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Electropolishing preparation method of sample for EBSD (Electron Back-Scattered Diffraction) analysis of titanium-aluminum alloy

An electropolishing, base alloy technology, applied in the preparation of test samples, analysis of materials, sampling, etc., to achieve the effect of simple and flexible operation, portable equipment, and large sample area

Inactive Publication Date: 2017-11-28
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no detailed explanation of the method for preparing samples by electrolytic polishing of titanium-aluminum-based alloys. In view of the important application value of EBSD analysis and testing technology in titanium-aluminum-based alloys, it is urgent to establish a complete set of EBSD test samples for titanium-aluminum-based alloys. Electrolytic Polishing Preparation Method

Method used

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  • Electropolishing preparation method of sample for EBSD (Electron Back-Scattered Diffraction) analysis of titanium-aluminum alloy
  • Electropolishing preparation method of sample for EBSD (Electron Back-Scattered Diffraction) analysis of titanium-aluminum alloy
  • Electropolishing preparation method of sample for EBSD (Electron Back-Scattered Diffraction) analysis of titanium-aluminum alloy

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preparation example Construction

[0033] In the specific implementation process, the electrolytic polishing preparation method of the sample for EBSD analysis of the titanium-aluminum base alloy of the present invention comprises the following steps:

[0034] (1) Sample pre-treatment:

[0035] As an intermetallic compound, titanium-aluminum-based alloy is hard, with a hardness of up to HRC50~HRC60, and is relatively brittle at room temperature. The sample can be cut by wire cutting or water jet cutting (slow wire cutting during wire cutting, so as to facilitate subsequent grinding). Samples should not be processed by milling machines, lathes and grinding machines. The size of the cut BESD sample is usually below 10mm×10mm×5mm, of which 5mm is the limit value of the sample height, and the height direction of the sample is also the ND direction (normal direction) during the test. Preferably, the size of the cut BESD sample is (5-7) mm×(3-6) mm×(2-4) mm, where (2-4) mm is the height direction, and the difference...

Embodiment 1

[0047] In this example, for the titanium-aluminum-based alloy subjected to high-temperature compression using the Gleeble thermal simulation testing machine, the sample for EBSD analysis was prepared by electrolytic polishing, including the following steps:

[0048] (1) Sample preparation:

[0049] Firstly, line-cut a sheet-like sample with a thickness of 0.5 mm at the center of the cake-shaped sample along the direction of compression. Since the sample is small and thin, it is necessary to move the wire slowly to reduce the depth of the wire-cut trace; wipe off the oil on the surface of the wire-cut sample, and Both sides of the cut flake sample are polished with 40#~800# sandpaper, and one side (test surface) is required to continue to be polished with standard metallographic method 1000#~5000# sandpaper; the thin sample is glued to the surface of the iron block with 502 for mechanical Polish until the surface is bright, then soak the thin slice sample in acetone, and clean ...

Embodiment 2

[0058] In this embodiment, for the sheet-shaped titanium-aluminum-based alloy I-shaped piece stretched at room temperature, the electrolytic polishing method is used to prepare the sample for EBSD analysis, including the following steps:

[0059] (1) Sample preparation:

[0060] Use pliers to break off a small piece at the gauge length, about 6mm×5mm×1.9mm (1.9mm is the sample height, as the ND direction in the EBSD test), the two 6mm×5mm surfaces of the sample are relatively smooth (the two sides of the I-shaped piece have been Use 800# sandpaper to polish), as above, carry out standard metallographic treatment on the test surface, and use 1000#~7000# sandpaper to polish; use the sample holder to clamp the sample for mechanical polishing; then fully clean the sample in alcohol and acetone spare.

[0061] (2) Electropolishing experiment preparation:

[0062] According to perchloric acid 7%, methanol 59%, n-butanol 34% (both volume ratio) configuration electrolytic electrolyt...

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Abstract

The invention belongs to the technical field of non-ferrous metal analysis and particularly relates to an electropolishing preparation method of a sample for EBSD (Electron Back-Scattered Diffraction) analysis of a titanium-aluminum alloy. The electropolishing preparation method comprises the following steps: firstly, carrying out earlier stage treatment on the sample: determining the size of the sample to be smaller than 7mm*6mm*4mm, and carrying out standard metallographic treatment and mechanical polishing on the testing surface; secondly, setting up a portable device: connecting the sample with a positive pole of a power supply, connecting a stainless steel plate with a negative pole of the power supply and matching the bottom end of electrolyte with a magnetic stirrer; thirdly, preparing the electrolyte: selecting 4 to 12 percent of perchloric acid, 55 to 65 percent of methyl alcohol and the balance of n-butyl alcohol according to the volume ratio, wherein the total amount of the electrolyte is 700ml; putting the electrolyte into a beaker with the volume of 1L; fourthly, carrying out electrolysis treatment, washing and drying: controlling the temperature to be 30 DEG C below zero to 20 DEG C below zero, controlling the voltage to be 25 to 35V and controlling the polishing time to be 40 to 55 seconds. The electropolishing preparation method disclosed by the invention has the advantages of large surface area for treating the sample and suitability for preparing titanium-aluminum alloy samples with various components and various test purposes, which are prepared by different processing method. In addition, the electropolishing preparation method has the advantages of easiness and flexibility in operation, no restriction from site facilities and the like, good polishing effect and high rate of finished products; the device has the characteristics of high mobility, low cost, easiness in promotion and wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of nonferrous metal analysis, and in particular relates to an electrolytic polishing preparation method of a sample for EBSD analysis of a titanium-aluminum base alloy. Background technique [0002] Since the 1990s, electron backscatter pattern crystal micro-domain orientation and crystal structure analysis technology based on scanning electron microscope technology has developed rapidly, and its wide application in the characterization of material microstructure has been realized. This technology is called Electron Backscattered Diffraction technology, the English name is Electron Backscattered Diffraction, hereinafter referred to as EBSD technology. The origin of this technology can be traced back to around the 1920s. When people observed calcite in a scanning electron microscope, they accidentally discovered a secondary diffraction pattern, called the Kikuchi pattern. This discovery laid the theoretical f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28C25F3/16
CPCG01N1/286C25F3/16G01N2001/2873
Inventor 董书琳王强刘铁王凯苑轶
Owner NORTHEASTERN UNIV
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