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

We investigated the penetration state of components under various immersion conditions by soaking unconditioned hair, specifically facial hair, in a conditioner or treatment. In the facial hair soaked in conditioner, it was observed that siloxanes penetrated to the hair cortex over time, while high fatty acids appeared to be lost. In the facial hair soaked in treatment, nitrogen-containing organic substances did not penetrate the hair cortex and were only distributed around the cuticle.

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We will extract small pieces from the wafer chip without breaking it and thin them down for high-resolution TEM observation and analysis. Furthermore, by cutting and preparing samples while leaving the areas to be analyzed, we will conduct TEM observation and analysis of the target areas from any desired direction and provide the data. Through advanced TEM sample preparation techniques, we will meet various observation, analysis, and evaluation needs.

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By using a high-voltage power supply (capable of applying up to 2000V), it is possible to induce breakdown in diodes with high breakdown voltage. In this case, a SiC Schottky diode with a breakdown voltage of 600V was operated, and by applying high voltage in the reverse direction, breakdown was induced. After removing the cathode electrode through polishing, emission microscopy observations were conducted to identify the location of the breakdown current generation. Commercially available products were used for the measurements.

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Lithium-ion secondary batteries use a wide variety of materials, ranging from metals and inorganic substances to organic materials, and from solids to liquids. The physical properties and combinations of each material significantly reflect the characteristics and reliability of the device, making accurate analysis and evaluation of the materials necessary. In this study, the anode of the lithium-ion secondary battery was measured using pyrolysis GC/MS (pyro-GC/MS), and it was found that the binder material is based on SBR (styrene-butadiene latex). Additionally, decomposition products of the binder and aromatic substances presumed to be reaction products were also detected.

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Insights into the relationship between electrical properties and crystals can be obtained through EBIC and EBSD, but the depth of information differs. For areas where electrical properties were characteristic in the EBIC distribution measurement, we created cross-sectional samples and conducted STEM imaging in the depth direction. Additionally, we measured electron diffraction for each crystal grain. This further clarified the relationship between electrical properties and crystal grains and grain boundaries. By performing STEM observation and electron diffraction measurements, it is possible to obtain localized information about specific crystal grains.

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By using low-energy STEM observation and STEM-EELS surface analysis, we evaluated the mixed state of the active layer in bulk heterojunction solar cells. For the evaluation, samples were prepared with only the active layer deposited on ITO. The contrast in the low-energy STEM image (Photo 1) corresponds to the elemental distribution of S and C in the STEM-EELS images (Photos 2 and 3), confirming that it reflects the bulk heterostructure. Additionally, a bias in the distribution of S was observed, suggesting that P3HT is segregated towards the surface side.

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The electrodes of lithium-ion secondary batteries are composed of active materials, conductive additives, and binders for both the positive and negative electrodes. The characteristics of the battery, such as capacity and reliability, are greatly influenced by the combination of materials, mixing ratios, filling density of active materials, and voids. Among these, FIB-SEM observation, which allows for processing and observation in a completely dry atmosphere, is very effective for observing filling density and voids. Furthermore, by conducting three-dimensional observation (Slice & View), it is possible to directly evaluate the condition of the electrodes.

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In AES (Auger Electron Spectroscopy), it is possible to perform elemental mapping (surface analysis) at sub-micron levels, allowing for clear confirmation of the elemental distribution in ternary materials (Co, Mn, Ni). Additionally, the distribution of carbon derived from binders and conductive additives can be measured with high sensitivity. In this study, a series of processes for the positive electrode active material were conducted in an atmosphere-free environment (inert gas atmosphere) until the introduction of the equipment, minimizing alterations during measurement. As a result, it was suggested that larger particles are LiCoO2, while smaller particles are LiCoxMnyNizO2 and LiMn2O4, indicating a non-uniform distribution of particles. Measurement methods: AES・SEM Product field: Secondary batteries Analysis purpose: Composition evaluation, identification, composition distribution evaluation For more details, please download the materials or contact us.

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As a result of evaluating the surface of lithium-ion secondary battery anodes, which showed a decrease in capacity, without exposure to the atmosphere, a coating layer containing approximately 100-200 nm of Co was confirmed, and it was found that Co is in a metallic state. Applicable observation methods: FIB-TEM, SEM Surface analysis: SIMS, XPS, AES, TOF-SIMS Other structural evaluations are also possible. Measurement methods: SEM, FIB, TEM, XPS, EDX Product field: Secondary batteries Analysis objectives: Evaluation of chemical bonding states, shape evaluation, composition evaluation, identification For more details, please download the materials or contact us.

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We conducted three-dimensional imaging SIMS measurements of commercial MEMS products for B and As (measurement area: 75μm square, depth: approximately 1.5μm). After data processing, it is possible to extract surface distributions at arbitrary cross-sections and depths, depth direction distributions in arbitrary areas, and line profiles at arbitrary locations. Note: Since the sample is being excavated with an ion beam while capturing images in the depth direction, this constitutes destructive analysis.

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This shows the results of extracting the qualitative spectra of each layer by performing cutting processing of organic EL devices under controlled atmosphere. By conducting the cutting process of the organic EL devices under atmosphere control, we were able to obtain spectra of each layer that are closer to the true state.

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■Principle HAADF-STEM (High-angle Annular Dark Field Scanning TEM) images are obtained by scanning a finely focused electron beam across the sample and detecting the electrons that are scattered at high angles using an annular detector. ■Features Materials with a larger Z2ρ scatter more at high angles ↓ Heavy elements appear dark in STEM images and bright in HAADF-STEM images. Since contrast is obtained that is proportional to atomic number (Z), it is also referred to as Z-contrast imaging.

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By overlaying the luminescent image and the IR image, it is possible to identify leak locations under microscopic observation. If there are large-scale appearance anomalies such as cracks or electrostatic breakdown, abnormalities can also be confirmed with an IR microscope. Additionally, if luminescence cannot be detected due to light shielding of the emitter electrode, the collector electrode is removed, and near-infrared light is detected from the collector side. An example is presented where a high-voltage power supply capable of applying up to 2000V is used to operate a power device with high voltage resistance and low leakage current, and the failure location is identified using an emission microscope.

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To extend the lifespan of organic EL devices, it is essential to evaluate the degradation caused by electromigration, making it important to investigate the diffusion state of electrode metal components into the organic layer. However, whether analyzed directly from the cathode side or through the SSDP method from the anode side, the depth resolution decreases, making it difficult to assess the diffusion from the interface into the organic layer. (Note: SSDP method refers to analysis from the backside. For details on the analytical method, see section B0013.) Therefore, by using special processing to expose the cathode/organic layer interface and the organic layer/anode interface, it has become possible to evaluate the organic layer with high depth resolution.

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We directly observed the CdS/CIGS heterojunction interface using a Cs-corrected STEM device. TEM images, high-resolution HAADF-STEM images, and simulations using first-principles calculations confirmed that CIGS and CdS are heteroepitaxially joined.

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The heterojunction interface of ZnO/CdS/CIGS in CIGS thin-film solar cells was analyzed using the SSRM method, and the local resistance distribution was measured. By conducting measurements in a vacuum environment, we were able to remove adsorbed water from the measurement surface and achieve high spatial resolution. The measurement results indicate that we can measure the resistance values of each layer with nanometer-level spatial resolution. The resistance values of each layer differ by several orders of magnitude, indicating differences in carrier concentration. It was found that the CIGS layer has a higher resistance than the i-ZnO layer, and that CdS has an even higher resistance than these layers.

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We will disassemble commercially available LED lighting, conduct composition analysis of each material, identify defects, perform physical analysis, and analyze impurities for energy-saving key devices.

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In bulk heterojunction solar cells using p-type and n-type material active layers, it is necessary to properly control the mixing state of the materials within the film. After performing annealing treatment post-deposition, we conducted TOF-SIMS depth profiling analysis on samples that showed an improvement in photoelectric conversion efficiency along with an increase in fill factor without any change in open-circuit voltage. As a result, it was found that PCBM was segregated at the interface with the PEDOT:PSS layer before annealing.

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We investigated the shape and positional relationship of the poly-Si gate, n-type source layer, and p-type body layer of commercially available power transistors (DMOSFETs). By overlaying AFM images, we can also understand the positional relationship with the gate.

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The electrodes of fuel cells have a structure in which Pt particles, serving as the catalyst, are supported on a carbon carrier. For the evaluation of Pt, XPS analysis is effective for state analysis, while TEM observation is useful for morphological observation. These methods can also be used to assess the degradation of Pt catalysts, such as oxidation (poisoning) and aggregation (decrease in specific surface area). By reconstructing images taken from different angles, a three-dimensional image of the Pt particles is obtained.

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Solid polymer fuel cells (PEFC) are attracting attention for their high output at room temperature, making them suitable for automotive applications, home cogeneration, and mobile use. This time, we will introduce examples of molecular structure evaluation using TOF-SIMS, bonding state analysis using XPS, and quantitative evaluation of solid polymer electrolyte membranes. Additionally, MST allows for comprehensive evaluation of battery materials using various analytical methods under controlled atmospheric conditions.

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The hair roots of human hair (both shed hair and pulled hair) were pressed against a Si wafer, and imaging measurements (surface analysis) were conducted on the transferred components. Shed hair shows a strong tendency for ■K and ●phospholipids to be present only at the tip of the hair root. Additionally, it is believed that the entire hair root contains ■CnHmCOOH (n=17–31) fatty acids (derived from human sebum), ●amide components derived from keratin plugs, ◆nitrogen-containing organic acids with a mass of 500–700, and ◆organic substances with a mass around 800 that are aggregated. However, the organic substances containing two COOH groups derived from human sebum, which are observed in pulled hair, show a weak tendency.

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We investigated the distribution of the blue pigment "Cu phthalocyanine" dispersed on the polyethylene surface. TOF-SIMS analysis allows us to capture the distribution of organic materials with a pigment size of 1μm.

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This paper introduces a method for evaluating the in-plane distribution of solar cells with surface roughness while avoiding the effects of the roughness, using cross-sectional samples assessed by imaging SIMS. It was found that in regions identified as p+ Si layers by cross-sectional SCM, B and Al were present in high concentrations. Furthermore, using line profiles, the dopant distribution was converted to concentration, quantifying the degree of inhomogeneity in the plane. This method can also be applied to deep junction evaluations of power devices and impurity distribution assessments between and within trenches. Measurement methods: SIMS, SCM, SNDM Product field: Solar cells Analysis objectives: Trace concentration evaluation, composition distribution evaluation, shape evaluation For more details, please download the materials or contact us.

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Organic EL is expected to be a self-emitting, flexible next-generation display and lighting panel, but further improvements in reliability are desired. By combining various methods, comprehensive evaluations such as structural analysis, condition analysis, and identification of degradation causes can be achieved.

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As a result of performing pre-treatment to depth direction analysis without exposing the organic layer of the degraded brightness element to the atmosphere, diffusion was observed at the Alq3/emission layer interface in the samples after applying voltage. Similar results were obtained from both Slope Mapping (Figure 1) and depth direction analysis using ion sputtering (Figure 2).

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CIGS thin-film polycrystalline solar cells are expected to be low-cost next-generation solar cells. Development is underway for large-area and high-quality production. To evaluate the characteristics of the polycrystalline thin film, we conducted assessments of the pn junction using EBIC and crystal grain evaluation using EBSD on the same cross-section. We prepared a cross-section of the CIGS film and measured the open-circuit voltage (EBIC) by scanning an electron beam, visualizing the in-plane distribution of the open-circuit voltage. Additionally, by measuring EBSD on the same surface, we correlated the distribution of the open-circuit voltage with the crystal grains.

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In solar cells, surface roughness is utilized to effectively absorb sunlight. When conducting SIMS analysis, the surface roughness leads to a decrease in depth resolution. Measurements from the surface appear to show that elements like Cd, Zn, and O are diffusing into the CIGS layer due to the effects of surface roughness and knock-on (Figure 3), but measurements taken from the substrate side (back side) reveal that there is no significant diffusion of Cd, Zn, and O into the CIGS layer (Figure 4). In addition to interdiffusion, it is also possible to evaluate changes in the composition of the main components (Cu, In, Ga, Se) and the concentration distribution of impurities (B, Na, Fe).

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CIGS thin-film polycrystalline solar cells are being developed as next-generation solar cells expected to achieve low cost, large area, and high quality, and crystal information is required in this process. The EBSD method allows for the evaluation of crystal grains in CIGS films. The crystal information obtained from the EBSD method mainly includes orientation and grain size.

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In bulk heterojunction solar cells using mixed films of p-type and n-type materials, it is necessary to appropriately control the mixing state of the materials within the film for high efficiency. In films with low density (such as organic films), it is difficult to achieve contrast using a dedicated TEM machine at high acceleration voltages (several hundred kV) due to the high transmission of the electron beam. On the other hand, in STEM imaging at low acceleration voltages, where slight differences in density are reflected, the mixing state within the film can be clearly observed.

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Lithium-ion secondary batteries have excellent characteristics among secondary batteries and are widely used as power sources for various portable devices. However, there are still various challenges remaining, such as increasing output, capacity, longevity, and reliability. Comprehensive evaluation of battery materials is possible using various analytical methods.

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It is possible to detect H, C, N, and O in semiconductor substrates at concentrations below 1 ppm (approximately 5E16 atoms/cm3) and F at concentrations below 1 ppb (approximately 5E13 atoms/cm3) using this method. Examples of measurements in actual FZ-Si (Figure 1) and the background levels of III-V semiconductors are presented (Table 2). In addition to III-V semiconductors, standard samples have been prepared for various materials such as metal films and insulating films, enabling highly sensitive quantitative analysis. This method is ideal for bulk analysis of various materials, including semiconductor substrates, and for evaluating the contamination of gas components during semiconductor processes.

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The STEM device equipped with a Cs collector (spherical aberration correction function) enables ultra-high-resolution observation (resolution of 0.10 nm). The HAADF*-STEM image, which is sensitive to atomic weight, is an effective tool for directly understanding multi-component crystal structures. In this study, we evaluated micro-particles in oxide semiconductors, which can be applied to the atomic arrangement at heterogeneous material interfaces and compound interfaces, as well as grain boundary segregation assessments. *High-Angle Annular Dark-Field: Contrast is obtained that is proportional to atomic weight (Z).

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We physically peeled off the buffer layer/Alq3 interface and conducted XPS analysis on the peeled surface (buffer layer side). By peeling in an inert gas atmosphere, we were able to expose the interface without destroying the chemical structure, and by transporting it to the XPS device while maintaining the inert gas atmosphere, we minimized post-peeling alterations (such as oxidation and moisture absorption). The main component of the buffer layer is LiF, and it was suggested that some of it may have oxidized. By controlling the atmosphere, it is possible to evaluate the oxidation states of metal elements such as Al and Li due to differences in film formation methods, treatment methods, and organic layers.

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For membranes with low density, it is difficult to achieve contrast at high acceleration voltages (hundreds of kV) due to the high transmission capability of the electron beam. However, in low acceleration voltage SEM-STEM images, slight differences in density can be reflected, allowing for clear composition contrast. This can be applied to organic EL films, low-k films, gate oxide films, TEOS films, BPSG films, etc., where the differences in density, average mass, and composition are small. 1) STEM observation using SEM equipment with lower acceleration voltage compared to dedicated TEM equipment. Measurement methods: TEM, SEM Product fields: LSI, memory, display, solar cells, lighting Analysis purposes: Shape evaluation, film thickness evaluation For more details, please download the materials or contact us.

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The Ion Polish (IP) method allows for the production of cross-sections with minimal processing damage (such as delamination at interfaces, step differences due to hardness variations, and scratches from polishing) that were problematic in mechanical polishing methods. The positional accuracy of processing is also improved, enabling the creation of wide-area cross-sections that include small features. Due to the minimal damage to the crystals, clean crystal patterns can be obtained. Additionally, since there is no influence from mechanical stress, detailed evaluation of the cross-sectional structure of specific areas can be conducted through AES analysis, SEM observation, and EDX analysis while faithfully preserving the internal structure.

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Titanium dioxide (TiO2), used in electronic materials, catalytic materials, ultraviolet absorbers, and photocatalysts, exists in two forms with the same composition but different crystal structures: anatase and rutile. We conducted measurements on a polycrystalline TiO2 sample with a thickness of 20 nm, deposited on a Si substrate (Photo 1), using an electron beam probe focused down to approximately 1 nmΦ (FWHM). The EELS spectra obtained from the sample match the standard spectra of anatase TiO2 for both Ti and O (Figures 1 and 2).

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In semiconductor device manufacturing, from the perspective of improving yield, it is necessary to enhance the cleanliness of the backside of the wafer and to remove substances that remain on the bevel area of the wafer. In this study, we conducted TOF-SIMS analysis of the bevel inclined surface to evaluate the distribution of contamination (Figure 2). Additionally, by comparing the mass spectra of the adhered substances with those of the normal area and the contamination source, we found that the adhered substances matched the metal (Cr) and organic components of the contamination source. TOF-SIMS can capture the contamination generation process in the bevel area (edge and inclined surface).

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Organic EL displays are advancing in practical applications by leveraging advantages such as high brightness, high-resolution color, and thinness due to their self-emissive principle. Organic EL devices are manufactured by stacking organic films, but analyzing the organic films in their stacked state has been challenging. This time, by using the XRR method, it has become possible to measure the film thickness and density of the organic films while maintaining the stacked state. Analysis of the thickness and density of stacked films is possible regardless of whether they are crystalline or amorphous.

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The uniformity of the film composition and the distribution of impurities, which are one of the elements in device creation, were evaluated using imaging SIMS analysis. Through data processing after measurement, we can obtain planar images (Figure 1), cross-sectional images (Figure 2), depth distribution profiles at arbitrary locations (Figures 3 and 4), and line profiles. From the distribution of constituent materials and impurities, we can gain information that leads to process and film quality improvements.

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It is possible to evaluate the distribution of nitrogen in SiON films in the depth direction, even down to low concentration areas where high-sensitivity SIMS analysis excels, and to assess the amount of nitrogen (unit: atoms/cm²) with high precision (Figure 1). Additionally, nitrogen can be converted to atomic% (Figure 2), and a fitting curve for nitrogen can be calculated, allowing for the determination of nitrogen's peak concentration, depth, and half-width through fitting (Figure 3).

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By conducting SIMS analysis (SSDP-SIMS) from the substrate side, it is possible to obtain measurements that are not affected by the knock-on effects from the high-concentration layer on the surface due to surface roughness and sputtering. We evaluated the amount of boron penetration from the gate electrode (B-doped Poly-Si) into the substrate. Measurements from the substrate side showed no effects from knock-on, indicating that a more accurate evaluation of the penetration amount is possible. Thus, SSDP-SIMS is effective for assessing the barrier properties of barrier metals, the incorporation of metals into Low-k films, and the evaluation just beneath the rough silicide.

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We conducted TOF-SIMS analysis on an organic EL device (Figure 1) estimated to be formed from four layers of different organic compounds (or organometallic complexes) using XPS. For multilayer structural samples, depth profiling analysis using sputtering is also performed; however, in this case, we created a slope surface to expose each layer without breaking the bonds of the constituent components. Molecular weight-related ions and fragment ions presumed to be Alq3, NPD, and CuPc were obtained, confirming that TOF-SIMS analysis of the slope surface is an effective method for component analysis of organic multilayer films.

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The NBD method allows us to gain insights into lattice strain from the changes in the diffraction angle of the electron beam (positions of electron diffraction spots) within the sample. Measurements can be conducted in any arbitrary crystal axis incident direction, tailored to the device pattern. Results measured on the Si substrate in the element separation region (around LOCOS) confirmed that the strain varies depending on the heat treatment temperature and crystal orientation.

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The miniaturization of devices has increased the need for evaluating the depth distribution of impurities in extremely shallow regions. To conduct an accurate assessment, SIMS analysis using a primary ion beam with lower energy (below 1 keV) is required. Figure 1 shows examples of measurements of Si wafers implanted with BF2+ 1 keV, P+ 1 keV, and As+ 1 keV, using a primary ion beam energy of 250 eV to 300 eV.

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