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Preparation method of sample for characterizing element distribution uniformity

A technology for element distribution and sample preparation, applied in electrical components, analytical materials, material analysis using wave/particle radiation, etc., which can solve the problem of low resolution, insufficient characterization of bulk element uniformity, and inability to accurately judge element distribution uniformity. To solve problems such as properties, to achieve the effect of simple and convenient preparation method, improve preparation efficiency and section quality

Inactive Publication Date: 2021-05-14
TIANJIN GUOAN MGL NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the uniformity of element doping is generally characterized by testing the energy spectrum of the element, but this method is only limited to the surface layer of the particle, and the resolution is low. For some elements with similar energy, the distribution uniformity of an element cannot be accurately judged.
In addition, photoelectron energy spectroscopy and electron energy loss spectroscopy are useful for the identification of element types and distribution uniformity of hundreds of nanometers on the surface, but they are slightly insufficient in the characterization of bulk element uniformity

Method used

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  • Preparation method of sample for characterizing element distribution uniformity

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preparation example Construction

[0026] According to the present invention, a sample preparation method for characterizing the distribution uniformity of positive electrode material elements is provided, the method comprising:

[0027] Step 1, preparing the positive electrode material and preparing the positive electrode sheet.

[0028] In the present invention, in the field of lithium-ion batteries, the cathode material plays a key role in the electrochemical performance of the lithium-ion battery. Usually, the cathode material is obtained by dry mixing for element doping or coating, and the doping or coating of elements The distribution uniformity in the cathode material has an important influence on the electrochemical performance of the cathode material.

[0029] In the present invention, the distribution uniformity of the bulk phase elements in the positive electrode material can be obtained by making the positive electrode material into a pole piece, and cutting the pole piece, and obtaining the element...

Embodiment 1

[0066] Weigh 6.25g of binder PVDF and disperse it into 2.4g of N-methylpyrrolidone, then weigh 9.5g of nickel-cobalt-manganese cathode material and add it to the above solution, and stir evenly to obtain a slurry;

[0067] Apply the slurry to the aluminum foil by an electric coater, and place it in a 60°C oven to dry to obtain the positive electrode sheet, which is set aside;

[0068] Cut the positive pole piece into a square pole piece of 8*8cm;

[0069] Fix the square pole piece on the sample table fixture, and use liquid nitrogen to control the temperature of the sample table to 25°C to balance the sudden rise in the cavity temperature during cutting;

[0070] Three argon ion beams are used to cut the positive pole piece, the middle ion beam is perpendicular to the positive pole piece, and the other two beams are located on both sides of the middle ion beam, forming an angle of 60° with the middle ion beam, and adjusting the appropriate Ar gas flow ( 0-1), first set the vo...

Embodiment 2

[0074] Weigh 1.5g of binder and disperse it into 2.9g of N-methylpyrrolidone, then add 9.88g of lithium cobaltate positive electrode material into the above solution, and stir to obtain a slurry;

[0075] The slurry is evenly coated on the aluminum foil by an electric coater, and then dried in an oven at 60°C to obtain the positive electrode sheet, which is set aside;

[0076] Cut the positive pole piece into a disc with a diameter of 15mm, and set aside;

[0077] Fix the wafer on the sample stage fixture, and control the temperature of the sample stage at 25°C to balance the sudden increase in the chamber temperature during cutting.

[0078] Three argon ion beams are used to cut the positive pole piece, the middle ion beam is perpendicular to the positive pole piece, and the other two beams are located on both sides of the middle ion beam, forming an angle of 60° with the middle ion beam, and adjusting the appropriate Ar gas flow ( 0-1), first set the voltage 4kV, grinding t...

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Abstract

The invention discloses a preparation method of a sample for characterizing element uniformity of a positive electrode material, which comprises the following steps of: step 1, preparing the positive electrode material, and preparing a positive electrode plate; step 2, cutting the positive pole piece to form a cutting section; and step 3, testing the cutting section. The positive pole piece is prepared and cut by an argon ion beam, and the formed section of the positive pole piece is used for electron microscope test analysis. Three argon ion beams are adopted to cut the positive pole piece in different directions to obtain the section of the positive pole piece, and the section sample is subjected to energy spectrum scanning, so that the uniformity degree of material surface and bulk phase element distribution can be effectively observed, and a reliable basis is provided for evaluating the performance of the positive pole material. The method provided by the invention is simple and quick, and the element distribution condition can be intuitively obtained.

Description

technical field [0001] The invention belongs to the technical field of material characterization, and in particular relates to a sample preparation method for characterizing element distribution uniformity. Background technique [0002] As one of the main power sources of 3C consumer electronics products and electric vehicles, lithium-ion batteries have the advantages of high energy density, high safety performance and low self-discharge. As an important part of the battery, the cathode material of the lithium-ion battery plays a key role in improving the energy density of the battery. [0003] Currently used positive electrode materials, such as lithium cobaltate, ternary materials, etc., will use element doping and coating to achieve the purpose of performance improvement. In the field of preparation of cathode materials for lithium-ion batteries, dry mixing is generally used to achieve element doping and coating, but it is not known whether the effect of doping and coati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202G01N23/2251H01M4/13H01M4/139
CPCG01N23/2202G01N23/2251H01M4/13H01M4/139G01N2223/07G01N2223/102Y02E60/10
Inventor 沈恋卢兴华白珍辉魏卫凌仕刚苏迎春朱卫泉
Owner TIANJIN GUOAN MGL NEW MATERIALS TECH CO LTD
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