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

Gas chromatography (GC) is classified as a type of chromatographic method that utilizes differences in the adsorption or distribution coefficients of gases against a stationary phase to separate components. Gas chromatography-mass spectrometry (GC/MS) allows for the qualitative and quantitative analysis of components by using a mass spectrometer to detect the components separated by GC, based on mass information. - Effective for analyzing components with relatively low molecular weights and high volatility - Capable of qualitative and quantitative analysis of trace organic components - Various introduction methods can be selected according to the state of the sample and the purpose - A wide range of organic component structure estimation is possible due to a rich library

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XRR measures the reflection intensity of X-rays incident on the sample surface at a very shallow angle. By comparing the reflection X-ray intensity profile obtained from this measurement with simulation results and optimizing the simulation parameters, this method determines the film thickness and density of the sample. - Evaluation of film thickness is possible (approximately 2 to 300 nm) - Evaluation of density is possible - Evaluation of surface roughness is possible (Rms ≤ 5 nm) - Non-destructive analysis is possible - Average information over a wide area of approximately 10×20 mm can be obtained

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This is a method for structural analysis of sample surfaces. It is suitable for identifying organic contamination on the very surface due to its sensitivity compared to other analytical devices. Using a sputter ion source, it is possible to analyze the distribution of inorganic and organic materials in the depth direction. - Structural analysis and identification of organic and inorganic compounds are possible. - Coordination data from foreign substance inspection devices can be linked. - Qualitative analysis is possible from micron-order microforeign substances to several centimeters. - It is possible to analyze the very surface with high sensitivity. - Image analysis is possible. - Qualitative analysis of depth direction analysis is possible.

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UPS is a method that measures the kinetic energy distribution of electrons emitted by ultraviolet light irradiation, providing insights into the valence states of the sample's surface (on the order of a few nanometers). On the other hand, it is also used to evaluate the work function of various metal materials by utilizing high energy resolution. Since it can be measured alongside XPS analysis, it is possible to investigate the qualitative and quantitative surface composition of the sample and the correlation between bonding states and work function values.

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SAXS is an analytical method that measures the X-rays scattered by a substance when X-rays are irradiated onto it, specifically in the low-angle region where 2θ < 10°. It is used to evaluate the structure of materials. Typically, it can assess structures ranging from a few nanometers to several tens of nanometers in size. - Enables evaluation of periodic structures and orientation at the nanoscale - Allows assessment of the distribution of voids in fine particles and materials - Capable of evaluating biological materials such as proteins - Allows for evaluation of samples under heating

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SCM/SNDM is a method that scans the surface of semiconductors using a conductive probe to visualize the carrier distribution in two dimensions. - SCM is sensitive to carrier concentrations of approximately 10^15 to 10^20 cm^-3, while SNDM is sensitive to concentrations of about 10^14 to 10^20 cm^-3. - It is possible to identify the polarity of the semiconductor (p-type/n-type). - A signal correlated with carrier concentration can be obtained, but quantitative evaluation is not possible. - AFM images can also be acquired.

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The white light interferometry measurement method is a device that enables non-contact (non-destructive) three-dimensional measurement of sample surfaces with "wide field of view, high vertical resolution, and wide dynamic range" using a high-brightness white light source. - Surface shape measurement device using a high-brightness white light source - Capable of three-dimensional measurement in a non-contact and non-destructive manner - Wide field of view (50μm×70μm to 5mm×7mm) - High vertical resolution (0.1nm) - Wide dynamic range (<150μm)

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We offer analysis seminars with technicians tailored to meet your needs. Depending on your requests, we can introduce analytical techniques and explain analysis data. The number of visiting technicians, seminar duration, and content can be customized according to your preferences. Please feel free to consult with us.

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ICP-MS allows for relatively easy preparation of standard samples that are difficult to produce for solid analysis, as it analyzes solutions. Therefore, it is frequently used for accurately quantifying trace inorganic elements in solutions. - It can detect the lowest concentrations (ppt or sub-ppt levels) due to its high sensitivity and low background, making it the most effective instrument for inorganic element analysis. (*: ppt: 10^-12 g/g) - It allows for flexible preparation of standard samples (standard solutions) that serve as a reference for quantitative analysis, resulting in lower uncertainty in the results. - It enables qualitative analysis by measuring many elements of the periodic table simultaneously. Additionally, it has a wide dynamic range, allowing for simultaneous analysis of major and trace components.

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TG-DTA simultaneously evaluates weight changes due to heating (TG) and thermal behavior of endothermic and exothermic reactions (DTA). Additionally, TG-DTA-MS continuously assesses volatile components (MS) along with TG and DTA evaluations. - TG allows for the detection of weight changes on the order of percentage. - DTA provides insights into reactions such as pyrolysis, melting, sublimation, oxidation, combustion, and phase transitions. - MS enables the structural estimation of volatile components and decomposition products.

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By irradiating an electron beam within a SEM device, electron-hole pairs are generated in the sample. Normally, these pairs recombine and disappear, but if they are generated in regions with an internal electric field, such as a depletion layer, the carriers can be drifted by the internal electric field and extracted as a current. This current is referred to as EBIC (Electron Beam Induced Current), and by obtaining it alongside the SEM image, it is possible to visualize the position of the pn junction and the extent of the depletion layer. - Evaluation of pn junctions and crystal defects (dislocations, stacking faults, etc.) is possible. - By overlaying with the SEM image, the positions of the junctions and crystal defects can be identified.

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EDX is a method for performing elemental and compositional analysis by detecting characteristic X-rays generated by electron beam irradiation and spectrally analyzing them by energy. It is also referred to as EDS: Energy Dispersive X-ray Spectroscopy. In many cases, it is attached to SEM or TEM, and this document will explain EDX attached to SEM. - The entire energy measurement range (from B to U) can be measured simultaneously in a short time. - It has excellent detection efficiency, allowing measurements with a low probe current. - Analysis can be easily performed without the need for pretreatment, except for special samples. - It is suitable for the analysis of unknown samples. - Measurements can be conducted in a frozen or cooled state using a cryo holder.

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EELS analysis is a method that measures the energy lost by electrons as they pass through thin samples due to interactions with atoms. It can analyze the constituent elements and electronic structure of materials. Compared to the elemental analysis device (EDX) attached to a TEM, it has the following features: - Better sensitivity for light elements compared to EDX - Higher energy resolution compared to EDX - Higher spatial resolution compared to EDX, making it difficult to detect surrounding information - Chemical state analysis is possible for certain elements

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- SIM imaging observation is possible with high resolution (accelerating voltage 30kV: 4nm). - Compared to SEM images, SIM images provide information about the extreme surface layer. - Observation of metal crystal grains is possible (e.g., Al, Cu). - The resolution is inferior to SEM images (SIM: 4nm, SEM: 0.5nm). ■Features of MST-owned equipment - Compatible with JEIDA standard wafers with a maximum sample size of 300mm in diameter. - Continuous cross-sectional SIM imaging acquisition is possible in combination with FIB (Focused Ion Beam) processing (Slice & View).

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SSRM is a method that visualizes the spreading resistance directly beneath the probe by scanning the surface of a sample with applied bias using a conductive probe and measuring the distribution of resistance values in two dimensions. When measuring silicon semiconductor devices, it is sensitive to carrier concentrations of 10^16 cm^-3 or higher, depending on spatial resolution. - Local resistance measurement at the nanometer level is possible - Effective for measuring the dopant concentration distribution in semiconductors - Cannot determine the polarity of semiconductors (p-type/n-type) - Quantitative evaluation is not possible

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FIB refers to a focused ion beam with diameters ranging from several nanometers to several hundred nanometers, which can be used to etch specific areas (sputtering) or deposit materials such as carbon (C), tungsten (W), and platinum (Pt) onto specific regions by scanning the sample surface. Additionally, the shape of the processed sample can be recognized through SIM images, which detect secondary electrons generated by irradiating the sample with the ion beam. - Arbitrary shape processing through etching in micro-regions (several nanometers to several tens of micrometers) is possible (typical processing size: around 20 μm) - Sample preparation for SEM, SEM-STEM, and TEM imaging (cross-sections of specific areas can be produced) - Fine pattern deposition and thin film formation (C, W, Pt deposition) are possible in the range of several micrometers to several tens of micrometers - High-resolution SIM (Scanning Ion Microscope) imaging is possible (acceleration voltage 30 kV: 4 nm) - Observation of metal crystal grains (Al, Cu, etc.) is possible with SIM images.

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The IP method is a technique that utilizes the sputtering phenomenon, where sample atoms are ejected from the sample surface when an ion beam with aligned energy and direction is irradiated onto the sample. The ion species used is typically a noble gas (Ar in MST) that does not pose concerns about chemical reactions with the sample. In the AES analysis of the processed surface, the components of the shielding plate (Ni, P) were below the detection limit.

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■Features ? By handling samples under atmospheric non-exposure, it is possible to minimize alteration and changes even for highly reactive samples. ? Cutting, peeling, and surface preparation under atmospheric non-exposure can reduce secondary contamination and oxidation from the atmosphere. ? Methods that can be evaluated under atmospheric non-exposure: SIMS, TOF-SIMS, AES, XPS, SEM, TEM, STEM, Raman, XRD, FIB, etc.

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Features - Soft samples can be hardened and machined by cooling. - Cooling to temperatures near liquid nitrogen is possible. - The temperatures of the sample, atmosphere, and microtome blade can be set independently. - It is mainly effective for processing soft materials (such as biological samples and polymer materials) at room temperature, and gel-like materials can also be processed by cooling.

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This is an introduction to a case study of SCM analysis of commercially available LSI internal MOSFETs. First, the cross-section of a specific transistor is exposed through mechanical polishing. At this time, the Si surface is polished flat to the order of nm. The SCM image allows for the two-dimensional confirmation of layer distribution. While quantitative discussions cannot be made, it is possible to roughly understand the relationship of concentration magnitudes. Additionally, the p/n polarity of the diffusion layer can also be identified. Furthermore, by conducting SEM observations at the same location and performing image synthesis with the SCM analysis results, the positional relationship between the diffusion layer and the upper wiring structure can be clarified.

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In SSRM, we can obtain insights into local resistance, while in EBSD, we can gain knowledge about crystal grains and grain boundaries. By conducting SSRM measurements at the same location as the EBSD measurements, we measured the local resistance in areas that include crystal grain boundaries, which we would like to introduce.

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By directly observing the junction interface using a Cs collector-equipped STEM device, it is possible to evaluate the crystal structure at the atomic level. In this study, we conducted HAADF-STEM imaging of the buffer layer/CIGS interface using Zn(S, O, OH) in the buffer layer of CIGS thin-film solar cells and evaluated the structure. As a result, it was suggested that the crystal structure at the junction is unclear compared to samples using CdS as the buffer layer, indicating that it is not an epitaxial junction.

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Organic devices are devices that use materials susceptible to the effects of oxygen and water. At MST, we conduct analyses with sample transport, processing methods, and measurement environments that minimize atmospheric influences, allowing for evaluations closer to true conditions. We assessed the interface state between the organic film and the electrode using XPS analysis. We can confirm the composition and bonding state of the titania present on the surface of the organic film. Through TOF-SIMS analysis, we examined the dispersion state of P3HT (p-type organic semiconductor) and PCBM (n-type organic semiconductor) within the organic film of bulk and heterostructure organic thin-film solar cells in the depth direction.

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When investigating the degradation mechanisms of secondary batteries, it is important to analyze the deposits on the electrode surface. At MST, we conduct TOF-SIMS measurements under controlled atmospheric conditions, allowing us to evaluate the chemical state of the electrode's outermost surface without alteration due to exposure to the atmosphere. Additionally, by consistently performing measurements from charge-discharge cycle tests to the electrode surface, we can examine the correlation between the state of charge-discharge and the condition of the deposits on the electrode surface.

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A degradation test was conducted on a battery cell made with LiCoO2 as the positive electrode, graphite as the negative electrode, and LiPF6/EC:DEC as the electrolyte, which was left in a constant temperature chamber at 60°C in a charged state of 4.2V for about one week. After that, the cell was disassembled and cleaned in an Ar atmosphere, and TOF-SIMS analysis of the negative electrode graphite was performed. Before the test, fragments derived from the binder and electrolyte salt were confirmed, and after the test, fragments such as Li3PO4 and PF3O, which are believed to have been generated due to the degradation of the electrolyte salt, as well as fragments from Li2CO3, were observed. Additionally, the detection of Co suggests the possibility of leaching of the positive electrode active material.

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This is an example of evaluating the organic solvent components of an electrolyte using GC/MS analysis. The measurement of the electrolyte in lithium-ion secondary batteries revealed that the main components of the organic solvents are ethylene carbonate (EC) and propylene carbonate (PC). Other components detected included diethyl carbonate (DEC) and sulfur compounds, with the latter possibly originating from additives.

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When measuring the distribution of alkali metals in SiO2 under general analytical conditions, it is known that changes occur in the depth profile concentration distribution due to influences such as the electric field caused by the measurement. In MST, by cooling the sample during SIMS measurements, we suppress changes in the concentration distribution of alkali metals and evaluate the concentration distribution with higher accuracy.

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The concentration distribution of boron (B) in silicon (Si), which significantly affects the characteristics of device design, can be evaluated with high sensitivity and high depth resolution through SIMS analysis. However, it has been found that under general analysis conditions, distortions occur in the concentration distribution of B due to measurement-related factors. In MST, it has been confirmed that sample cooling is effective for correcting these distortions, enabling a more accurate evaluation of the concentration distribution.

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Substances composed of carbon include those with crystalline structures such as diamond, graphite, carbon nanotubes, and graphene, as well as those with amorphous structures like diamond-like carbon (DLC). Raman spectroscopy is effective for the structural identification, crystallinity, and sp3 character evaluation of these materials.

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Ergothioneine, an amino acid homologue found abundantly in edible mushrooms of the Pleurotaceae family, is gaining attention in the fields of food, medicine, and beauty as a natural substance with high antioxidant properties. Recently, chemical synthesis techniques have also been established, but there is still a need for the development of high-efficiency separation and purification techniques from natural food resources, and it is required to accurately measure the yield and evaluate the level of purification.

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Measuring hair and obtaining the distribution of components within it is effective when investigating the effects of hair care and dyeing. We will introduce a case where gray and black hair were collected from the same individual and the internal component distribution was evaluated. A cross-section of the hair was created, and TOF-SIMS measurements were conducted. TOF-SIMS can provide distribution information on inorganic substances such as metals and organic molecules. This time, we focused on measuring the distribution of metals in the hair cross-section.

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It is possible to observe in detail from an overview of the NPN bipolar transistors within commercially available LSI to an enlarged view of the emitter section. This is an example where a cross-section passing through the center of the emitter electrode was exposed, and AFM observation and SCM measurement were conducted. By overlaying the AFM image, the positional relationship with the wiring becomes clear.

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In recent years, with the introduction of lead-free solder, the flux components have also been improved (with higher activity and heat resistance, etc.), leading to increased corrosiveness and a growing importance of residue issues. Therefore, the removal of flux is required. An analysis of foreign substances in the electrode parts of printed circuit boards using TOF-SIMS revealed the presence of flux components.

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In the mass production of LCD panels, it is necessary to remove defects (foreign substances and dirt). Therefore, investigating the causes of these foreign substances and dirt is effective for improving yield. Here, we introduce a case study evaluating foreign substances and dirt on LCD panels. TOF-SIMS can capture cleaning residues in the order of micrometers to centimeters as images. Additionally, by comparing with standard spectra, it is possible to estimate the components.

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Raman spectroscopy is an effective method for the qualitative analysis of microscopic foreign substances. When it becomes difficult to evaluate due to the detection of background information along with the foreign substances, measurements can be performed by combining sampling. Foreign substances on electrodes with minimal background influence were identified as flux, but no information from the foreign substances could be obtained from the foreign substances on printed circuit boards (Figure 1). By performing sampling on inorganic crystals without background influence, information about the foreign substances was obtained, and the foreign substances were identified as flux (Figure 2).

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It was found that there are water-repellent stains on the surface of the aluminum material. The stained area was adhered to tape (transferred), and analysis was conducted using TOFSIMS. Fragments identical to those from the stained area on the aluminum surface were detected from the "tape surface where the stained area was transferred," suggesting that the substance causing the stain has been transferred to the tape. This method of transferring and collecting the causative substance onto tape is effective for parts that cannot be cut.

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There are various types of fluorine-based compounds. During the investigation of contamination sources, performing qualitative analysis of the types of fluorine compounds allows us to examine the processes that caused the contamination. Therefore, we conducted an analysis using surface-sensitive TOF-SIMS to determine what is adhering to areas with good water repellency. By utilizing the fact that the fragment patterns of the fluorine-based oils used in each process differ by type, we performed a fingerprint matching and found that a substance corresponding to the oil from process B was adhering.

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Residue from adhesive tape can cause poor adhesion and peeling during the manufacturing process. When residue is suspected to be the cause of defects, TOF-SIMS, which can analyze the composition and distribution of surface contaminants, is effective. We will present a case where the surface of a silicon wafer was adhered with adhesive tape and measured with TOF-SIMS after peeling it off.

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In oxide ReRAM, it was suggested that oxygen diffusion associated with the application of an electric field is related to memory operation (resistance change). Since SIMS analysis allows for the measurement of isotopes, utilizing the isotope 18O ion implantation technique enables the tracking of oxygen diffusion. For devices where 18O was locally implanted, a bridge structure that serves as the operating region was formed by applying an electric field, and elemental mapping revealed that the intensity of 18O in the bridge area was weak, indicating localized reduction.

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An example is shown where secondary ion mass spectrometry (SIMS) was used to analyze the intersection (4μm×10μm) of the data signal wiring and gate electrode wiring of a commercially available TFT LCD from the substrate side (SSDP-SIMS). By measuring from the substrate side (SSDP-SIMS), it becomes possible to provide data free from the influence of high-concentration layers or metal films on the surface side.

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The Fast Fourier Transform Mapping method is a technique that performs a Fourier transform on high-resolution TEM images to analyze and visualize the minute lattice distortions of crystals from the spot positions of the FFT pattern. Through FFTM analysis, it is possible to (1) analyze lattice distortions in the x and y directions of the image, (2) analyze lattice distortions in the crystal plane direction, (3) analyze the distribution of crystal plane spacing and crystal plane orientation, (4) display the data distribution as a histogram, and (5) detect distortions of 0.5% with a spatial resolution of 5 nm. An example of its application to compound heterojunction multilayer film samples is presented.

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A scanning white light interferometer (optical interferometer) can perform high-precision, non-contact three-dimensional measurements of the surface shape of a sample with "high vertical (Z) resolution (0.1 nm) and a wide (X-Y) measurement field of view (50 μm to 4.2 mm)." It is capable of measuring up to a field of view of 4.2 mm × 4.2 mm.

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A scanning white light interferometer (optical interferometer) can perform high-precision non-contact three-dimensional measurements of the surface shape of a sample with "high vertical (Z) resolution (0.1 nm) and a wide (X-Y) measurement field of view (50 μm to 4.2 mm)." An example of observing the surface shape of a Si/SiGe layered sample (crosshatch pattern) is presented. Shape evaluation with an average roughness (Ra) of approximately 1 nm is possible.

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Using TOF-SIMS for ion imaging analysis of hair (beard) cross-sections, we investigated the distribution of long-chain fatty acids, which are also detected as sebum. As a result, it was found that the distribution varies depending on the type of fatty acid.

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We analyzed the hair cross-sections of five individuals (A to E) who use different hair care products in their daily lives using TOF-SIMS. As a result, it was found that the types of hair care products lead to differences in the detected components and their distribution within the hair.

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