A kind of ultra-low temperature weak current control metal material EBSD sample preparation method

A sample preparation and metal material technology, applied in the analysis of materials, material analysis using wave/particle radiation, instruments, etc., can solve the unfavorable application and development of EBSD technology, the ecological environment hazards of scientific research workers, increase the input of manpower and material resources, etc. problem, to achieve the effect of good polishing effect, high repeatability and simple operation

Inactive Publication Date: 2021-11-09
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that there is currently no universal electrolytic polishing solution and electrolytic corrosion method for the sample preparation of alloy EBSD. For the preparation of metal material EBSD samples, it is necessary to select the polishing solution experimentally, or to continuously adjust the electrolytic polishing parameters according to the polishing effect. Unnecessary manpower and material resources are added, and it is not conducive to the application and development of EBSD technology in material research, and most of the commonly used electrolytic polishing corrosion solutions are highly harmful nitric acid solutions and hydrofluoric acid solutions. It is very harmful to the relevant scientific research workers and the ecological environment

Method used

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  • A kind of ultra-low temperature weak current control metal material EBSD sample preparation method
  • A kind of ultra-low temperature weak current control metal material EBSD sample preparation method
  • A kind of ultra-low temperature weak current control metal material EBSD sample preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] In this example, rolled TC4 (Ti-6Al-4V) rods are used, and an ultra-low temperature, weak current control metal material EBSD sample preparation method of the present invention is adopted, which specifically includes the following steps:

[0036] (1) Sample preparation

[0037] Cut a cylindrical EBSD sample with a wire, first clean the oil on the surface of the sample with alcohol, and use 150#, 320#, 800#, 2000# sandpaper to pre-grind the surface of the sample to remove defects such as the oxide layer on the surface of the sample, and then Metallographic treatment was carried out on the test surface, and mechanical polishing was carried out. Finally, the sample was fully washed in alcohol and dried for later use.

[0038] (2) Electrolytic polishing test preparation

[0039] According to 10% perchloric acid and 90% absolute ethanol, 500ml of electrolyte solution was prepared, and an electrolytic polishing test platform was built. The electrolytic polishing solution was...

Embodiment 2

[0046] In this embodiment, the forged Zircaloy-4 alloy is used, and a sample preparation method for ultra-low temperature and weak current control metal material EBSD of the present invention is used to prepare a sample for analysis, which specifically includes the following steps:

[0047] (1) Sample preparation

[0048] A block EBSD sample was taken along the forging direction by wire cutting, and other steps were the same as step (1) of Example 1.

[0049] (2) Electrolytic polishing test preparation

[0050] Prepare 500ml of electrolyte solution according to 8% perchloric acid and 92% absolute ethanol, set up an electrolytic polishing test platform, put the electrolytic polishing solution in a beaker, pour liquid nitrogen to cool the electrolytic polishing solution to about -120°C, turn on the power switch to 60V, the specimen is held in tweezers, ready for electropolishing.

[0051] (3) Electropolishing treatment and subsequent treatment

[0052] When the added liquid n...

Embodiment 3

[0057] Using an ultra-low temperature and weak current control metal material EBSD sample preparation method of the present invention to electropolish the rolled GH99 superalloy to prepare a sample for texture analysis, specifically includes the following steps:

[0058] (1) Sample preparation

[0059] Cut the bulk sample with a wire, and mark the sample RD, TD and ND directions. The surface of the sample is treated by pre-grinding with sandpaper to remove defects such as oil stains and oxide layers on the surface. Finally, carry out metallographic treatment on the observation surface, mechanically polish it, wash it with alcohol and blow dry it for later use.

[0060] (2) Electrolytic polishing test preparation

[0061] According to 12% perchloric acid and 88% absolute ethanol, prepare 500ml of electrolyte solution, set up an electropolishing test platform, put the electrolytic polishing solution in a beaker, pour liquid nitrogen to cool the electrolytic polishing solution ...

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Abstract

The invention aims to provide a general electrolytic polishing method for the preparation of EBSD samples of metal materials, so as to improve the quality, efficiency and stability of the preparation of alloy EBSD samples. In this method, the electrolytic sample is firstly pretreated, and then the electrolytic polishing solution containing only perchloric acid and absolute ethanol is prepared. Finally, the stainless steel sheet is used as the cathode, and the required electrolytic polished sample is used as the anode, at low temperature and weak current. Electrolytic polishing. This method not only has simple equipment, strong practicability, and easy operation, but also is suitable for the preparation of EBSD samples of various metal materials. During the preparation process, there is no need to adjust the electrolytic polishing parameters. The test repeatability is high, the sample preparation effect is good, and it is economical. benefits and promotional value.

Description

technical field [0001] The invention belongs to the technical field of surface treatment of alloy materials, and in particular relates to an ultra-low temperature and weak current control metal material EBSD sample preparation method. Background technique [0002] Electron Backscatter Diffraction (EBSD) technology appeared in the late 1980s. With the continuous development of this technology, it has become an indispensable means of crystal structure in material science, especially texture analysis. Because its imaging depends on the orientation of the grains inside the material, it is also called orientation imaging microscopy. The microstructure map of orientation imaging can not only obtain the morphology, size and distribution information of grains, sub-grains and phases, but also obtain crystallographic information such as the crystal structure, grain orientation, and orientation difference of adjacent grains. , and using relevant processing software, you can also obtai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/203G01N23/2005
CPCG01N23/2005G01N23/203
Inventor 李阁平韩福洲刘承泽袁福森张英东郭文斌穆罕默德.阿里顾恒飞
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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