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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  • Claims
  • Application Information

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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

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

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Example Embodiment

[0034] Preparation of cathode material samples before SEM testing: double-sided conductive tape is glued to the load plate, a small amount of positive material samples are placed on the tape near the center of the carrier disk, and the ear wash bulb is gently blown in the outward direction of the carrier disc radially, so that the sample powder can be evenly distributed on the tape, and the loosely bonded powder is blown away, and the conductive silver paste is coated on the edge of the tape to connect the sample and the carrier tray, and the silver paste is dried after the gold processing is carried out.

[0035] S102: XRD testing of the cathode material yields subgrain size l;

[0036] XRD test analysis of the selected cathode material sample, XRD scanning range 2θ is 10-80 °, scanning speed ≤2 ° / min, step length 0.01-0.02 °, the obtained XRD map is refined on the JADE software, and the half-height wide FWHM of the strongest diffraction peak is calculated by the refined XRD map ...

Example Embodiment

[0049] Example 1

[0050] Testing the primary particle size of a lithium iron phosphate: Weighing the sample, XRD testing on the Bruker X-ray diffractometer of model D2PHASER, scanning range 2θ is 10-80°, scanning speed is 2° / min, step length is 0.02°, the resulting XRD spectra is processed on JADE software to obtain a refined XRD profile, using the highest peak of diffraction (2θ between 30 °-40°) of the half-height wide β, the data is read out by the device software, β = 0.00953, θ = 17.875 °, substituted into the Xie Le formula l = Kλ / (βcosθ), K is the shape factor, take K = 1, λ is the X-ray incident wavelength, using the Cu target Kα line, λ = 0.15418 nm, to obtain the corresponding grain size l, l = 17.4 nm, step S103 to obtain the relationship formula of lithium iron phosphate is L = 5.75l, and the L = 100 nm of the sample sample can be obtained by substitution.

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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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