Preparation method of thin-film material section scanning electron microscope sample

A thin film material, scanning electron microscope technology, applied in the direction of analyzing materials, material analysis using wave/particle radiation, measuring devices, etc., can solve the problems of high difficulty, high process cost, error, etc., to reduce mechanical deformation, cross-section flatness High, guaranteed accuracy

Active Publication Date: 2020-09-29
CHINA AUTOMOTIVE BATTERY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, when conducting SEM observation on the cross-section of the thin film material, due to the thinner and softer material of the diaphragm, it is extremely easy to bend, and the microporous structure is also easily deformed. The difficulty of sample preparation is relatively high, and there is no particularly representative sample. preparation method; moreover, in the actual testing process of polymer microporous membranes, there is no uniform preparation method for SEM samples, and the previous methods are also difficult to prepare samples with high reproducibility and complete pore shape, which also limits the research on Observation and Analysis of Internal Microstructure of Microporous Thin Film Material
[0005] Chinese patent CN111122629A discloses a method for making a cross-sectional SEM sample of a thin film material, using liquid pouring to fix the microporous structure of the film material, but when using resin for normal temperature or heating pouring, the influence of the liquid on the surface of the material during the pouring and curing process cannot be ruled out Factor; Another example is the method for preparing the cross-sectional scanning electron microscope sample of the microporous film material disclosed by Chinese patent CN103512785A, which is also to use the volatile liquid to pour the microporous structure of the film material at low temperature, although it can reduce the impact of liquid on the film to a certain extent. The effect of the surface of the material, but the process cost is very high, and when the machine breaks, there is still a certain error caused by stretching

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  • Preparation method of thin-film material section scanning electron microscope sample

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Embodiment 1

[0026] The preparation method of the thin film material section scanning electron microscope sample described in this embodiment comprises the following steps:

[0027] (1) Cut the composite coated diaphragm material for lithium-ion batteries to be tested into a square sample with a thickness of 10 μm and a sampling size of 20×30 mm, with a size of 8×10 mm, and place the sample on the original film Necessary records of the location, orientation, etc.;

[0028] The film sample is stacked with the flat sheet-shaped first clamping body and the second clamping body, the diaphragm sample is located between the clamping bodies, and one side edge is aligned, and the diaphragm sample and the second clamping body are aligned. A clamping body is fixed together to obtain the desired thin film sample assembly;

[0029] In this embodiment, the first clamping body used is an aluminum sheet with a thickness of 15 μm, and the second clamping body is a silicon wafer with a thickness of 50 μm;...

Embodiment 2

[0034] The preparation method of the thin film material section scanning electron microscope sample described in this embodiment comprises the following steps:

[0035] (1) Cut the composite coated diaphragm material for lithium-ion batteries to be tested into a square sample with a thickness of 20 μm and a sampling size of 20×30 mm, with a size of 8×10 mm, and place the sample on the original film Necessary records of the location, orientation, etc.;

[0036] The film sample is stacked with the flat sheet-shaped first clamping body and the second clamping body, the diaphragm sample is located between the clamping bodies, and one side edge is aligned, and the diaphragm sample and the second clamping body are aligned. A clamping body is fixed together to obtain the desired thin film sample assembly;

[0037] In this embodiment, the first clamping body used is a nickel sheet with a thickness of 20 μm, and the second clamping body is a silicon chip with a thickness of 100 μm; an...

Embodiment 3

[0042] The preparation method of the thin film material section scanning electron microscope sample described in this embodiment comprises the following steps:

[0043] (1) Cut the composite coated separator material for lithium-ion batteries to be tested with a thickness of 30 μm and a sampling size of 20×30mm, cut it into a square sample with a size of 8×10mm, and place the sample on the original film Necessary records of the location, orientation, etc.;

[0044] The film sample is stacked with the flat sheet-shaped first clamping body and the second clamping body, the diaphragm sample is located between the clamping bodies, and one side edge is aligned, and the diaphragm sample and the second clamping body are aligned. A clamping body is fixed together to obtain the desired thin film sample assembly;

[0045] In this embodiment, the first clamping body used is an aluminum sheet with a thickness of 50 μm, and the second clamping body is a silicon wafer with a thickness of 1...

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Abstract

The invention belongs to the technical field of material testing, particularly relates to the field of testing of polymer microporous thin film materials, and particularly to a preparation method of athin-film material section scanning electron microscope sample. According to the preparation method of the thin-film material section scanning electron microscope sample, a film material cross section sample is prepared in an argon ion polishing mode, so that mechanical deformation is reduced to the greatest extent, the cross section flatness is high, and the original form of a micropore structure can be kept as much as possible; a conductive first clamping body and a conductive second clamping body are used for fixing the film sample in the argon ion polishing process, so that factors such as curling and burrs influencing the polishing quality are avoided; liquid medicine is not used, contamination to the surface of a thin film sample is little, potential influences of the liquid medicine on the surface of a film material are avoided, and the accuracy of sample detection is guaranteed to the greatest extent.

Description

technical field [0001] The invention belongs to the technical field of material testing, in particular to the testing field of macromolecule microporous film materials, and in particular relates to a method for preparing a cross-sectional scanning electron microscope sample of a film material. Background technique [0002] With the vigorous development of new energy technologies, lithium-ion battery technology has received extensive attention and development. Diaphragm is a key material in the manufacturing process of lithium-ion batteries. The diaphragm material needs to insulate the positive and negative electrodes to prevent short circuit, and also requires itself to have a microporous structure to allow lithium ions to pass through. Therefore, the microstructure of the diaphragm directly affects the performance of the diaphragm. Good or bad, which directly affects the cycle performance, service life and application safety of lithium-ion batteries. Therefore, observing t...

Claims

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Application Information

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IPC IPC(8): G01N23/2202
CPCG01N23/2202G01N2223/07G01N2223/61
Inventor王泽方彦彦沈雪玲袁敏娟严细峰李晓兵刘美王晓丹李晓萍王喆唐玲云凤玲崔义张杭闫坤张向军王琳
OwnerCHINA AUTOMOTIVE BATTERY RES INST CO LTD