize the structure where polyethylene and nylon 6 are layered within a thickness of 10μm through depth profiling with TOF-SIMS.

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The surface shape of foundation puffs and the adhesion of cosmetics were evaluated using a digital microscope. The digital microscope has a greater depth of field compared to optical microscopes, allowing for accurate observation of large uneven objects that could not be focused on with a microscope. The observation results of commercially available foreign puffs are shown in Figures 1 to 4. The surface shape of the puffs and the adherence of the foundation can be confirmed. Additionally, as shown in Figure 5, it is also possible to directly observe the surface of the hand.

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The large-scale pet food recall incident in 2007 and the melamine-contaminated milk powder incident in 2008 led to the detection of melamine in dairy products, livestock feed, and other foods, prompting nationwide measures to address the issue. MST has established a method for extracting and recovering melamine from food with high precision, and quantifying it using LC/MS/MS analysis. Below are the LC/MS/MS analysis results. We hope this helps alleviate your concerns about food safety.

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Generally, in SIMS, the quantification of major elements with concentrations exceeding a certain percentage is considered to be low. However, by using the M Cs+ (M: target element) detection mode with Cs+ as the primary ion, it is possible to determine the compositional distribution of major elements in the depth direction. An example of depth compositional evaluation for Al and Ga in AlGaAs is presented.

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High impact resistance is required for the joints of lead-free solder used in electronic devices such as mobile terminals. To address this issue, solder alloys with trace amounts of elements like Ni have been developed. This document presents a case study comparing the in-plane distribution of a five-component lead-free solder with trace amounts of Ni and Ge added to a Sn-Ag-Cu system, and a three-component solder without additives, using imaging from D-SIMS, which excels in high-sensitivity analysis.

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In GaN-based LEDs, it is said that the diffusion of the dopant element Mg into the active layer leads to a decrease in luminous efficiency. This document presents a case study where SIMS analysis was conducted on GaN-based LED structural samples from both the surface side and the sapphire substrate side (back side) to evaluate the depth profile of Mg concentration.

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In general, the quantification of major elements with concentrations exceeding a certain percentage in SIMS is considered to be low. However, by using the M Cs+ (M: element of interest) detection mode with Cs+ as the primary ion, it is possible to determine the compositional distribution of major element elements in the depth direction. An example of depth compositional evaluation for Al, Ga, and In in GaN-based LED structures is presented.

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TOF-SIMS has the characteristics of simultaneously evaluating organic and inorganic materials, being capable of analyzing small areas with high sensitivity at the very surface, and allowing evaluation while still in the form of 300mm wafers, making it effective for residue investigations during cleaning processes. We will introduce an analysis case of the removal effect of organic contamination on Si surfaces. TOF-SIMS analysis was conducted on samples where amine-based organic materials were confirmed to be in extremely small quantities by XPS. Even in small areas, it is possible to measure components in such extremely small amounts.

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In the SiC power MOSFET (Figure 1), the concentration distribution of the dopant element Al in the SiC beneath the gate pad was evaluated using SIMS from both the surface side and the backside (Figure 2). Regardless of the direction of analysis, the distribution beyond a depth of approximately 0.5 μm also matches well, suggesting that the spread of the Al concentration distribution reflects the actual elemental distribution rather than being measurement-induced. SSDP-SIMS analysis is possible even on hard substrates like SiC, which are difficult to process. Please feel free to consult us first.

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SiC power devices are expected to reduce power loss and handle large power in a compact form as power conversion elements. We will introduce a case where the thickness and density of the gate oxide film, necessary for improving the characteristics of the device, were evaluated using XRR (X-ray reflectivity) and the bonding state was assessed using XPS (X-ray photoelectron spectroscopy).

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It is possible to identify the components of foreign substances confirmed by the foreign substance inspection device using a TOF-SIMS installed in a clean room. After evaluating the foreign substances following CMP cleaning, copper and hydrocarbon components were detected from the substances of interest. A wide distribution of the same components was observed around the foreign substances. This suggests that the foreign substance is more likely to be cleaning residue resembling a watermark rather than a particle.

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In SIMS analysis of layered structure samples, there is a concern that in structures where the layer of interest is located at a deep position from the sample surface, the depth resolution may degrade due to the influence of the concentration distribution of the upper layers. In such cases, it is effective to remove the upper layers through pretreatment before analysis. This document presents an example of selectively and progressively removing layers from InP/InGaAs-based SHBT (Single Heterojunction Bipolar Transistor) samples.

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By comparing the impurity concentration distribution obtained from SIMS with the carrier concentration distribution from SRA, not only can we understand the activation state of the dopants, but the presence of unknown impurities and inherent structural issues are also suggested in areas that do not align. Using Profile Viewer, it is possible to overlay and analyze SIMS data and SRA data on your own. As an example, we will introduce a case where SIMS and SRA were performed on a commercially available diode chip, specifically on the central part of the surface and the outer edge (Figure 1) as well as the backside after the package was opened.

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SRA (Spreading Resistance Analysis) is a method that involves polishing a sample at an angle, making contact with two probes on the polished surface, and measuring the spreading resistance (Figure 1). By evaluating the carrier concentration distribution, it is possible to gain insights into the activation status of dopants. As an example, we present a case of SRA conducted on the central and outer regions of a diode chip surface after package opening (Figure 2).

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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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