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

- Qualitative and quantitative analysis of solid material surfaces (depth of several nm) is possible. - Qualitative and quantitative analysis of micro-regions (approximately tens of nm to sub-micron) is possible. - Depth profile analysis, line analysis, and area analysis of major component elements can be measured. - For several elements such as Si and Al, evaluation in both oxide and metallic states is possible. - Identification of specific areas of interest using SEM images is possible.

SEM is a technique that allows for obtaining contrast based on the information from electrons emitted from a sample when an electron beam is directed at it, revealing the sample's surface roughness and compositional differences. - High magnification observation (up to about 500,000 times) is possible with simple operation. - Observation of secondary electron (SE) images, backscattered electron (BSE) images, and transmitted electron (TE) images is possible. - Observation can be conducted within an acceleration voltage range of 0.1 to 30 kV. - Samples up to 6 inches can be loaded into the device (depending on the equipment). - By combining options with SEM, various types of information can be obtained: - Elemental analysis using an EDX detector is possible. - Measurement of electron beam induced current (EBIC) allows for evaluation of the junction position and shape in semiconductors. - Crystal information can be obtained using electron backscatter diffraction (EBSD) method. - Three-dimensional structural information can be acquired through repeated FIB processing and SEM observation (Slice & View). - Cooling observation and atmosphere-controlled observation are available.

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.

This is a method for orientation analysis of crystalline samples using EBSD. It allows for easier and broader acquisition of crystal information compared to electron diffraction methods. EBSP: Electron Backscatter Pattern, also referred to as SEM-OIM or OIM. - Measurement of the surface orientation of single crystal grains is possible. - Orientation measurement of the measurement area is possible. - Observation of crystal grain size is possible. - Observation of twin grain boundaries (corresponding grain boundaries) is possible. - Extraction of specific crystal orientations is possible. - Measurement of the rotation angle of adjacent crystal grains is possible. - Evaluation of grains larger than 10 nm is possible using transmission methods.

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.

Using a high-resolution SEM device equipped with FIB, we can obtain three-dimensional structural information by repeatedly performing cross-sectioning (Slice) with FIB and observing (View) with SEM, and then reconstructing the acquired images. Similarly, Slice & View is also possible for SIM (Scanning Ion Microscope) images. - It is possible to observe secondary electron (SE), backscattered electron (BSE) images, and scanning ion microscope (SIM) images.

TEM (Transmission Electron Microscopy) is a method that involves irradiating a thin sample with an electron beam, imaging the electrons that have passed through or scattered from the sample, and observing it at high magnification. ■ Advantages - Enlarged images can be obtained with sub-nanometer spatial resolution, allowing for the observation and analysis of the sample's fine structure and lattice defects. - It is possible to evaluate the crystallinity of the sample and identify materials. - By fabricating samples using FIB (Focused Ion Beam), it is possible to observe specific locations within a device with pinpoint accuracy. - By combining optional features, it is also possible to analyze the composition and state of localized areas. ■ Disadvantages - It is necessary to thin the sample (in some cases, thinning may be difficult for certain samples). - It does not observe individual atoms but rather displays average information in the thickness direction of the sample (typically about 0.1 μm thick). - Sample processing and observation may lead to alteration or deformation of the sample.

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

ED is a method for investigating crystal structures from diffraction patterns obtained by irradiating a sample with an electron beam. - Crystallographic information about the material can be obtained. In the case of a transmission electron microscope, a single crystal shows regularly arranged diffraction spots, a polycrystal shows concentric circular rings, and an amorphous material shows broad circular electron diffraction patterns. - It is possible to examine the crystal structure of small regions observed with a transmission electron microscope. - By combining the crystal structure with elemental analysis results from the EDX method, it is also possible to identify materials that possess crystallinity.

- 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).

EDX is a method that measures the energy and occurrence of characteristic X-rays generated when an electron beam is irradiated onto the analysis target area, allowing for elemental and compositional analysis. It is also referred to as Energy Dispersive X-ray Spectroscopy (EDS). In many cases, it is attached to a SEM or TEM, and this document introduces the EDX that accompanies the TEM. - Simultaneous analysis of the entire range of elements (from B to U) is possible (detection of Be is also possible depending on the attached device). - Measurements can be made with a fine electron beam probe of 0.1 nm in diameter or smaller. - By using drift correction functionality, sub-nanometer layered films can be identified as distribution images in surface analysis. - In surface analysis, it is possible to extract spectra from arbitrary locations and display line analysis.

Understanding the degradation mechanism of liquid crystal display panels is an essential theme for extending the lifespan of the panels. Among the degradation symptoms, a decrease in brightness can be attributed to various factors, including liquid crystals, alignment films, sealing materials, and TFTs. A comprehensive analysis will be conducted, incorporating surface, structure, composition, and computational science. By capturing the slight differences between good and defective products and conducting a comprehensive evaluation, we can elucidate the degradation mechanism of liquid crystal displays.

We observed a sample mixed with three types of lactic acid bacteria using SEM, and extracted the bacteria by type using deep learning from the obtained images. Furthermore, we conducted data analysis to determine the presence ratio on the cell cycle based on the shape of the lactic acid bacteria. Measurement methods: SEM, computational science, AI, data analysis Product fields: Biotechnology, pharmaceuticals, daily necessities, cosmetics, food Analysis purpose: Shape evaluation, product investigation For more details, please download the materials or contact us.

By scanning the electron beam probe and measuring the electron diffraction patterns at each point, high spatial resolution crystal information can be obtained. This method allows for the acquisition of information on smaller crystal grains than the EBSD method in SEM. It is also referred to as ACOM (Automated Crystal Orientation Mapping) - TEM method. - Crystal grain size analysis is possible - Orientation measurement of the measurement area is possible - Observation of twin grain boundaries (corresponding grain boundaries) is possible - Extraction of specific crystal orientations is possible - Measurement of the rotation angle of adjacent crystal grains is possible - Evaluation of crystal grains larger than a few nanometers is possible

GaN-based high electron mobility transistors, known as GaN HEMTs (High Electron Mobility Transistors), utilize an AlGaN/GaN heterostructure to achieve a two-dimensional electron gas layer (2DEG), resulting in high electron mobility. They are used in applications such as fast chargers, leveraging these characteristics. This document presents the disassembly and evaluation of normally-off GaN HEMT devices. We will introduce a case study that employs a combination of analytical methods to gather comprehensive insights about the samples. Measurement methods: SIMS, TEM, SCM, SMM. Product field: Power devices. Analysis objectives: Trace concentration measurement, shape evaluation, film thickness evaluation, structural evaluation, product investigation. For more details, please download the document or contact us.

Power devices are attracting attention from the perspective of power and energy conservation as switches for high voltage and large current. In power devices, wiring defects and electrical failures occur due to the application of high voltage. Additionally, identifying and analyzing the causes of defects is essential for improving product reliability. This document presents a case study where the identification of defective areas was conducted using EMS (Emission Microscopy Method), and the analysis of defect causes was evaluated using SCM (Scanning Capacitance Microscopy) and SEM (Scanning Electron Microscopy). Measurement methods: EMS, SCM, SEM Product field: Power devices Analysis purpose: Failure analysis and defect analysis For more details, please download the document or contact us.

For the SiC transistor, where the leak location was identified using a backside emission microscope, cross-sectional SEM observation was conducted using Slice & View. With Slice & View, it is possible to capture images of the leak location without missing it by performing cross-sectional observations at a pitch of several tens of nanometers around the leak area. By converting the SEM images into 3D, the leak path can be confirmed. Measurement method: Slice & View, EMS Product area: Power devices Analysis purpose: Failure analysis, defect analysis, product investigation For more details, please download the materials or contact us.

We conducted Slice & View on a SiC transistor where the leak location was identified using a backside emission microscope, and performed magnified observation and SEM-EDX analysis at the confirmed destruction site. Bright contrast was observed in the reflected electron images, indicating the segregation of Si and Ni. It is believed that some segregation of elements such as Si and Ni occurred due to the destruction caused by the leak. Measurement methods: Slice & View, SEM-EDX, EMS Product field: Power devices Analysis purpose: Failure analysis, defect analysis, product investigation For more details, please download the materials or contact us.

By analyzing characteristic X-rays using a wavelength dispersive X-ray spectrometer (WDX), measurements with higher sensitivity than those obtained with an energy dispersive X-ray spectrometer (EDX) can be achieved. Additionally, using soft X-ray emission spectroscopy (SXES) allows for the acquisition of information regarding local chemical bonding states.

- Possible to identify high resistance abnormal areas - The current flowing through the wiring is weak (pA) - Measurement is possible even with a surface protective film present - Measurement is possible even with multilayered wiring - Measurement is possible under conditions almost identical to SEM observation

It achieves high positional accuracy and wide-area cross-section production, making it usable as a new large-capacity analysis application. Even small structures within a large area can be targeted for processing, enabling wide-area structural analysis.

The separator, which is a key component material of batteries, 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 composite materials have low softening points, with PE being around 125°C and PP around 155°C. We will introduce a case where the structure of a PP separator with a low softening point was observed, and cooling was performed during cross-section processing to suppress degradation for evaluation.

High-resolution HAADF-STEM images reflect the atomic arrangement of crystals, and by simulating STEM images corresponding to various crystal orientations, they help in accurately understanding the relative orientations between crystal grains and the observed images in polycrystalline materials. This document presents a case where STEM images were simulated from the crystal orientation information obtained by the EBSD method for the crystal grains in a polycrystalline neodymium magnet, and compares them with actual high-resolution HAADF-STEM images.

Next-generation all-solid-state batteries, which are lithium-ion batteries, are expected to have high safety, high energy density, high output, and a wide operating temperature range. In recent years, research and development aimed at practical application has been actively conducted, but there are various development challenges. At MST, we propose evaluation content suitable for solving development challenges based on comprehensive analysis and evaluation of structure, composition, and electrical properties. This document introduces specific examples of development challenges for all-solid-state batteries, their evaluation content, and representative evaluation methods for each component.

The separator in lithium-ion secondary batteries not only serves the role of isolating the positive and negative electrodes to prevent internal short circuits, but in automotive batteries, it is also required to have heat resistance to prevent a decrease in strength or melting even in high-temperature environments. This report introduces a case study on separators used in overseas automotive batteries, where heat resistance and thermal decomposition behavior were investigated using TG-DTA, and structural and compositional evaluations were conducted using SEM-EDX, FT-IR, XPS, TOF-SIMS, and XRD. It was found that the separator used in the battery consists of a porous polyethylene and a layered structure of polygonal AlO(OH) aimed at heat resistance.

The charge and discharge characteristics of lithium-ion secondary batteries are influenced by electronic conductivity. I will introduce a case where the decreased conductivity of active materials, due to degradation or blockage of conduction paths, was visualized as a resistance value distribution using SSRM. By comparing the results obtained from SSRM with the elemental distribution of Li and other elements measured by TOF-SIMS, it is possible to confirm the correlation between resistance values and elemental distribution. Additionally, it is feasible to classify conductive additives and binders based on resistance values, perform statistical processing, and quantify the mixing degree for each material.

This article introduces a case study evaluating the surface morphology, cross-sectional structure, components, composition, crystal structure, and resistance value distribution of Li(NiCoMn)O2 (NCM), which is used as a positive electrode in lithium-ion secondary batteries. Based on a comprehensive evaluation of structure, composition, and electrical properties, MST proposes assessments suitable for solving development challenges aimed at improving characteristics and enhancing reliability.