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[Analysis Case] Cross-sectional Observation and Elemental Analysis of Soft Materials

Direct evaluation of the structure of solution samples through cryo-SEM observation and EDX analysis.

To observe and analyze the internal structure of organic materials and liquid samples that are sensitive to heat, it is necessary to suppress temperature increases caused by processing or electron beam irradiation and to conduct a series of analyses while maintaining the original structure of the sample. In this case study, we will introduce an example where a cosmetic was used as an evaluation sample, and structural analysis was performed from cross-section FIB processing to SEM observation and EDX analysis while maintaining a cooling environment.

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[Analysis Case] Observation of Emulsions in Cryo FIB-SEM Processed Food

Observe the dispersion state of moisture and oil while maintaining the structure.

Emulsions are dispersion systems in which water-soluble and fat-soluble components are mixed without separation due to the action of emulsifiers, and various emulsion technologies are widely used in processed foods. Mayonnaise is a representative processed food of the O/W type (oil-in-water emulsion). As a result of evaluation using cryo FIB-SEM observation, we were able to visualize the distribution of water, oil, emulsifiers, and other components. By conducting magnified observations, we can evaluate the fine structure, which is expected to be applied to sensory evaluations such as the smoothness and flavor of food.

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[Analysis Case] Structural Evaluation of Magnetic Head MTJ Section

High-resolution TEM observation using Cs-corrected TEM

By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. In this case, we present data from high-resolution (HR)-TEM observations of the MTJ: magnetic tunnel junction part, extracted from a commercially available hard disk. Thus, it is possible to clearly observe the structure even in multilayer structures of ultra-thin metal films.

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[Analysis Case] Atomic Level Structural Analysis of CIGS Thin-Film Solar Cells

Atomic-level resolution EDX analysis using Cs-corrected STEM.

By using a Cs-corrected TEM device that compensates for spherical aberration, it is possible to observe the cross-sectional structure of devices with high resolution. This case presents data from high-resolution (HR)-STEM observation and EDX elemental distribution analysis of the light-absorbing layer of CIGS thin-film solar cells. In CIGS, which has a polycrystalline structure composed of four elements, atomic resolution EDX analysis was performed, visually revealing the distribution of atoms.

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[Analysis Case] Observation of Fine Structures under Ultra-Low Acceleration Voltage Conditions using SEM

Evaluation of separator structure by ultra-low acceleration SEM observation.

As exemplified by the separators used in lithium-ion secondary batteries, the microstructure of materials, such as porosity and shape, significantly influences the characteristics and functions of products. When materials have a low softening point, such as resins or polypropylene (PP), they may be damaged by electron beam irradiation during observation, leading to changes in their original structure. We will present a case where ultra-low acceleration SEM observation at an acceleration voltage of 0.1 kV was used to suppress alteration and evaluate the surface morphology of the sample in detail.

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[Analysis Case] Evaluation of Particle Size and Composition of Catalyst Materials using TEM and EDX

Evaluation of catalyst particles using STEM-EDX.

The electrodes of fuel cells are supported by Pt particles or Pt alloy (such as PtRu) particles as catalysts on carbon. Due to the fine structure of these catalyst particles, which are on the order of a few nanometers, SEM and TEM analyses are used for morphological observation and compositional analysis. In addition to evaluations in the initial state, degradation after current application has been reported, including modulation of alloy composition, leaching of Ru, and an increase in the diameter of catalyst particles; HAADF observation and high-resolution EDX analysis are very effective for these evaluations. Furthermore, multi-field observation and analysis enable the assessment of particle size and compositional distribution.

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[Analysis Case] Atomic Column Observation of Strontium Titanate SrTiO3

High-resolution STEM observation using Cs-corrected STEM

ABF-STEM images (scanning transmission annular dark field images) allow for the direct observation of atomic positions of light elements. Simultaneous acquisition with HAADF-STEM images enables more detailed structural analysis. In this case, we present an example of observing atomic columns of strontium titanate (SrTiO3). By combining EDX elemental distribution analysis, we can visually clarify the distribution of atoms. Measurement methods: TEM・EDX Product fields: LSI・Memory Analysis purposes: Shape evaluation・Structural evaluation For more details, please download the materials or contact us.

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$Types and Characteristics of Electron Diffraction$

Types and Characteristics of Electron Diffraction

TEM: Transmission Electron Microscopy

The electron diffraction method using an electron microscope is classified into three types based on the way the electron beam is incident on the sample. The characteristics of each type and examples of data are presented. It is necessary to choose the appropriate method according to the size of the evaluation object and the analysis purpose.

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[Analysis Case] Polarity Evaluation of GaN by ABF-STEM Observation

Atomic-level observation is possible with the Cs collector-equipped STEM.

GaN, which is being utilized as a power device and optical device, has a hexagonal wurtzite structure and exhibits crystallographic asymmetry (Ga polarity and N polarity) in the c-axis direction. The growth processes of epitaxial films differ between Ga polarity and N polarity, and the surface physical properties and chemical reactivity of the crystal also vary. In this document, the polarity of GaN was evaluated through annular bright field (ABF)-STEM observation. As a result, the positions of the Ga sites and N sites were identified, allowing for a visual clarification of the characteristics of Ga polarity and N polarity. Measurement method: TEM Product fields: Power devices, optical devices Analysis objectives: Shape evaluation, structural evaluation, thickness evaluation For more details, please download the document or contact us.

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[Analysis Case] Evaluation of High Electron Mobility Transistors

Evaluation of crystal coherence and compositional distribution is possible with Cs collector attached STEM.

GaN-based high electron mobility transistors, known as GaN HEMTs (High Electron Mobility Transistors), achieve a two-dimensional electron gas layer through an AlGaN/GaN heterostructure, resulting in high electron mobility. This document presents a case study of the disassembly and evaluation of commercially available GaN HEMT devices. Using HAADF-STEM, we confirmed the crystallographic integrity near the AlGaN/GaN interface. Additionally, we assessed the compositional distribution using EELS. Measurement methods: TEM, EELS. Product field: Power devices. Analysis purpose: Structural evaluation, film thickness evaluation. For more details, please download the document or contact us.

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[Analysis Case] Atomic Resolution Analysis of Lithium-Ion Secondary Battery Cathode Materials

Atmosphere control + atomic-level observation under cooling

In MST, atomic-level TEM analysis is possible under atmosphere control (and cooling). This document presents a case where LiCoO2 particles, extracted from a lithium-ion secondary battery without exposure to the atmosphere, were processed using FIB and analyzed with TEM under atmosphere control and cooling. STEM observation and EDX analysis were conducted while cooling to -174°C, allowing for a visual confirmation of the atomic arrangement. This method can be applied to materials with low thermal stability and crystalline materials that undergo changes in the atmosphere for high-resolution analysis.

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[Analysis Case] Observation of Fine Surface Morphology of Three-Dimensional Cultured Human Skin

Visualization of nanoscale roughness on the skin surface using AFM.

In recent years, the development of alternative methods to animal testing for the efficacy and safety testing of pharmaceuticals and cosmetics has been progressing, with particular attention being paid to testing methods using three-dimensional cultured skin. In this case study, a percutaneous absorption test of a cosmetic (lotion) was conducted using three-dimensional cultured human skin, which was measured using AFM (Atomic Force Microscopy). This allows for a visual evaluation of the microstructure of the skin surface, and it is also possible to quantitatively assess the roughness of any specific area. By measuring under atmospheric conditions, it is possible to observe the samples while minimizing alterations that would occur under vacuum conditions.

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[Analysis Case] Observation of Shape Changes of Polymers on a Substrate Using Liquid AFM Measurements

Visualization of structural changes in samples in the atmosphere and in aqueous solutions.

Polymers are known to exhibit diverse functions by altering their composition and structure, and they are utilized in various products. In the evaluation of polymers, assessment in real environments is crucial. This time, we will introduce a case where the shape of polymers on a substrate was visualized in the atmosphere and in aqueous solution using an environmental control atomic force microscope (AFM). Additionally, by combining data analysis, we quantified the dispersion of polymer particles.

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[Analysis Case] AFM Analysis of Smartphone Protective Films

Quantitative evaluation of the quality of sensory products is possible.

The penetration rate of smartphones is increasing year by year, and along with that, the protective films applied to their surfaces are diversifying in functionality. In this instance, we will introduce a case where two types of films (A and B) with fingerprint prevention and anti-reflection features were quantitatively evaluated in terms of roughness, simulating the sensation of touch through AFM analysis.

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[Analysis Case] Comparison of Secondary Electron Images of Cu Surface Using SEM and SIM

It is effective to differentiate between the two methods depending on the surface structure of interest.

Scanning Electron Microscopy (SEM) and Scanning Ion Microscopy (SIM) are both techniques used to evaluate the structure near the surface of a sample by obtaining secondary electron images. Differences in the primary probes lead to variations in contrast and spatial resolution, making it effective to choose between the two methods depending on the surface structure of interest. This document summarizes the comparison of the two methods and presents an example of measurements observing a Cu surface.

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"Basics of TEM" "Applications and Case Studies of TEM" *A gift for all interested participants.

Basic knowledge and analysis examples of TEM (Transmission Electron Microscopy) used in a wide range of research and development fields such as polymers and semiconductors.

TEM (Transmission Electron Microscopy) is a method that involves irradiating a thin sample with electrons, imaging the electrons that have passed through or scattered from the sample, and observing it at high magnification. At MST, we are offering "Basics of TEM," which includes fundamental knowledge such as the characteristics of TEM and sample preparation methods, and "Applications and Examples of TEM," which features representative analysis cases and examples of combined analysis with other methods! This material is presented in an easy-to-understand manner using photographs and diagrams. [Contents (partial)] <Basics of TEM> 　■What can be understood with TEM and STEM ■Characteristics of TEM and STEM 　■Sample preparation methods ■Factors affecting contrast 　■Differentiation between TEM and STEM ■Ultra-high resolution HAADF observation <Applications and Examples of TEM> 　■Analysis examples 　　・TEM analysis under controlled atmosphere and cooling 　　・Evaluation of contact electrodes in SiC power MOSFETs 　　・Structural evaluation of fine transistors *If you would like a booklet, please check the box for "Request for catalog" in the "Contact Us" section to apply. (The downloadable PDF material consists of the first few pages.)

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[Analysis Case] 3D Observation of Cosmetics Using X-ray CT and Cryo-SEM

It is possible to confirm the shape of emulsified particles and inorganic powders! Visualizing the film of liquid foundation from macro to micro levels.

We would like to introduce a case study of 3D observation of cosmetics using X-ray CT and cryo-SEM, analyzed by the foundation. Liquid foundation applied to a plastic substrate was observed using X-ray CT and cryo-SEM, visualizing the dispersion state within the sample. X-ray CT allows for the confirmation of macroscopic morphology in a non-destructive and non-contact manner, while cryo-SEM enables the observation of even more microscopic structures. 【Features】 ■ The internal structure of the liquid foundation film can be evaluated through macroscopic morphological observation. ■ Detailed structural observation using an electron microscope allows for the confirmation of the shapes of emulsified particles and inorganic powders. *For more details, please refer to the PDF document or feel free to contact us.

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[Analysis Case] Structural Evaluation of Positive Electrode Active Material in Secondary Batteries

Evaluation of particle size and crystal orientation of living materials, atomic-level observation is possible.

Lithium-ion secondary batteries undergo changes in the composition and crystal structure of the electrode active materials due to ion extraction and insertion during charging and discharging. As a structural evaluation of the positive electrode active material Li(NiCoMn)O2 (NCM), we assessed the particle size and orientation of primary particles using EBSD. Furthermore, we conducted high-resolution STEM observations on the primary particles whose orientations were confirmed, showcasing the atomic positions of light elements (Li, O) in ABF-STEM images and the atomic positions of transition metals (Ni, Co, Mn) in HAADF-STEM images. Measurement methods: SEM, EBSD, TEM Product field: Secondary batteries Analysis purpose: Shape evaluation, structural evaluation, product investigation For more details, please download the materials or contact us.

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[Analysis Case] AFM Video Observation of Temporal Changes During Heating and Cooling Processes

Evaluate the shape change of the sample surface in situ.

Polymers can change shape depending on environmental factors such as temperature, humidity, and solvents, and by varying the environmental conditions during evaluation, we can deepen our understanding of their physical properties. In this study, we conducted heating and cooling experiments using polycaprolactone (PCL), which is known for its biodegradability. PCL has a melting point of approximately 60°C, and we continuously observed through video how it changes from a crystalline state to an amorphous state upon heating, and how it recrystallizes upon cooling. Measurement method: AFM Product fields: Biotechnology, Pharmaceuticals, Daily Goods, Food Analysis purpose: Shape evaluation For more details, please download the materials or contact us.

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[Analysis Case] Observation of Surface Shape of Non-Woven Fabric Masks Before and After Disinfection

Comparison of the surface shape of the mask before and after alcohol disinfection.

The frequency of mask usage has increased to prevent infections caused by viruses. However, there is a lack of structural data that serves as a basis for their usage methods and resistance. This document presents the results of observing the fibers on the surface of masks before and after alcohol disinfection using SEM. After alcohol disinfection, it was found that the shape of the fibers changed, and the characteristic convex shapes observed before disinfection decreased. Measurement method: SEM Product field: Daily necessities, virus prevention-related products Analysis purpose: Shape evaluation, structural evaluation, degradation investigation, reliability assessment, product investigation For more details, please download the document or contact us.

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[Analysis Case] Heating SSRM Evaluation of Multilayer Ceramic Capacitors (MLCC)

Visualization of conduction paths (insulation degradation areas) within the dielectric.

Multilayer Ceramic Capacitors (MLCC) are capacitors that have a laminated structure consisting of internal electrodes (metal) / dielectric layers (insulator) / internal electrodes (metal). One of the issues with MLCCs is the insulation degradation (lower resistance) of the dielectric layer under high electric fields and high temperatures, which can lead to short circuits between the electrodes. Visualizing the low-resistance conductive paths formed within the dielectric layer is an important clue to understanding the insulation degradation phenomenon. This document presents a case where the insulation degradation of dielectric materials due to temperature changes was visualized by combining SSRM measurement (high electric field) and heating mechanisms (high temperature). Measurement method: SSRM (Scanning Spreading Resistance Microscopy) Product fields: Dielectric materials, capacitors, MLCC Analysis objectives: Resistance value distribution, current distribution, insulation degradation evaluation For more details, please download the document or contact us.

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[Analysis Case] Trench-type Si-MOSFET IDSS Leakage Location Analysis

One-stop service from identifying device defects to analyzing causes.

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.

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[Analysis Case] Evaluation of Ion Implantation Damage Layer in Gallium Oxide Ga2O3

Confirming the differences due to variations in annealing conditions after ion implantation.

Gallium oxide (Ga2O3) has a wider bandgap than SiC and GaN, and possesses excellent physical properties, making it a focus of attention as a material for power devices that can be expected to be high-efficiency and low-cost. Controlling impurity concentration and crystallinity, which influence the characteristics of the devices, is crucial for their development. This document presents the results of observations of the damage layer and changes in surface roughness caused by disturbances in the crystal structure due to ion implantation, under various annealing conditions. Measurement methods: TEM, AFM Product fields: Oxide semiconductors, power devices Analysis objectives: Shape evaluation, structural evaluation For more details, please download the document or contact us.

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[PFM] Piezoelectric Response Microscope

By using a probe coated with a conductive film and applying an alternating voltage to the sample surface, the sample surface is vibrated to obtain electromechanical information.

- Visualization of attraction and repulsion due to the electric dipole effect of piezoelectric samples is possible. - Quantitative evaluation of the sample's expansion and contraction due to piezoelectric response is a reference value. - AFM images can also be obtained simultaneously.

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[Analysis Case] STEM, EBSD Image Simulation for Polycrystalline Structure Analysis

Evaluation of crystal forms using simulations.

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.

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[Analysis Case] TEM Analysis under Atmosphere Control and Cooling (B0156)

Observation with a high-resolution SEM equipped with FIB without atmospheric exposure (controlled atmosphere)!

Our organization has established a system that suppresses atmospheric exposure through atmosphere control, and further cools the samples for processing, observation, and analysis. We can produce TEM thin samples while maintaining the original structure of the specimen, allowing for observation and analysis. Even with unstable materials, we can perform thinning processing while cooling, and by maintaining a vacuum during the transfer between processing and observation devices, we enable cross-sectional TEM/SEM observation that minimizes atmospheric exposure and thermal alteration. 【Measurement and Processing Methods】 ■ [(S)TEM] Scanning Transmission Electron Microscopy ■ Processing under atmosphere control ■ Cryo-processing *For more details, please download the PDF or feel free to contact us.

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[Analysis Case] Dynamic Viscoelastic Evaluation of PDMS using AFM

Introduction to the evaluation of in-plane distribution of viscoelasticity and frequency dependence!

Our organization offers dynamic viscoelastic evaluation of PDMS using AFM. Dynamic Mechanical Analysis (DMA) is an effective method for investigating viscoelastic behavior, which is an important factor in the research and development of polymer materials. Additionally, by combining it with the AFM mechanism, it becomes possible to measure in-plane distribution and evaluate localized areas. This document presents a case study using AFM-DMA to map the viscoelastic modulus of PDMS (polydimethylsiloxane) and conduct frequency-dependent spectroscopy evaluation. [Measurement Method / Processing Method] ■ [AFM] Atomic Force Microscopy *For more details, please download the PDF or feel free to contact us.

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[Analysis Case] (S)TEM Observation by Negative Staining

Examples of morphological observation of liposomes, CNF, microparticles, proteins, etc.!

Our organization offers (S)TEM observation using negative staining. Organic functional materials, such as fine particles and fibrous substances, are primarily composed of light elements like C (carbon), H (hydrogen), O (oxygen), and N (nitrogen), which do not provide sufficient contrast for morphological observation in (S)TEM. Therefore, by applying staining to these materials, we can enhance the contrast and enable observation. In this instance, we will introduce a case where negative staining was performed using phosphotungstic acid (H3[P(W3O10)4]·nH2O, abbreviated as PTA). 【Measurement Method / Processing Method】 ■ [(S)TEM] Scanning Transmission Electron Microscopy ■ Others *For more details, please download the PDF or feel free to contact us.

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OBF STEM method (Optimal Bright Field Scanning Transmission Electron Microscopy)

OBF STEM: Optimum Bright-Field STEM Method

The OBF STEM method is a technique that reconstructs a single STEM image by applying a weighted frequency filter to multiple STEM images obtained from each segment of a segmented STEM detector, appropriately emphasizing different spatial frequency components for each segment. It is characterized by its ability to efficiently utilize the detection signal, allowing for the visualization of structures with low noise and high contrast even under conditions of low electron beam exposure.

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Hamamatsu Photonics PHEMOS-X

Equipped with a multi-wavelength laser, it can handle everything from visible light to near-infrared light with a single device.

PHEMOS-X is a high-resolution emission microscope that captures light emission and heat generation caused by semiconductor device failures to identify the failure location. 1. Capable of mounting up to two ultra-high sensitivity cameras. 2. Can accommodate up to seven light sources for OBIRCH, DALS, EOP, and laser markers. 3. Equipped with an optical stage compatible with various samples.

Company：Toki Commercial Co., Ltd.
Price：More than 100million yen

Optical microscope
microscope

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