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[Analysis Case] Evaluation of Si Anode in Lithium-Ion Secondary Batteries

It is possible to evaluate the structure of the Si anode after charging through sample cooling.

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

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[Analysis Case] Evaluation of Lithium-Ion Secondary Battery Separators

Cool the sample and evaluate the shape of the separator more accurately.

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

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[Analysis Case] Photoluminescence Mapping Measurement of SiC Diodes

Detection cases of stacking faults in SiC.

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

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[Analysis Case] Diffusion Evaluation of Ga and Al in Si Substrate using SSDP-SIMS

Measurement avoiding the influence of high concentration layers using SSDP-SIMS.

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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[Analysis Case] Evaluation of Element Distribution in Textured GaN-based LEDs

Even with a structure that has uneven surfaces, depth distribution evaluation is possible through flattening processing.

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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[Analysis Case] Dopant Investigation in NPT-IGBT Using SIMS

Evaluation of localized elements is possible with imaging SIMS.

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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[Analysis Case] Evaluation of Gate Oxide Film on SiC Substrate

Evaluate film thickness, density, and bonding state.

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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[Analysis Case] Numerical Evaluation of Active Material Volume by Three-Dimensional SEM

It is possible to calculate the volume of each substance from Slice&View data.

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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[Analysis Case] Evaluation of Contact Electrodes for SiC Power MOSFETs

Identification of the interface between contact electrodes and SiC layer, and evaluation of elemental distribution.

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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[Analysis Case] Lock-in Thermal Analysis of Package Products

Non-destructive analysis of leakage points in Si-based power diodes.

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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About Cryo-SEM

Cryo-processing cooling SEM: Scanning Electron Microscopy method

To observe the structure of liquid samples, it is necessary to conduct a series of analyses while maintaining the original structure of the sample. In cryo-SEM, the sample can be observed by rapidly freezing it to create a cross-section. Furthermore, by combining this with cross-section fabrication techniques using FIB processing, it is possible to obtain more detailed information about the internal structure.

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[Analysis Case] Evaluation Case of Hydrogen Injection Sample using SRA/SIMS

Introduction to Case Studies on Carrier Concentration Analysis in Lifetime Control Samples

In power semiconductor devices, crystal defects may be formed within the Si substrate for lifetime control. This presents a case study evaluating the carrier concentration distribution due to differences in thermal treatment conditions of hydrogen ions, one of the elements used to create the lifetime control region.

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[Analysis Case] Simultaneous Analysis of Polyphenols in Eucommia Tea

Examples of the detection of active ingredients in health foods.

In recent years, with the increase in health consciousness, various health foods have been attracting attention. One of these, Du Zhong tea, is suitable for individuals with high blood pressure and is designated as a Food for Specified Health Uses (Tokubetsu Hōshō). In this case study, Du Zhong tea was analyzed using LC/MS/MS, and five polyphenols were detected: geniposidic acid, chlorogenic acid, asperuloside, p-coumaric acid, and quercetin. Among these components, geniposidic acid, one of the glycosides from Du Zhong leaves, serves as a benchmark for the effective ingredient of Foods for Specified Health Uses.

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Large-diameter imaging SIMS using RAE detectors

SIMS: Secondary Ion Mass Spectrometry

Imaging SIMS is effective for obtaining spatial distribution information of hydrogen and impurities at ppm levels. By using a RAE (Resistive Anode Encoder) detector for projection-type imaging SIMS, it is possible to obtain distribution images with a larger diameter and deeper regions compared to the commonly used scanning methods in imaging analysis.

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[Analysis Case] Screening Test for Contaminants in Food

We analyze with high precision whether pesticides and drugs are mixed in food.

Incidents of foreign substances contaminating food have frequently caused public uproar, and in a Cabinet Office survey conducted in January 2014 regarding the promotion of consumer administration, the consumer issue that garnered the most attention was "food safety." To ensure food safety, MST conducts highly accurate analyses for cause investigation, making it possible to determine whether pesticide levels in food exceed the acceptable daily intake. An analysis of miso soup with a small amount of the herbicide glyphosate added revealed that the contaminant could be detected without overlooking any components.

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[Analysis Case] Quantitative Analysis of Vitamin B1 and Vitamin B2

Testing of content using HPLC method with fluorescence detector (official method)

Foods such as pork and eggs are rich in vitamin B1 (thiamine, HET) and vitamin B2 (riboflavin). These are often present as derivatives such as phosphate esters. The content of vitamin B1 and vitamin B2 can be quantified by performing enzymatic treatment as a pretreatment to convert them to their free forms, followed by analysis using HPLC with a fluorescence detector. Although vitamin B1 itself is not fluorescent, it is possible to detect fluorescence by reacting it with a red blood salt alkaline solution in a post-column method, converting it to the oxidized form of thiocrome.

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[Analysis Case] Depth Direction Analysis of Thin Carbon Films

Depth-direction analysis of diamond-like carbon (DLC) and graphene is possible.

TOF-SIMS allows for the acquisition of mass spectra in the depth direction, enabling the analysis of components in very thin layers through qualitative assessment of each layer. In this case, we analyzed a hard disk in the depth direction. As a result, it was found that the diamond-like carbon (DLC) layer formed on the surface has a two-layer structure, with a nitrogen-containing C layer on the surface side and a layer consisting solely of C on the deeper side. This method can also be applied to the depth analysis of graphene films. Measurement method: TOF-SIMS Product fields: Electronic components, manufacturing equipment, parts Analysis objectives: Composition evaluation, identification, composition distribution evaluation For more details, please download the materials or contact us.

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[Analysis Case] Analysis of H termination on Si surface

Qualitative and relative comparison of SiH and states on the Si surface due to differences in processing.

We compared the states of the Si surface after HF treatment and after ozone treatment. In the positive ion spectrum, the peak intensity of Si was different. The weaker Si intensity after HF treatment is due to Si being metallic, while the stronger Si intensity after UV-ozone cleaning and in the As Received state is due to Si being oxide-based. From the negative ion spectrum, fragment ions reflecting the surface state were detected: SiF, SiH, and Six series after HF treatment, and SiO2 series after UV-ozone cleaning and in the As Received state.

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[Analysis Case] Evaluation of Odor Components in Essential Oils

Concentration analysis of odor components using solid-phase microextraction (SPME).

The concentration of volatile components that humans perceive as odors can be very low, and they may not be detectable using the conventional HS (Headspace) method for GC/MS measurements used for analyzing volatile components. By using Solid-Phase Micro Extraction (SPME), it becomes possible to concentrate the volatile components and introduce them into GC/MS, allowing for the detection of many trace components. This document presents a case study analyzing odor components in trace amounts of essential oils.

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[Analysis Case] Evaluation of Carrier Distribution in Near-Infrared VCSEL Using SMM

We can consistently perform everything from disassembly and processing of the implemented product to measurement of the diffusion layer.

We disassembled a near-infrared VCSEL (vertical-cavity surface-emitting laser) implementation to extract a tiny chip, and after cross-section processing, we conducted SMM measurements. A high-resistance current confinement layer was observed surrounding the aperture of the VCSEL. Additionally, near the active layer, films of different materials were stacked, and this composition was measured as a contrast. Contrast was also confirmed within layers of the same composition, which is believed to reflect differences in carrier concentration and band bending.

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[Analysis Case] Evaluation of Impurity Concentration in Gallium Oxide Ga2O3 Films Using SIMS

It is possible to quantitatively evaluate impurity elements.

Gallium oxide (Ga2O3) has a higher band gap and superior physical properties compared to SiC and GaN, making it a material of interest for power devices that can be expected to be high-efficiency and low-cost. Controlling the impurity concentration, which affects the characteristics, is crucial in wafer development. This document presents a case study of impurity concentration analysis in Ga2O3 films. It is found that B and C are below the background level, while Si is present. MST offers a range of Ga2O3 standard samples and can quantify over 30 types of impurities.

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[Analysis Case] Evaluation of Liquid Inside Smartphone Cases

Non-target analysis of liquid components using GC/MS is possible.

Products containing liquid in smartphone cases are being sold, but there have been incidents of skin injuries such as chemical burns due to leaks of this liquid, as well as cases of people experiencing health issues due to unpleasant odors. In response, the National Consumer Affairs Center issued a warning in April 2016, and in some cases, liquids with modified ingredients have been used. Here, we conducted non-target analysis using GC/MS on the liquid inside cases that were sold before the warning was issued to investigate what components are present.

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[Analysis Case] Evaluation of Carrier Concentration Distribution in Si-IGBT Chips

SRA evaluation of field stop layers and lifetime killers.

SRA can analyze the depth profile of carrier concentration distribution over a wide range from shallow regions (a few hundred nm) to deep regions (a few hundred μm). It is also possible to evaluate the in-plane distribution of resistance values at the sample surface or at specified depths. As an example, we will introduce a case where the depth profile of carrier concentration distribution for a commercially available Si-IGBT chip was evaluated, including the entire chip, the field stop layer, and the lifetime killer, as well as the in-plane distribution of resistance values at the irradiation depth of the lifetime killer using SRA.

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Analysis of trace metal elements in the environment

ICP-MS: Inductively Coupled Plasma Mass Spectrometry

Metal elements suspended in environments such as clean rooms and production lines can adhere to or contaminate products, potentially leading to a deterioration in product performance. With ICP-MS, exposure tests can be conducted on clean Si wafers, allowing for the measurement of the amount of metal elements adhered to the surface at ppt levels. Additionally, we also offer the loan of Si wafers that have been pre-cleaned.

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[Analysis Case] Evaluation of Organic Contamination of Wafers in Wafer Cases

You can evaluate the causes and total amount of organic contamination in the manufacturing process.

It is known that the adsorption of organic substances on the wafer surface can lead to various issues, such as the degradation of gate oxide film breakdown voltage. Therefore, as the miniaturization and high integration of semiconductor devices progress, it has become increasingly important to monitor not only inorganic substances but also trace amounts of organic substances. Here, we present a case where silicon wafers were stored in two types of wafer cases, and the organic contamination components adhered to the entire wafer surface were concentrated using a wafer analyzer and evaluated using GC/MS.

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Shotgun analysis of proteins

LC/MS/MS: Liquid Chromatography-Mass Spectrometry

In protein composition analysis, there are methods to examine only the target protein after electrophoresis, but this document introduces "shotgun analysis," which comprehensively investigates proteins. In shotgun analysis, after separating proteins and obtaining mass information using LC/MS/MS measurements, a database search is conducted to comprehensively analyze the proteins present in the solution.

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[Analysis Case] Evaluation of Pharmaceutical Crystal Polymorphism

It is possible to evaluate the structure of crystalline polymorphs.

The majority of pharmaceuticals are crystalline and are known to have multiple crystal forms. Even for the same substance, the physical and chemical properties, such as solubility, can differ depending on the crystal form, which can also affect the efficacy and safety of the drug. Therefore, the identification of crystal forms is extremely important. In this case, XRD analysis was conducted to evaluate the crystal forms of the active pharmaceutical ingredient in question, both for the pure active pharmaceutical powder and for the commercial products.

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Sample introduction method in Karl Fischer volumetric titration.

Karl Fischer titration method

The Karl Fischer titration method is a way to evaluate the moisture content, and the method of introducing the sample into the device varies depending on the properties of the sample. Here, we will introduce two sample introduction methods for titration.

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[Analysis Case] Evaluation of Band Structure by X-ray Absorption and Emission Spectroscopy

Detailed information about the valence band, conduction band, and gap states of the material can be obtained.

Understanding the band structure, including valence bands, conduction bands, and gap states, is an extremely important evaluation criterion for controlling various properties of materials. However, there are limited analytical methods available for direct and detailed assessment of these aspects. Simultaneous measurements of X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) using synchrotron radiation allow for a comprehensive understanding of the band structure, as well as detailed information regarding the attribution of the elements and orbitals that compose it. This document presents the XAS and XES spectra of GaN substrates as an example of measurement.

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[Analysis Case] Analysis of Fucoidan Food Standards and Specifications

MST is a designated testing organization for the JHFA standard (fucoidan food).

Fucoidan is a high molecular weight polysaccharide found in seaweeds, and various functional properties, including anti-cancer effects, have been reported. The Japan Health and Nutrition Food Association (JHFA) announced the standards for fucoidan foods in July 2017, and MST was registered as a designated testing institution capable of conducting the necessary analyses. The JHFA standards specify fucoidan food regulations for three types: Okinawa mozuku, mekabu, and gagome kombu. The testing items include not only the fucoidan content in raw materials and products but also tests to confirm the safety of the products, such as arsenic and bacterial count tests.

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analysis Product List and Ranking from 179 Manufacturers, Suppliers and Companies | IPROS GMS

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