At present, there are many materials analysis and testing techniques and instruments, and each has its own advantages. With the wider application range, the existing test characterization methods are increasingly unable to meet the requirements. It is imperative to develop new characterization methods and testing techniques. As far as the current situation is concerned, Xiao Bian summarizes all the equipment used in the material characterization and performance testing process for your reference.
Material characterization
Composition analysis of materials
1. Characterization method: X-ray photoelectron spectrometer
Effect: Obtain the elemental composition and valence or chemical state of the material.
Need to pay attention to the problem: the sample can not be more than 2mm thick, can only test the surface elements, can be tested by sputtering one layer.
2. Characterization method: Pyrolysis chromatograph
Effect: The structure of the polymer material is obtained.
Need to pay attention to the problem: the cracking temperature should be suitable.
3. Characterization method: X-ray diffractometer (XRD)
Effect: The composition of the sample, especially the material of the crystal structure, can be used to measure the lattice constant, composition and quantitative calculation and simulation of the crystal.
Need to pay attention to the problem: the material preparation is simple, but the material size is not too large, it can be in accordance with the sample table standard.
4. Characterization: Nuclear Magnetic Resonance (NMR)
Effect: The structure identification of the organic sample, the commonly used H spectrum, C spectrum, can obtain the type of H in the sample molecule, the type of hybrid, the quantity, the information of the main chain C, and the like.
Need to pay attention to the problem: divided into liquid nuclear magnetic and solid nuclear magnetic.
5. Characterization method: gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS)
Effect: Mass spectrometry is generally more useful in combination with gas phase and liquid phase. It is used to analyze small organic molecules. It has a powerful library for qualitative and quantitative analysis of sample composition.
Problems to be aware of: Requirements for sample polarity, solubility, and gasification temperature.
6. Characterization: Inductively coupled plasma mass spectrometer (ICP-MS), single-channel scanning photoelectric direct reading spectrometer (ICP-AES), inductively coupled plasma optical emission spectrometer (ICP-OES), etc.
Need to pay attention to the problem: the sample needs to be first dissolved in the solution, commonly used nitric acid, hydrochloric acid, aqua regia, and other various organic acids as the dissolved acid, to ensure that the heavy metals in the sample can be dissolved.
7. Characterization method: Scanning electron Microscope spectrometer (EDS)
Effect: The elements in the sample can be qualitatively and quantitatively analyzed. Although organic elements such as C, N, O, etc. can also be analyzed, the analysis of inorganic elements with larger element numbers is more accurate.
Need to pay attention to the problem: EDS is an accessory of SEM or TEM. The sample needs to be prepared according to SEM or TEM sample preparation requirements, so the sample preparation requirements are higher.
8. Characterization: Electronic Energy Loss Spectrometer (EELS)
Effect: It can qualitatively and quantitatively analyze the elements in the sample, the range is larger than EDS, and the resolution is several orders of magnitude higher than EDS. When doing MAPPING analysis, the distribution of elements can be characterized at the nanoscale.
Need to pay attention to the problem: EELS requires higher TEM configuration. Generally, TEM does not contain this accessory, and is not a universal test method.
9. Characterization: Thermogravimetric Analyzer - Thermal Analysis - Fourier Transform Infrared Spectrometer (TGA-DSC-FTIR), or Gas Chromatography-Mass Spectrometry (GC-MS)
Effect: TGA can record the weight of organic and inorganic samples with temperature, characterize the thermal stability of the sample, quantitatively analyze the sample composition, etc., together with DSC, can analyze the thermal enthalpy effect of the sample with temperature, analyze the melting point of the sample, the demarcation point, the heat of chemical reaction. Etc., in combination with infrared or temperament, the composition of the thermal decomposition product can be analyzed.
Need to pay attention to the problem: the amount of TGA sample alone is 5-10mg, but the amount of swelling sample must be reduced, energy storage materials, explosives, etc. can not be used for TGA or can only be tested with a very small amount of sample. In combination with infrared or temperament, the sample dosage should be reduced appropriately. Signal to noise ratio and background interference.
10. Characterization: Atomic Force Microscopy (AFM), Atomic Force Microscopy-Infrared (AFM-IR)
Effect: AFM can perform true 3-dimensional analysis on the surface morphology of the sample. AFM and infrared can simultaneously perform infrared functional group analysis on any area on the AFM image, and do mapping of functional groups, composite materials, multilayer materials, Microscopic phase separation materials are very effective.
Need to pay attention to the problem: the sample requirements must be smooth and smooth, otherwise the probe may be damaged, and the sample should be kept free of water when used in combination with infrared.
11. Characterization method: specific surface area tester (BET)
Effect: Analyze the specific surface area, pore shape, pore size, pore distribution, etc. of porous materials, common instruments in the fields of catalysis, powder preparation and so on.
12. Characterization: Gel Permeation Chromatograph (GPC)
Effect: The polymer material is commonly characterized. Several molecular weights of the polymer can be measured, but different packed columns and solvents should be selected according to the characteristics of the sample.
13. Characterization method: ion chromatograph
Effect: Qualitative and quantitative analysis of common anions such as F-, Cl-, Br-, NO2-, NO3-, SO42-, PO43- and cations such as Li+, Na+, NH4+, K+, Mg2+, Ca2+, etc. The composite application is an analysis tool.
14. Characterization method: laser particle size analyzer
Effect: Analysis of particle size, particle size distribution, etc. of the particle sample.
15. Characterization method: organic element analyzer
Effect: Quantitative analysis of common elements in several organic samples such as C, H, O, N, S, etc. is a common method for analysis.
16. Characterization: Other spectrometers such as infrared, ultraviolet, Raman, and fluorescence are suitable for different types of samples, and can be used for qualitative and quantitative characterization.
17. Other characterization methods: dynamic thermomechanical analysis (DMA), thermomechanical analysis (TMA), comprehensive physical property analysis, contact angle, small-angle scattering, single crystal diffraction, etc. are all useful in some specialized fields.
Qualitative and quantitative analysis of materials (solid liquid powder)
X fluorescence analyzer
The characteristic X-ray energy and wavelength emitted by different elements are different. Therefore, by measuring the energy or wavelength of the X-ray, it is known which element it emits, and the qualitative analysis of the element is performed. At the same time, the characteristic X-ray intensity of an element emitted by the sample after excitation is related to the content of the element in the sample, so the strength of the element can be measured for quantitative analysis of the element.
Microscopic atomic arrangement
Instrument: 3ADP/APT (three-dimensional atom probe)
Effect: Analysis of different atomic arrangements in a few hundred nanometers
Characterizing the pore size distribution of macroporous materials
Instrument mercury intrusion test
The effect of the nitrogen adsorption test can only be limited to the distribution of micropores in the measurement, and the macroporous materials are generally measured by the mercury intrusion test.
Performance characterization
Corrosion resistance of materials
1. Characterization: Electrochemical impedance spectroscopy
Effect: Obtain the information of the capacitance, resistance, inductance and other materials of the material to obtain the anti-corrosion mechanism of the material.
Need to pay attention to the problem: to ensure that the area of ​​the substrate is fixed
2. Characterization: polarization curve
Effect: Corrosion current density, polarization resistance, corrosion potential, corrosion rate, etc. when the material is corroded
Need to pay attention to the problem: to ensure that the area of ​​the substrate is fixed
3. Characterization method: salt spray test
Effect: Accelerated test to obtain corrosion resistance of materials
Need to pay attention to the problem: pay attention to changes in brine concentration
Characterizing material conductivity
Instrument four probe
Effect: Test the conductivity of the film or block
Characterizing the material's hydrophilic (other solvent) properties
Instrument contact angle measuring instrument
Effect test material surface tension, contact angle, etc.
Characterizing the stability of colloidal systems
Instrument zeta potentiometer
Material characterization: coating (film) wear resistance
Characterization method: pin disc friction and wear meter
Effect: The friction coefficient was tested under a certain load and time and the wear mechanism was analyzed in combination with the surface morphology.
Material characterization: coating (film) bonding force
Characterization: Scratch
Effect: The bonding strength between the test film and the substrate needs to be comprehensively evaluated in combination with the scratch morphology, acoustic emission spectrum and friction coefficient change.
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