Physical Analyses by JFE Techno-Research

JFE-TEC's Approach to Physical Analysis

By utilizing physical analysis and nano-material analysis methods, JFE-TEC analyzes the microstructure of objects and substances from a macro to atomic scale on the basis of material, product, and part.

We introduce optimum methods of analysis according to the material and provide optimum analysis techniques.

Devices and methods used for physical analysis are rapidly advancing. We also introduce physical analyses on the basis of the method of analysis.

Physical Analyses based on Material Field

Roles of physical analysis and nano-material analysis

To give direction to research and development, solve malfunctions and failures, and manage processes, it is necessary to consider the conditions of use and examine phenomena after correctly understanding the physical properties of the materials used.

JFE-TEC offers solutions to issues after understanding the physical properties of materials and examining the phenomena.

STEP 1. Understanding of physical properties

Properties determined by chemical analysis and physical property evaluation

  • Strength: structure/orientation
  • Corrosion, catalyst, battery, friction: electrochemical reaction and surface reaction
  • Electronic/electric physical property: electronic state
  • Magnetic property: structure/orientation, magnetic domain

Properties determined by physical analysis

  • Morphological observation: structure (macro to nano level), particle diameter distribution
  • Qualitative/quantitative analysis: average/local composition
  • State analysis: compound species, crystalline phase
  • Mapping/depth direction analysis: composition, chemical state distribution

STEP 2. Examination of phenomenon

We examine phenomena by considering the process, use condition, etc.

  • Corrosion reaction,
  • Joining reaction,
  • Electric characteristics, etc.

STEP 3. Consulting

Based on examination result, we can make following proposals:

  • Setting direction of research and development,
  • Solution of malfunction and failure
  • Process management
Fig.

Material-dependent analysis techniques

The structure to exhibit the necessary physical property differs from material to material. We provide optimum analysis techniques according to the structure.

Thin film, surface treatment

  • Friction, sliding, corrosion resistance, color tone, electronic physical property, magnetic property, optical characteristics, etc.

Inorganic material, ceramics

  • High strength, high corrosion resistance, electric physical property (insulation property, electrical conductivity, dielectric property), optical characteristics

Magnetic material

  • Magnetic characteristics of hard magnetic material/soft magnetic material (B-H characteristic, hysteresis), and others

Catalyst, ultrafine particle, nano material

  • Catalyst, ultrafine particle, nano material

Battery material

  • Material for lithium-ion secondary battery (material for positive electrode, material for negative electrode, etc.):
    Charging/discharging characteristics, electromotive force, durability
  • Capacitor, fuel cell, solar cell: Electromotive force, catalytic activity, oxidation reduction, hydrogen permeability, durability, corrosion resistance, etc.

Organic/high polymer material

  • Strength, high corrosion resistance, electric physical property (insulation property), optical characteristics

Health care, biotechnology

  • Strength, corrosion resistance, biocompatibility, mixing-in and generation of foreign substance, etc.

Environment and safety

  • Safety of fine particles (asbestos, nano particles)

Physical Analyses based on Analysis Method

JFE-TEC observes and analyzes the sections, interface structures, and morphologies of products and composite materials that employ thin films and fine particles of metal, ceramics, and high polymers at nano-scale resolutions. We will also undertake precise sample preparation for observation of section/interface structure and morphology.

The size of controlled structure and analysis method vary from material to material.

We offer optimum analysis techniques for optimum morphological observation, element analysis, surface chemical state analysis, and crystalline structure analysis.

Practical sample thickness and detectable concentration range in nano material analysis

The practical sample thickness and detectable concentration range in various analysis methods are restricted. The table below shows some examples.

Practical sample thickness and detectable concentration range in nano material analysis

Selection of microscope for material

As the structure to analyze differs from subject to subject, the analysis method differs as well.

Selection of microscope for material

Morphological observation

Various bulk materials, thin film/surface treatment, and fine particle morphology (shape, size/thickness, particle size distribution, aggregability) are observed.

  • Surface morphology/structure observation
  • Section/fine structure observation

Elementary analysis

Elements composing various bulk materials, thin film/surface treatment, fine particles are analyzed (qualitative/quantitative analysis, in-plane distribution/depth direction distribution/ three-dimensional distribution, chemical bonding state).

  • Analysis of element of minute part
  • Surface chemical state analysis
  • Bulk chemical state analysis

Crystalline structure analysis

Various bulk materials, thin film/surface treatment, and the crystalline structure of fine particle (substance identification, determination of crystalline structure, crystalline orientation/aggregate structure, and residual stress) are observed, and then evaluated and analyzed.

  • Average information
  • Local analysis

Sample preparation

Samples suitable for analyses in atomic scale to macro scale such as section polishing, FIB processing, argon ion beam processing, and microtoming of various materials (steel/non-ferrous metal, ceramics, semiconductor, polymer, thin film/surface treatment, etc.) are prepared.

In the case with cryo microtome/FIB suitable for polymer materials susceptible to damage, material for lithium-ion secondary battery and neodymium magnet, we also undertake preparation in environment unexposed to atmosphere, which is a prerequisite.

Main Evaluation Items and Analysis Methods of Physical Analysis (Our Proprietary Techniques)

Morphological observation

Contents of evaluation: shape, size/thickness, particle size distribution, aggregability
  Abbreviation
Transmission Electron Microscopy with Cs corrector Cs corrector TEM
Transmission Electron Microscopy TEM
Ultra Low Voltage Scanning Electron Microscopy ULV-SEM
Scanning Electron Microscopy SEM
Three Dimensional Scanning Electron Microscopy 3D-SEM
Focused Ion beam - Scanning Electron Microscopy FIB-SEM

Surface chemical state analysis

Contents of evaluation: qualitative analysis, chemical state analysis, compound identification, element analysis (depth direction, in-plan, three-dimensional), quantitative analysis
  Abbreviation
X-ray Photoelectron Spectroscopy XPS
Auger Electron Spectroscopy AES
Secondary Ion Mass Spectrometry SIMS
Time Of Flight-Secondary Ion Mass Spectrometry TOF-SIMS
Electron Probe Micro-Analysis EPMA
Field Emission-Electron Probe Micro-Analysis FE-EPMA
Electron Energy Loss Spectroscopy EELS
Thermal Desorption Spectroscopy TDS
Raman Scattering Spectroscopy RSS
Fourier Transform Infrared Absorption FT-IR
Laser Ablation Inductively Coupled Plasma Mass Spectrometry LA-ICP-MS

Evaluation item: crystalline structure analysis

Contents of evaluation: substance identification, crystalline structure, crystalline orientation
  Abbreviation
X-ray Diffraction (capable of Rietveld analysis) XRD
Electron Diffraction ED
Electron Backscatter Diffraction
Electron Backscatting Pattern
EBSD/EBSP

Evaluation item: composition analysis

Contents of evaluation: Composition quantitative analysis (chemical analysis/analysis by device)
  Abbreviation
Inductively Coupled Plasma Atomic Emission Spectrometry ICP-AES
Inductively Coupled Plasma Mass Spectrometry ICP-MS
UV-VIS (Ultraviolet Visible Absorption Spectroscopy) - Spectrophotometer in near-infrared to near-ultraviolet region UV-VIS
Atomic Absorption Spectrometry AAS
Gas Chromatograph Mass Spectrometry GC-MS
Liquid Chromatograph Mass Spectrometry LC-MS

Evaluation item: physical property evaluation

Contents of evaluation: particle size distribution, thermos-physical property, specific surface area/pore size distribution, density oxidation/reduction solubility/ dispersibility
  Abbreviation
Laser diffraction particle size distribution measurement  
Thermal Analysis TA
Thermogravimetric Analysis TG
Differential Thermal Analysis DTA
Differential Scanning Calorimetry DSC
Specific surface area measurement, pore size distribution (BET method)  

Evaluation item: working environment analysis/investigation

Contents of evaluation:
  Abbreviation
Nano particle concentration measurement by TEM  

Example of Papers and Presentations at Symposium by JFE-TEC

Paper/ symposium Place of publication Year of publication Title
Paper Journal of the Surface Finishing Society of Japan 2013 The Effect of Steel Sheet Pretreatment on Alloying Behavior of Galvanized Steel Sheet
Paper Bulletin of Gunma Industrial Technology Center 2013 Forefront of Material Nano Structure Observation Using Electron Microscopy
International symposium 6th International Symposium
on Practical Surface Analysis
2013 "Damage of ZrO2 by Argon Ion Bombardment"
Domestic symposium Polymer Material Meeting of The Japan Society for Analytical Chemistry 2008 New Analysis Method of Material Electrode Surface by Ultra Low Voltage SEM
Domestic symposium 29th meeting held by Surface Analysis Society of Japan in 2009 2009 Ultra Low Voltage SEM as New Form of Surface Observation
Domestic symposium 1st Forum of Society for Study of Foreign Substances in 2009 2009 Physical Analysis Technique for Foreign Substance Analysis and Malfunction Investigation
Domestic symposium Meeting of the Surface Science Society of Japan in 2009 2009 Progress of Material Observation by Ultra Low Acceleration Voltage SEM
Domestic symposium Meeting held by Nanotech Department of The Surface Finishing Society of Japan 2010 Analysis Techniques in Nano Material Development
Domestic symposium Meeting of the Surface Science Society of Japan in 2011 2011 Roles of Surface Analysis in Progress of Steel Material
Domestic symposium Meeting of the Japan Society for Heat Treatment in 2011 2011 Forefront of Analysis of Metallic Material Microstructure by ULV-SEM
Domestic symposium Meeting of the Japan Society for Applied Physics in 2012 2012 Damage of Zr Oxide by Ar Ion Irradiation
Domestic symposium Meeting of the Surface Science Society of Japan in 2012
32nd Surface Science Academic Meeting
2012 Damage of ZrO2 by Ar Ion Irradiation
Domestic symposium Corporate exhibitions in 20th meeting held by Advanced Power Semiconductors Workshop, The Japan Society for Applied Physics 2012 Electron Microscopy Technologies Used According to Structure Size from Atomic Scale to Macro Scale
Domestic symposium 37th conference of the Gunma Industrial Technology Center 2013 Forefront of Material Nano Structure Observation Using Electron Microscopy
Domestic symposium Meeting of the Japanese Society of Microscopy in 2013 2013 Examples of Utilization of Ultra Low-voltage Scanning Electron Microscopy for Surface/Interface Analysis
Domestic symposium 22nd meeting of the Advanced Power Semiconductors Workshop, The Japan Society for Applied Physics 2013 Analysis of C State in Gate Oxide/SiC Interface Using Cs Corrector STEM
Domestic symposium 22nd meeting of the Advanced Power Semiconductors Workshop, The Japan Society for Applied Physics 2013 Electron Microscopy Technologies Used According to Structure Size from Atomic Scale to Macro Scale
Domestic symposium 30th panel discussion on rare earth by the Rare Earth Society of Japan 2013 Analysis Technique of Atomic Scale Structure of Intercrystalline Phase in Meodymium Magnet Using Cs Corrector STEM
Domestic symposium 2nd meeting held by Advanced Power Semiconductors Division, the Japan Society for Applied Physics 2014 Techniques of Interface Observation Using Electron Microscopy According to Structure Size from Atomic Scale to Macro Scale

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