Preparation method of TEM electrolytic double-spray film sample of small-sized metal material

A technology of electrolytic double-spraying and metal materials, applied in the preparation of test samples, etc., can solve the problems of failure and fragmentation of nanocrystalline dual-phase rare earth permanent magnetic alloy TEM products, achieve good polishing effect, simple production, and shorten the preparation time the effect of time

Active Publication Date: 2017-11-24
武汉钢铁有限公司
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Problems solved by technology

Due to the impact of the double-sprayed electrolyte on the surface of the analyzed sample, it may cause fragmentation due to the brittleness of the nanocrystalline dual-phase rare earth permanent magnetic alloy sample, resulting in the failure of the production of nanocrystalline dual-phase rare earth permanent magnetic alloy TEM products

Method used

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Embodiment Construction

[0020] The technical scheme designed by the present invention comprises the steps:

[0021] 1) Prepare gasket:

[0022] Grind the surface of the low-carbon low-alloy steel material with 400-1200 sandpaper, and then use HF and H 2 o 2 The mixed solution is chemically thinned until it is reduced to 50-80 μm, and punched into a disc with an outer diameter of 3 mm and an inner hole diameter smaller than the narrow side of the metal sample with a punching machine, and then uses 800-1200 No. The curling generated in the process is ground flat, that is, a low-carbon low-alloy gasket is prepared; the carbon content of the low-carbon low-alloy steel material is less than 0.3% by weight, and the weight percentage content of the alloy is less than 5%.

[0023] 2) Grind a metal sample with a size of less than 2.5mm into a thickness of 50-80 μm and paste it on the gasket to ensure that the entire inner hole of the gasket is covered, that is, the size of the sample is successfully expande...

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Abstract

The invention discloses a method for preparing a TEM electrolytic double-spray film sample of a small-sized metal material. The method comprises the following steps: 1) grinding the surface of the low-carbon and low-alloy steel material with 400-1200 sandpaper, and then using HF and h 2 o 2 Chemically thinning the mixed solution of the metal sample, punching a disc with an outer diameter of 3mm and an inner hole diameter slightly smaller than the narrow side of the metal sample with a punching machine and grinding it flat to prepare a gasket; The metal sample is ground to a thickness of 50-80 μm and pasted on the gasket to ensure that the entire inner hole of the gasket is covered, and then the double-spray electrolytic thinning is carried out according to the conventional method, and the TEM electrolytic double-spray film sample can be prepared. The method of the present invention has the following advantages: 1) the sample preparation time is short, and the tissue observation effect is good; 2) in the sample thinning process, there is no pollution to the sample; 3) the gasket is simple to make, does not affect the conductivity of the sample, and the polishing effect good.

Description

technical field [0001] The invention belongs to the technical field of transmission electron microscope (TEM) sample preparation, and in particular relates to a method for preparing a TEM electrolytic double-spray film sample of a small-sized metal material. Background technique [0002] With the development of modern science and technology and industrial level, higher requirements are put forward for the performance of steel, and many properties of steel are determined by the substructure in the nanometer or smaller scale, such as subgrain boundary and phase interface structure Various crystal defects, precipitated phase distribution and state, etc., make transmission electron microscope analysis the main method of microstructure analysis in steel material research. However, in actual work, it is often encountered that the steel material size (width or diameter) is too small to prepare a qualified TEM thin film sample. For example, the diameter of steel cord produced in re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 关云邓照军马家艳王志奋许竹桃欧阳珉路吴立新杨志婷许颖
Owner 武汉钢铁有限公司
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