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Method for preparing metal material EBSD (electron backscatter diffraction) sample on basis of ultra-low temperature weak current control

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

Inactive Publication Date: 2019-06-18
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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  • Method for preparing metal material EBSD (electron backscatter diffraction) sample on basis of ultra-low temperature weak current control
  • Method for preparing metal material EBSD (electron backscatter diffraction) sample on basis of ultra-low temperature weak current control
  • Method for preparing metal material EBSD (electron backscatter diffraction) sample on basis of ultra-low temperature weak current control

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Experimental program
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Effect test

Embodiment 1

[0035] What adopted in the present embodiment is the rolled state TC4 (Ti-6Al-4V) rod, and adopts a kind of ultra-low temperature, weak current control metal material EBSD sample preparation method of the present invention, specifically comprises 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) Electropolishing 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 set up. to 60V, the specimen...

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 piece of 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) Electropolishing 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 nitr...

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) Electropolishing 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 to abo...

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Abstract

The present invention provides a general electrolytic polishing method for preparing a metal material EBSD (electron backscatter diffraction) sample. The invention aims to improve the quality, efficiency and stability of the preparation of alloy EBSD samples. According to the method, an electrolytic sample is pre-treated at an earlier stage; an electrolytic polishing liquid containing only perchloric acid and absolute ethyl alcohol is prepared; and with a stainless steel sheet adopted as a cathode, the sample requiring electrolytic polishing adopted as an anode, and electrolytic polishing is performed under low temperature and weak current. The method has the advantages of simple equipment, high practicability and simple operation, high test repeatability, good sample preparation effect, great economic benefits and high popularization value. With the method adopted, the debugging of electrolytic polishing parameters is not required in a preparation process.

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, especially texture analysis in material science. 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 Applications(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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