Preparation method of large-particle powder transmission electron microscope sample

A technique for TEM samples and large particles, which is used in material analysis, measurement devices, and instruments using wave/particle radiation. The effect of unclear problems, strong practicability and short sample preparation cycle

Active Publication Date: 2017-05-10
GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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Problems solved by technology

At present, for large-particle powder samples, in order to meet the requirements of transmission electron microscope observation, there are three main sample preparation methods: the first one is directly dispersed on the carbon support film or micro-grid, for micron-sized particles, even the edge of the sample will be very thick , it is not easy to carry out transmission electron microscope observation, and it is impossible to obtain high-resolution images at the atomic resolution level. In addition, the charge of large particles will cause the sample to be extremely unstable under the actio

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  • Preparation method of large-particle powder transmission electron microscope sample
  • Preparation method of large-particle powder transmission electron microscope sample
  • Preparation method of large-particle powder transmission electron microscope sample

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Embodiment 1

[0020] according to figure 1 According to the preparation process, the MnNiGe alloy brittle particle sample is mixed with carbon-containing conductive powder at a volume ratio of 1:99 to form a mixed powder; the mixed powder is put into a metallographic mounting machine, and the pressure of the mounting machine is controlled to 3MPa. The heating temperature is 180°C, the holding time is 2 minutes, and the cooling time is 3 minutes. Control the amount of mixed powder so that the height of the mounted sample is 0.5 cm and the diameter is 2 cm to make a metallographic sample; Melting will cause the large particle powder to settle to the bottom naturally, so directly grind the bottom of the metallographic sample with 4000 mesh sandpaper until the large particle powder can be seen, and the grinding time is 1min to make the initial grinding sample; The sandpaper of 2000 mesh and 2000 mesh is ground step by step, and the thickness of each sandpaper is about 100 μm, 50 μm and 35 μm re...

Embodiment 2

[0025] according to figure 1 The preparation process of the method is to take a large particle sample of MnCoGe alloy and mix it with carbon-containing conductive powder at a volume ratio of 1:4 to form a mixed powder; put the mixed powder into a metallographic mounting machine, and control the pressure of the mounting machine to 0.5MPa , the heating temperature is 150°C, the holding time is 5min, the cooling time is 3min, the amount of mixed powder is controlled so that the height of the mounted sample is about 0.5cm, and the diameter is 2cm to make a metallographic sample; The melting of the powder will cause the large particle powder to settle to the bottom naturally, so directly grind the bottom of the metallographic sample with 6000 mesh sandpaper until the large particle powder can be seen, and the grinding time is 3 minutes to make the initial polished sample; for the top of sample C, use 400 mesh , 1000-mesh and 2000-mesh sandpapers are ground step by step, and the thi...

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Abstract

The invention discloses a preparation method of a large-particle powder transmission electron microscope, which belongs to the technical field of the preparation of a transmission electroscope sample. The preparation method comprises the following steps: mixing large-particle powder and carbon-containing conductive powder to form mixed powder, mounting the sample with a gold phase, grinding the bottom, grinding the top, fixing and washing the sample, and thinning by virtue of ion, thereby preparing the sample capable of being used for the transmission electron microscope observation. In a large-particle powder transmission electron microscope sample prepared by adopting the method, large particles with a thin area on multiple edges are difficult to find, the observation of a high-resolution image of an atomic resolution level is realized, and the unclear problem of the high-resolution image caused by the drifting or jittering of the sample can also be avoided; and the preparation method is short in sample preparation period, simple in operation, high in implementation and low in cost.

Description

technical field [0001] The invention belongs to the technical field of transmission electron microscope sample preparation, and in particular relates to a preparation method of a large particle powder transmission electron microscope sample. Background technique [0002] With the development of new materials, in recent years, the need for in-depth research on the surface coating state and crystal structure of micron-scale large-particle powders has become more and more urgent, such as positive electrode materials for lithium-ion batteries, various magnetic functional materials, and hard materials. alloy. At present, for large-particle powder samples, in order to meet the requirements of transmission electron microscope observation, there are three main sample preparation methods: the first one is directly dispersed on the carbon support film or micro-grid, for micron-sized particles, even the edge of the sample will be very thick , it is not easy to carry out transmission e...

Claims

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Application Information

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IPC IPC(8): G01N23/22
CPCG01N23/2202
Inventor 徐云培杜志伟夏雯刘淑凤韩小磊李婷李聪
Owner GUOBIAO BEIJING TESTING & CERTIFICATION CO LTD
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