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Method for measuring particle size of primary particles of positive electrode material

A cathode material, particle size technology, applied in the analysis of materials, particle and sedimentation analysis, material analysis using wave/particle radiation, etc., can solve the problem that the primary particle size is not representative, the test efficiency is low, and the test process is complicated and other problems to achieve the effect of efficient and fast testing

Pending Publication Date: 2022-04-22
HUBEI JINQUAN NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 2. Although the primary particles of the material can be observed and the single particle size can be measured by SEM, since SEM can only observe the sample part within the field of view, the observed primary particle size is not representative
In particular, for secondary sphere type cathode materials (such as polycrystalline NCM / NCA ternary cathode), since the primary particles inside the secondary sphere cannot be observed by SEM, the internal primary particles can only be estimated from the primary particles on the surface. At the same time, the primary particles in the outer layer of the secondary ball are densely arranged, and the particles cover each other. The whole picture of the primary particles cannot be truly observed through SEM, so the observation error of the primary particle size is relatively large
[0007] 3. A more feasible solution is to conduct SEM observations in multiple fields of view, and then take the average of several obtained primary particle sizes, but this solution will cause complex testing procedures, low testing efficiency, and high testing costs The problem

Method used

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  • Method for measuring particle size of primary particles of positive electrode material
  • Method for measuring particle size of primary particles of positive electrode material
  • Method for measuring particle size of primary particles of positive electrode material

Examples

Experimental program
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preparation example Construction

[0034] Preparation of positive electrode material samples before SEM test: stick a double-sided conductive tape on the loading tray, take a small amount of positive electrode material samples on the tape near the center of the loading tray, and use the ear cleaning ball to radially outward toward the loading tray Blow lightly in the direction so that the sample powder can be evenly distributed on the tape, and at the same time blow off the powder that is not firmly bonded. Apply conductive silver paste to the edge of the tape to connect the sample to the loading plate. After the silver paste dries, steam gold deal with.

[0035] S102: Carry out XRD test to anode material, obtain subgrain size l;

[0036] Carry out XRD test and analysis on the selected cathode material samples. The XRD scanning range 2θ is 10-80°, the scanning speed is ≤2° / min, and the step size is 0.01-0.02°. The obtained XRD pattern is refined on the JADE software, and passed The XRD spectrum after refinemen...

Embodiment 1

[0050] Test the primary particle size of a lithium iron phosphate: Weigh the sample to prepare a sample, and perform an XRD test on a Bruker X-ray diffractometer of the model D2PHASER. The scanning range 2θ is 10-80°, and the scanning speed is 2 ° / min, step length 0.02°, the obtained XRD spectrum was processed on the JADE software to obtain a refined XRD spectrum, using the half maximum width β of the strongest diffraction peak (2θ between 30°-40°), the data Read out by the equipment software, β=0.00953, θ=17.875°, and substitute it into the Scherrer formula l=Kλ / (βcosθ), K is the shape factor, take K=1, λ is the incident wavelength of X-rays, and use the Cu target Kα line, λ=0.15418nm, obtain the corresponding sub-grain size l, l=17.4nm, step S103 obtains the relational formula of lithium iron phosphate as L=5.75l, and substitute it to obtain the L=100nm of the test sample.

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Abstract

The invention relates to a method for measuring the primary particle size of a positive electrode material, which comprises the following steps of: performing SEM (scanning electron microscope) test on a calibrated positive electrode material to obtain an average primary particle size L; performing XRD (X-Ray Diffraction) test on the calibrated positive electrode material to obtain a sub-grain size l; establishing a relational expression L = a * l between the average primary particle size L and the subgrain size l for calibrating the positive electrode material to obtain a value of a coefficient a; the to-be-tested positive electrode material is subjected to XRD testing to obtain the corresponding sub-grain size l, the sub-grain size l is substituted into the relational expression corresponding to the same type of positive electrode material to obtain the primary particle size of the to-be-tested positive electrode material, and the calibration positive electrode material and the to-be-tested positive electrode material are the same in type. The test method provided by the invention overcomes the problems that a laser particle analyzer cannot reflect the primary particle size of the material and the error of the primary particle size of the SEM test material is large, and can efficiently and quickly test the primary particle size of the positive electrode material.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for measuring the primary particle size of positive electrode materials. Background technique [0002] The positive electrode material is one of the key materials that determine the electrical performance of lithium-ion batteries, and has a greater impact on lithium-ion batteries. The mainstream cathode materials currently used in lithium-ion batteries include lithium cobalt oxide (LCO), lithium iron phosphate (LFP), lithium manganese oxide (LMO), ternary materials nickel cobalt lithium manganate (NCM) and nickel cobalt lithium aluminate ( NCA) etc. [0003] Lithium iron phosphate (LFP) material is orthorhombic olivine structure, 1 PO 4 tetrahedron with 1 FeO 6 Octahedral, 2 LiO 6 Octahedrons share edges, thus forming a three-dimensional space network structure. Among them, the conductive unit FeO 6 Due to the arrangement of common vertices of octahedrons, elec...

Claims

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Application Information

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IPC IPC(8): G01N15/02G01N23/2251G01N23/2055
CPCG01N15/02G01N23/2251G01N23/2055
Inventor 石忠洋刘范芬赵平李咏军温圣耀
Owner HUBEI JINQUAN NEW MATERIALS CO LTD
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