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Preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples

A high magnetic induction orientation and sample preparation technology, which is applied in the field of preparation of high magnetic induction orientation silicon steel EBSD samples, can solve the problems of sample occlusion, limited number of placed samples, and increased number of times of scanning electron microscope vacuuming, etc., to achieve simple operation, The Effect of Complexity Reduction

Inactive Publication Date: 2016-01-20
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to its own characteristics, the electrolytic polishing corrosion method has precise requirements on current, voltage, temperature and time, and the operation is relatively complicated; and after electrolytic polishing corrosion, the edge of the sample observation surface will inevitably be thinned. phenomenon, while the hot-rolled and primary recrystallized annealed texture of high magnetic induction oriented silicon steel has a special texture gradient along the thickness direction, and this gradient has a very important influence on the final product performance
Therefore, for the acquisition of texture data of high magnetic induction oriented silicon steel hot rolling and primary recrystallization, it is necessary to collect the entire thickness direction, and the electrolytic polishing corrosion that will cause edge thinning obviously cannot meet the EBSD sample preparation requirements of high magnetic induction oriented silicon steel ; At the same time, when performing EBSD data collection on samples after electrolytic polishing, it is necessary to deflect the observation surface by 70°. If multiple samples are overlapped, once the sample and the observation surface of the sample are not parallel, the sample will be blocked and EBSD cannot be performed. The phenomenon of data collection
Therefore, the number of samples placed on the sample stage is limited each time, resulting in an increase in the number of repeated vacuuming of the scanning electron microscope, wasting a lot of time, resulting in low efficiency of EBSD experiments, and thus affecting production efficiency

Method used

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  • Preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples
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  • Preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples

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Embodiment 1

[0041] A method for preparing an EBSD sample of high magnetic induction oriented silicon steel. The concrete steps of described preparation method are:

[0042] Step 1: Cutting one kind of high magnetic induction oriented silicon steel into original samples, the size of the original samples is RD×ND×TD=(9~11)×(0.3~4)×(4~6).

[0043] Step 2. Embed the original sample described in step 1 into the conductive mounting material to obtain the following: figure 1 and figure 2 The mosaic sample shown; the height H of the mosaic sample is 6-8 mm, and the cumulative thickness B of the original mosaic sample in the mosaic sample is ≤ 4 mm.

[0044] Step 3: Perform mechanical polishing on the mosaic sample, polish the target observation surface until the roughness Ra is 0.012-0.05 μm, obtain a mechanically polished sample, wash and dry it.

[0045] Step 4, cutting the cleaned and dried mechanically polished sample into a size of RD×ND×TD=(14~16)×(6~8)×(6~8) mm to obtain a cut sample; T...

Embodiment 2

[0050] A method for preparing an EBSD sample of high magnetic induction oriented silicon steel. The concrete steps of described preparation method are:

[0051] Step 1. Cut 2~5 different high magnetic induction oriented silicon steels into original samples respectively. The size of a single original sample is RD×ND×TD=(9~11)×(0.3~0.8)×(4~ 6).

[0052] Step 2. Embed the original sample described in step 1 into the conductive mounting material to obtain the following: figure 1 and figure 2 The mosaic sample shown; the height H of the mosaic sample is 6-8 mm, and the cumulative thickness B of the original mosaic sample in the mosaic sample is ≤ 4 mm.

[0053] Step 3: Perform mechanical polishing on the mosaic sample, polish the target observation surface until the roughness Ra is 0.012-0.05 μm, obtain a mechanically polished sample, wash and dry it.

[0054] Step 4: Cut the cleaned and dried mechanically polished sample into a size of RD×ND×TD=(14~16)×(6~8)×(6~8) mm, and obt...

Embodiment 3

[0059] A method for preparing an EBSD sample of high magnetic induction oriented silicon steel. The concrete steps of described preparation method are:

[0060] Step 1. Cut 6~8 kinds of high magnetic induction oriented silicon steel into original samples respectively. The size of a single original sample is RD×ND×TD=(9~11)×(0.3~0.5)×(4~ 6).

[0061] Step 2. Embed the original sample described in step 1 into the conductive mounting material to obtain the following: figure 1 and figure 2 The mosaic sample shown; the height H of the mosaic sample is 6-8 mm, and the cumulative thickness B of the original mosaic sample in the mosaic sample is ≤ 4 mm.

[0062] Step 3: Perform mechanical polishing on the mosaic sample, polish the target observation surface until the roughness Ra is 0.012-0.05 μm, obtain a mechanically polished sample, wash and dry it.

[0063] Step 4, cutting the cleaned and dried mechanically polished sample into a size of RD×ND×TD=(14~16)×(6~8)×(6~8) mm to obt...

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Abstract

The invention provides a preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples. According to the technical scheme, 1 to 10 different types of high-magnetic-induction grain-oriented silicon steel are cut into original samples independently, wherein the size of original samples meets the equation RD*ND*TD=(9-11)*(0.3-4)*(4-6); the original samples are embedded in a conductivity type inlay to obtain an inlay sample; mechanical polishing is conducted on the inlay sample, the inlay sample is cut into cut samples with the size meeting the equation RD*ND*TD=(14-16)*(6-8)*Hmm, and washing and blow-drying are conducted; then, materials are prepared according to the volume ratio, of NHO3 to glacial acetic acid to C2H5OH, of 4 to 1 to 94-97, and mixing is conducted to obtain destressed corrosive liquid; finally, the destressed corrosive liquid is dropwise added to the target observation faces of the cut samples at the speed of 1-2 drops per second for 8-10 seconds, and rapid cleaning and blow-drying are conducted. The preparation method has the advantages that operation is easy and convenient, the requirement for conducting data acquisition on high-magnetic-induction grain-oriented silicon steel in the whole thickness direction can be met, the vacuumizing time can be saved, and the detection efficiency can be improved.

Description

technical field [0001] The invention belongs to the technical field of silicon steel EBSD samples. In particular, it relates to a method for preparing a high magnetic induction oriented silicon steel EBSD sample. Background technique [0002] Electrical steel, also known as silicon steel sheet, is the most widely used soft magnetic alloy in electrical, electronics and national defense military industries, and is also the functional metal material with the largest output. It is often used to make iron cores for various generators, motors and transformers. It occupies a very important position in the national economy. According to the classification of grain orientation, silicon steel sheets are divided into oriented silicon steel and non-oriented silicon steel, in which the core of oriented silicon steel is a Gaussian texture with a texture orientation of {110}<001>. The {110}<001> texture has only a pair of <001> directions with the highest magnetic perme...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/32
Inventor 肖欢赵刚鲍思前叶传龙林希峰刘升
Owner WUHAN UNIV OF SCI & TECH
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