阅读说明：本技术 硅钢ebsd试样的制备方法 (Preparation method of silicon steel EBSD sample ) 是由 杨峥 *** 牟祖茂 徐辉 王德宝 程志远 于 2019-10-11 设计创作，主要内容包括：本发明公开了一种硅钢EBSD试样的制备方法,包括步骤：S1、镶嵌：采用导电型镶嵌料对硅钢试样进行镶嵌；S2、机械抛光：对镶嵌后的试样进行抛光；S3、配置腐蚀剂；S4、侵蚀：将抛光后的试样浸入腐蚀剂中,侵蚀时间为6-8秒；S5、清洁：对侵蚀后的试样表面进行清洁。本发明的硅钢EBSD试样的制备方法,可以制备符合硅钢EBSD分析的试样,制备过程操作简单,易于掌握,通过对试样的机械抛光和简单的化学浸蚀,可以提高硅钢EBSD试样的衍射花样解析率,效果良好。(The invention discloses a preparation method of a silicon steel EBSD sample, which comprises the following steps: s1, inlaying: embedding the silicon steel sample by adopting a conductive embedding material; s2, mechanical polishing: polishing the embedded sample; s3, preparing a corrosive agent; s4, erosion: immersing the polished sample into a corrosive agent, wherein the corrosion time is 6-8 seconds; s5, cleaning: and cleaning the corroded surface of the sample. The preparation method of the silicon steel EBSD sample can be used for preparing the sample which accords with the analysis of the silicon steel EBSD, the preparation process is simple to operate and easy to master, the diffraction pattern resolution of the silicon steel EBSD sample can be improved through mechanical polishing and simple chemical etching of the sample, and the effect is good.)

1. The preparation method of the silicon steel EBSD sample is characterized by comprising the following steps:

s1, inlaying: embedding the silicon steel sample by adopting a conductive embedding material;

s2, mechanical polishing: polishing the embedded sample;

s3, preparing a corrosive agent;

s4, erosion: immersing the polished sample into a corrosive agent, wherein the corrosion time is 6-8 seconds;

s5, cleaning: and cleaning the corroded surface of the sample.

2. The method for preparing the silicon steel EBSD sample according to claim 1, wherein the step S2 includes:

s201, carrying out primary polishing treatment on a sample by adopting 240-mesh aluminum oxide sand paper;

s202, carrying out secondary grinding treatment on the sample by adopting 240-mesh aluminum oxide sand paper;

s203, carrying out primary polishing treatment on the sample by using 600-mesh aluminum oxide sand paper;

s204, carrying out secondary grinding treatment on the sample by using 600-mesh alumina sand paper;

s205, carrying out primary polishing treatment on the sample by adopting 1000-mesh alumina sand paper;

s206, carrying out secondary grinding treatment on the sample by adopting 1000-mesh aluminum oxide sand paper;

s207, carrying out primary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s208, carrying out secondary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s209, carrying out first polishing treatment on the sample by adopting a 3um diamond polishing agent;

s210, carrying out secondary polishing treatment on the sample by adopting a 3um diamond polishing agent;

s211, carrying out first polishing treatment on the sample by adopting a 0.05um silicon oxide polishing agent;

and S212, carrying out secondary polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent.

3. The method for preparing the silicon steel EBSD sample according to claim 2, wherein when the sample is subjected to first polishing treatment by using 240-mesh alumina sand paper, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the sample is subjected to secondary polishing treatment by adopting 240-mesh aluminum oxide sand paper, the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

4. The method for preparing the silicon steel EBSD sample according to claim 2, wherein when the sample is subjected to first polishing treatment by using 600-mesh alumina sand paper, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the 600-mesh aluminum oxide abrasive paper is used for polishing the sample for the second time, the polishing time for the second time is 2-4 minutes, and the pressure is 8-12N.

5. The method for preparing the silicon steel EBSD sample according to claim 2, wherein when the sample is subjected to first polishing treatment by using 1000-mesh alumina sand paper, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the 1000-mesh aluminum oxide abrasive paper is used for polishing the sample for the second time, the polishing time for the second time is 2-4 minutes, and the pressure is 8-12N.

6. The method for preparing the silicon steel EBSD sample according to claim 2, characterized in that 9um diamond polishing agent is adopted to carry out the first polishing treatment on the sample, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and carrying out secondary polishing treatment on the sample by adopting a 9-micron diamond polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

7. The method for preparing the silicon steel EBSD sample according to claim 2, characterized in that a 3um diamond polishing agent is adopted to carry out first polishing treatment on the sample, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and carrying out secondary polishing treatment on the sample by adopting a 3-micrometer diamond polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

8. The method for preparing the silicon steel EBSD sample according to claim 2, wherein a silicon oxide polishing agent with 0.05um is adopted to carry out first polishing treatment on the sample, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and (3) carrying out secondary polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

9. The method for preparing the silicon steel test piece according to any one of claims 1 to 8, wherein the etchant is a mixture of nitric acid and absolute ethyl alcohol in step S3.

10. The method for preparing the silicon steel sample according to claim 9, wherein in the step S3, the content of the nitric acid in the etchant is 2% by mass, and the content of the absolute ethyl alcohol in the etchant is 98% by mass.

Technical Field

The invention belongs to the technical field of silicon steel EBSD samples, and particularly relates to a preparation method of a silicon steel EBSD sample.

Background

EBSD (Electron Back Scattering diffraction) is a material microstructure detection and analysis technology which is increasingly widely established and applied in recent years, can carry out submicron-level crystallography analysis on materials, and can carry out observation, statistical determination and quantitative analysis on grain boundary types, orientations, orientation differences, structures and distribution thereof of polycrystalline materials, thereby establishing quantitative and semi-quantitative relations between grain boundary structures, orientations, textures and the like and the performance of the polycrystalline materials, and being an important experimental technology for modern material research.

Texture (i.e. orientation distribution rule of polycrystal) in the silicon steel has great influence on the performance of the silicon steel material, non-oriented silicon steel requires low iron loss and high magnetic induction intensity, and whether coarse grains with favorable texture orientation can be obtained after recrystallization annealing is the key of the performance of the non-oriented silicon steel.

The EBSD technology can be applied to research on the aspects of silicon steel micro-area orientation, texture, recrystallization and the like, can obtain parameters such as crystal grain orientation, orientation difference between crystal grains and the like, and can lay a foundation for establishing texture control technical parameters of materials.

The existing preparation method of the silicon steel EBSD sample mainly comprises mechanical polishing and electrolytic polishing, the sample preparation process is complex, electrolytic polishing parameters are not easy to determine and are particularly difficult to master by beginners, and the EBSD diffraction pattern acquisition is greatly influenced by the sample preparation level, so that the diffraction pattern resolution rate is low.

Disclosure of Invention

The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of a silicon steel EBSD sample, aiming at improving the diffraction pattern resolution of the silicon steel EBSD sample.

In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the silicon steel EBSD sample comprises the following steps:

s1, inlaying: embedding the silicon steel sample by adopting a conductive embedding material;

s2, mechanical polishing: polishing the embedded sample;

s3, preparing a corrosive agent;

s4, erosion: immersing the polished sample into a corrosive agent, wherein the corrosion time is 6-8 seconds;

s5, cleaning: and cleaning the corroded surface of the sample.

The step S2 includes:

s201, carrying out primary polishing treatment on a sample by adopting 240-mesh aluminum oxide sand paper;

s202, carrying out secondary grinding treatment on the sample by adopting 240-mesh aluminum oxide sand paper;

s203, carrying out primary polishing treatment on the sample by using 600-mesh aluminum oxide sand paper;

s204, carrying out secondary grinding treatment on the sample by using 600-mesh alumina sand paper;

s205, carrying out primary polishing treatment on the sample by adopting 1000-mesh alumina sand paper;

s206, carrying out secondary grinding treatment on the sample by adopting 1000-mesh aluminum oxide sand paper;

s207, carrying out primary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s208, carrying out secondary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s209, carrying out first polishing treatment on the sample by adopting a 3um diamond polishing agent;

s210, carrying out secondary polishing treatment on the sample by adopting a 3um diamond polishing agent;

s211, carrying out first polishing treatment on the sample by adopting a 0.05um silicon oxide polishing agent;

and S212, carrying out secondary polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent.

When the sample is subjected to primary polishing treatment by adopting 240-mesh aluminum oxide sand paper, the primary polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the sample is subjected to secondary polishing treatment by adopting 240-mesh aluminum oxide sand paper, the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

When the 600-mesh aluminum oxide abrasive paper is used for carrying out first polishing treatment on the sample, the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the 600-mesh aluminum oxide abrasive paper is used for polishing the sample for the second time, the polishing time for the second time is 2-4 minutes, and the pressure is 8-12N.

When the sample is subjected to primary polishing treatment by using 1000-mesh alumina sand paper, the primary polishing treatment time is 2-4 minutes, and the pressure is 28-32N; when the 1000-mesh aluminum oxide abrasive paper is used for polishing the sample for the second time, the polishing time for the second time is 2-4 minutes, and the pressure is 8-12N.

Carrying out first polishing treatment on the sample by adopting a 9-micron diamond polishing agent, wherein the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and carrying out secondary polishing treatment on the sample by adopting a 9-micron diamond polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

Carrying out first polishing treatment on the sample by adopting a 3-micrometer diamond polishing agent, wherein the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and carrying out secondary polishing treatment on the sample by adopting a 3-micrometer diamond polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

Carrying out first polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent, wherein the first polishing treatment time is 2-4 minutes, and the pressure is 28-32N; and (3) carrying out secondary polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent, wherein the secondary polishing treatment time is 2-4 minutes, and the pressure is 8-12N.

In step S3, the etchant is formed by mixing nitric acid and absolute ethyl alcohol.

In step S3, the content of nitric acid in the etchant is 2% by mass, and the content of absolute ethyl alcohol in the etchant is 98% by mass.

The preparation method of the silicon steel EBSD sample can be used for preparing the sample which accords with the analysis of the silicon steel EBSD, the preparation process is simple to operate and easy to master, the diffraction pattern resolution of the silicon steel EBSD sample can be improved through mechanical polishing and simple chemical etching of the sample, and the effect is good.

Drawings

The description includes the following figures, the contents shown are respectively:

FIG. 1 is a process flow diagram of the method for preparing a silicon steel EBSD sample according to the present invention;

fig. 2 is a diffraction band contrast diagram.

Detailed Description

The following detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings for a purpose of helping those skilled in the art to more fully, accurately and deeply understand the inventive concept and technical solution of the present invention and to facilitate its implementation.

As shown in fig. 1, the invention provides a preparation method of a silicon steel EBSD sample, which comprises the following steps:

s1, inlaying: embedding the silicon steel sample by adopting a conductive embedding material;

s2, mechanical polishing: polishing the embedded sample;

s3, preparing a corrosive agent;

s4, erosion: immersing the polished sample into a corrosive agent, wherein the corrosion time is 6-8 seconds;

s5, cleaning: and cleaning the corroded surface of the sample.

Specifically, in step S1, the silicon steel sample is about 10mm × 10mm in size, and is inlaid with a conductive insert, and the test surface is a rolled full cross section.

The above step S2 includes the following processes:

s201, carrying out primary polishing treatment on a sample by adopting 240-mesh aluminum oxide sand paper;

s202, carrying out secondary grinding treatment on the sample by adopting 240-mesh aluminum oxide sand paper;

s203, carrying out primary polishing treatment on the sample by using 600-mesh aluminum oxide sand paper;

s204, carrying out secondary grinding treatment on the sample by using 600-mesh alumina sand paper;

s205, carrying out primary polishing treatment on the sample by adopting 1000-mesh alumina sand paper;

s206, carrying out secondary grinding treatment on the sample by adopting 1000-mesh aluminum oxide sand paper;

s207, carrying out primary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s208, carrying out secondary polishing treatment on the sample by adopting a 9um diamond polishing agent;

s209, carrying out first polishing treatment on the sample by adopting a 3um diamond polishing agent;

s210, carrying out secondary polishing treatment on the sample by adopting a 3um diamond polishing agent;

s211, carrying out first polishing treatment on the sample by adopting a 0.05um silicon oxide polishing agent;

and S212, carrying out secondary polishing treatment on the sample by adopting 0.05um of silicon oxide polishing agent.

That is, in the step S2, the automatic sample grinding machine is used to polish the sample in the order of 240-600-1000-9 um diamond polishing agent-3 um diamond polishing agent-0.05 um silicon oxide polishing agent, and each polishing is divided into two times until the sample is polished to the mirror surface.

In the step S201, an automatic sample grinding machine is adopted, and 240-mesh alumina sand paper is adopted to perform a first grinding treatment on the sample, wherein the duration of the first grinding treatment is 2-4 minutes, and the pressure is 28-32N.

In the step S202, when the automatic sample grinding machine is used and the 240-mesh alumina sand paper is used to perform the second grinding treatment on the sample, the duration of the second grinding treatment is 2 to 4 minutes, and the pressure is 8 to 12N.

In step S203, when an automatic sample grinding machine is used and 600-mesh alumina sand paper is used to perform a first grinding process on the sample, the duration of the first grinding process is 2 to 4 minutes, and the pressure is 28 to 32N.

In the step S204, when the automatic sample grinding machine is used and 600-mesh alumina sand paper is used to perform the second grinding treatment on the sample, the duration of the second grinding treatment is 2-4 minutes, and the pressure is 8-12N.

In step S205, when the sample is subjected to the first polishing treatment by using a 1000-mesh alumina sand paper using an automatic sample grinding machine, the duration of the first polishing treatment is 2 to 4 minutes, and the pressure is 28 to 32N.

In the step S206, when the automatic sample grinding machine is used and the 1000-mesh alumina sand paper is used to perform the second grinding treatment on the sample, the duration of the second grinding treatment is 2 to 4 minutes, and the pressure is 8 to 12N.

In the step S207, an automatic sample grinding machine is adopted, and a 9um diamond polishing agent is adopted to perform a first polishing treatment on the sample, wherein the duration of the first polishing treatment is 2-4 minutes, and the pressure is 28-32N.

In the step S208, an automatic sample grinding machine is adopted, and a 9um diamond polishing agent is adopted to perform a second polishing treatment on the sample, wherein the duration of the second polishing treatment is 2-4 minutes, and the pressure is 8-12N.

In the step S209, an automatic sample grinding machine is adopted, and a 3um diamond polishing agent is adopted to perform a first polishing treatment on the sample, wherein the duration of the first polishing treatment is 2-4 minutes, and the pressure is 28-32N.

In the step S210, an automatic sample grinding machine is adopted, and a 3um diamond polishing agent is adopted to perform a second polishing treatment on the sample, wherein the duration of the second polishing treatment is 2-4 minutes, and the pressure is 8-12N.

In the step S211, an automatic sample grinding machine is adopted, and a 0.05um silicon oxide polishing agent is adopted to perform a first polishing treatment on the sample, wherein the duration of the first polishing treatment is 2-4 minutes, and the pressure is 28-32N.

In the step S212, an automatic sample grinding machine is adopted, and a 0.05um silicon oxide polishing agent is adopted to perform a second polishing treatment on the sample, wherein the duration of the second polishing treatment is 2-4 minutes, and the pressure is 8-12N.

In this embodiment, in step S201, the duration of the first polishing process performed on the sample with 240-mesh alumina sand paper is 3 minutes, and the pressure is 30N. In the above step S202, the duration of the second polishing treatment of the test piece with 240-mesh alumina sandpaper was 3 minutes, and the pressure was 10N. In the above step S203, the duration of the first polishing treatment of the sample with 600 mesh alumina paper was 3 minutes, and the pressure was 30N. In the above step S204, the duration of the second polishing treatment of the test piece with 600 mesh alumina paper was 3 minutes and the pressure was 10N. In the above step S205, the duration of the first polishing treatment of the sample with 1000-mesh alumina sandpaper was 3 minutes, and the pressure was 30N. In the above step S206, the duration of the second polishing treatment of the sample with 1000-mesh alumina sandpaper was 3 minutes, and the pressure was 10N. In the above step S207, the duration of the first polishing treatment of the sample with 9um of diamond polishing agent was 3 minutes and the pressure was 30N. In the above step S208, the duration of the second polishing process of the sample with 9um of diamond polishing agent was 3 minutes and the pressure was 10N. In the above step S209, the duration of the first polishing treatment of the sample with 3um of diamond polishing agent was 3 minutes, and the pressure was 30N. In the above step S210, the duration of the second polishing process of the sample with 3um diamond polishing agent was 3 minutes and the pressure was 10N. In the above step S211, the duration of the first polishing treatment of the sample with 0.05um of the silicon oxide polishing agent was 3 minutes and the pressure was 30N. In the above step S212, the duration of the second polishing treatment of the sample with 0.05um of the silicon oxide polishing agent was 3 minutes and the pressure was 10N.

Through the mechanical polishing process, the sand paper is sequentially increased from 240 meshes, 600 meshes to 1000 meshes, the polishing agent is sequentially reduced from 9um, 3um and 0.05um, each pass of polishing is divided into two times, the polishing pressure of each pass is set to be different, the brightness of the surface of the sample can be ensured, the surface quality of the sample can be improved, and the sample with high diffraction pattern resolution rate can be obtained.

In step S3, the etchant is formed by mixing nitric acid and absolute ethanol, and the mixture is uniformly stirred. The content of the nitric acid in the corrosive agent is 2 percent by mass, and the content of the absolute ethyl alcohol in the corrosive agent is 98 percent by mass. By using such an etchant, the brightness of the sample surface can be further improved, which contributes to obtaining a sample having a high diffraction pattern resolution.

In the step S4, the polished sample is immersed in the etchant for 6 to 8 seconds and then taken out, the surface of the sample is cleaned with deionized water and absolute ethyl alcohol, and then the sample is dried by blowing to obtain the sample.

And (3) putting the prepared sample into a scanning electron microscope, collecting the EBSD pattern, and obtaining a diffraction band contrast diagram, wherein the resolution rate of the diffraction pattern is as high as 99.77% as shown in figure 2.

The preparation method has the advantages that vibration polishing or electrolytic polishing is not needed, the electrolytic polishing mode is difficult to control, electrolyte, electrolytic voltage and time are required to be adjusted, the change of mechanical polishing force value and corrosion are combined, the stress layer on the surface of the sample is removed, the operation is simple, the control and implementation are easy, the effect is good, and the prepared sample meets the requirements of silicon steel EBSD analysis.

The invention is described above with reference to the accompanying drawings. It is to be understood that the specific implementations of the invention are not limited in this respect. Various insubstantial improvements are made by adopting the method conception and the technical scheme of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.