CN110967356A - Method for improving surface quality of plastic metal electron back scattering diffraction sample - Google Patents
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Abstract
The invention relates to a method for improving the surface quality of a plastic metal electron back scattering diffraction sample, which comprises the following steps: sample preparation, grinding, mechanical polishing, electrolytic polishing and ion etching; the invention has the advantages that: the polishing treatment can eliminate the residual trace of sample preparation on the surface of the sample; the mechanical polishing treatment can further eliminate the residual scratches of the surface sandpaper; the stress layer on the surface of the sample can be removed through electrolytic polishing and ion etching treatment, so that the characterization quality of electron back scattering diffraction is improved, the surface quality of the sample is improved, the stress layer on the surface is reduced, the resolvable rate of the sample is improved, and a higher-quality electron back scattering diffraction result is obtained.
Description
Technical Field
The invention relates to a method for improving the surface quality of a plastic metal electron back scattering diffraction sample.
Background
With the rapid development of the industrialization process, people have higher and higher demands for high-strength metal structural materials. The metal plastic forming technology is a method for effectively improving the strength of a metal material, the shape and the size of the metal are changed after plastic processing, the internal structure and the strength of the metal can be improved, and the strength of the metal material is closely related to the microstructure of the metal material. Therefore, the microstructure of the metal sample determines its macro-mechanical behavior. Generally, after plastic deformation processing is performed on a metal material, people need to observe and characterize a corresponding microstructure of the metal material, and analyze a strengthening mechanism of the metal material based on the observation and characterization, so that theoretical guidance and directions are provided for designing and optimizing the microstructure of a next-generation high-strength metal structure material. Therefore, accurate characterization of microstructure is an important link in the research of high-performance materials.
An Electron Back Scattering Diffraction (EBSD) technique is a commonly used characterization method for analyzing the microstructure of a structural material, and can accurately obtain information such as the size of crystal grains, the crystal orientation, the type of grain boundary, strain distribution, phase distribution and the like in a sample. Because diffracted electrons in the using process of the electron back scattering diffraction technology come from the surface of a sample with the depth of only dozens of nanometers, any pollution, stress layer and flatness on the surface of the sample can affect the result of electron back scattering diffraction, so that the quality of the finally obtained diffraction pattern is not high, and a large number of plastic deformation regions usually exist in plastic metal, so that the accurate experimental result is difficult to obtain in the characterization of the electron back scattering diffraction.
Disclosure of Invention
The invention aims to provide a method for improving the surface quality of a plastic metal electron back scattering diffraction sample, which can effectively improve the surface quality of the sample and the resolvable rate of electron back scattering diffraction.
In order to solve the technical problems, the invention is realized by the following technical scheme: a method of improving the surface quality of a plastic metal electron backscatter diffraction sample, the method comprising the steps of:
the method comprises the following steps: sample preparation: obtaining a cylindrical sample along the radial direction of the metal;
step two: polishing: carrying out surface polishing treatment on the radial section of the sample obtained in the step one;
step three: mechanical polishing: performing surface mechanical polishing treatment on the sample polished in the step two;
step four: electrolytic polishing: performing surface electrolytic polishing treatment on the sample subjected to the mechanical polishing treatment in the step three;
step five: ion etching: and carrying out surface ion etching treatment on the sample subjected to the four-point solution polishing treatment.
Preferably, the sample in the step one is cut by wire cut electrical discharge machining, and the height of the sample is equal to 10 mm.
Preferably, the sample in the second step is subjected to surface grinding treatment by SiC sand paper.
Preferably, the surface grinding times of the sample are four times, and the surface granularity of the SiC sand paper used in the four times of grinding is different.
Preferably, the sample in the third step is subjected to surface mechanical polishing treatment by an aqueous solution of MgO, and the aqueous solution of MgO includes MgO powder and water, and the volume ratio of MgO powder to water is 1: 4.
Preferably, the sample in the fourth step is subjected to surface electrolytic polishing treatment by a perchloric acid-alcohol mixed solution, wherein the perchloric acid-alcohol mixed solution comprises perchloric acid and alcohol, the volume ratio of the perchloric acid to the alcohol is 1:9, the electrolytic polishing voltage is 12-16V, the current is 0.5-2.0A, the electrolytic polishing time is 40-80 s, and the electrolytic polishing temperature is 0 ℃.
Preferably, the electropolishing temperature is controlled by placing a beaker containing a mixed perchloric acid alcohol solution in a container containing an ice-water mixture.
Preferably, the sample in the fifth step is subjected to surface ion etching treatment through an ion thinning instrument, the ion thinning instrument comprises an instrument ion etching gun, the current of the instrument ion etching gun is 1.0-1.5 mA, the voltage is 3.5-4.5 kV, the tilting angle is 10-15 degrees, and the etching time is 30-60 min.
In conclusion, the invention has the advantages that: 1. the plastic metal surface is processed by sample preparation, grinding, mechanical polishing, electrolytic polishing and ion etching, the sample prepared in the first step is prepared into a cylindrical shape, the sample surface treatment of operators is facilitated, the working efficiency and the surface treatment quality are improved, and the cylindrical sample is convenient to process; the sample surface is polished in the two steps, so that residual traces of sample preparation on the sample surface can be eliminated; the surface of the sample after being polished is subjected to mechanical polishing treatment through the third step, so that the residual scratches of the polished surface of sand paper can be further eliminated; the surface of the sample after mechanical polishing is subjected to electrolytic polishing treatment through the fourth step, so that the surface stress caused by mechanical polishing of the surface can be eliminated; and performing ion etching on the surface of the sample subjected to electrolytic polishing in the fifth step to further eliminate surface stress, wherein the stress layer on the surface of the sample can be removed by both electrolytic polishing and ion etching treatment, so that the characterization quality of electron back scattering diffraction is improved, the surface quality of the sample is improved, the stress layer on the surface is reduced, the resolvable rate of the sample is improved, and a higher-quality electron back scattering diffraction result is obtained.
Drawings
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a radial secondary electron image of an Al-Mg-Si alloy wire according to the present invention, wherein: a is a sample of the aluminum-magnesium-silicon alloy wire after mechanical polishing and electrolytic polishing, and b is a sample of the aluminum-magnesium-silicon alloy wire after mechanical polishing, electrolytic polishing and ion etching;
FIG. 2 is the result of radial electron back scattering diffraction of the Al-Mg-Si alloy wire of the present invention, wherein a is the orientation distribution diagram of the Al-Mg-Si alloy wire after the electrolytic polishing treatment, b is the orientation distribution diagram of the Al-Mg-Si alloy wire after the electrolytic polishing and ion etching treatment, c is the stress distribution diagram of the Al-Mg-Si alloy wire after the electrolytic polishing treatment, and d is the stress distribution diagram of the Al-Mg-Si alloy wire after the electrolytic polishing and ion etching treatment.
Detailed Description
As shown in fig. 1 and fig. 2, a method for improving the surface quality of a plastic metal electron back scattering diffraction sample comprises the following steps:
the method comprises the following steps: sample preparation: obtaining a cylindrical sample along the radial direction of the metal;
step two: polishing: carrying out surface polishing treatment on the radial section of the sample obtained in the step one;
step three: mechanical polishing: performing surface mechanical polishing treatment on the sample polished in the step two;
step four: electrolytic polishing: performing surface electrolytic polishing treatment on the sample subjected to the mechanical polishing treatment in the step three;
step five: ion etching: and carrying out surface ion etching treatment on the sample subjected to the four-point solution polishing treatment.
The plastic metal surface is processed by sample preparation, grinding, mechanical polishing, electrolytic polishing and ion etching, the sample prepared in the first step is prepared into a cylindrical shape, the sample surface treatment of operators is facilitated, the working efficiency and the surface treatment quality are improved, and the cylindrical sample is convenient to process; the sample surface is polished in the two steps, so that residual traces of sample preparation on the sample surface can be eliminated; the surface of the sample after being polished is subjected to mechanical polishing treatment through the third step, so that the residual scratches of the polished surface of sand paper can be further eliminated; the surface of the sample after mechanical polishing is subjected to electrolytic polishing treatment through the fourth step, so that the surface stress caused by mechanical polishing of the surface can be eliminated; and performing ion etching on the surface of the sample subjected to electrolytic polishing in the fifth step to further eliminate surface stress, wherein the stress layer on the surface of the sample can be removed by both electrolytic polishing and ion etching treatment, so that the characterization quality of electron back scattering diffraction is improved, the surface quality of the sample is improved, the stress layer on the surface is reduced, the resolvable rate of the sample is improved, and a higher-quality electron back scattering diffraction result is obtained.
The invention selects a drawn aluminum-magnesium-silicon alloy wire as a characterization object: the aluminum-magnesium-silicon alloy wire is obtained by performing cold drawing on an aluminum-magnesium-silicon alloy rod with the diameter of 9.5mm for 10 passes, the diameter of the aluminum-magnesium-silicon alloy wire is 2.5mm, and the total drawing deformation reaches 93.1%.
A method of improving the surface quality of a plastic metal electron backscatter diffraction sample, the method comprising the steps of:
the method comprises the following steps: sample preparation: adopting wire cut electrical discharge machining to obtain a cylindrical sample with the height of 10.0mm along the radial direction;
step two: polishing: sequentially grinding the radial cross section of the sample obtained in the step one by using 400#, 800#, 1200# and 2000# SiC sand paper;
step three: mechanical polishing: performing surface mechanical polishing treatment on the sample polished in the step two by using an MgO aqueous solution;
step four: electrolytic polishing: performing surface electrolytic polishing treatment on the sample subjected to the mechanical polishing treatment in the third step by using a perchloric acid alcohol mixed solution, wherein the voltage of electrolytic polishing is 14V, the current is 1.2A, the electrolytic polishing time is 50s, and the electrolytic polishing temperature is 0 ℃;
step five: ion etching: and (4) carrying out surface ion etching treatment on the sample subjected to the four-point solution polishing treatment by an ion thinning instrument with the model number of LEICA EM RES 101.
FIG. 1 shows the secondary electron morphology of the sample after electropolishing and the secondary electron morphology of the sample after electropolishing combined with ion etching, as shown in FIG. 1(a), the surface of the sample after electropolishing is relatively flat, and after ion etching, the surface of the sample shows a typical morphology after ion bombardment as shown in FIG. 1 (b).
Fig. 2 shows the comparison results of the electron backscatter diffraction characterization of the sample after electropolishing and the sample after electropolishing combined with ion etching, as shown in fig. 2(a) and 2(b), the white part is the area where the electron backscatter diffraction technique cannot obtain the sample information, i.e. the unsolved area; the presence of a large area of unsolved area in FIG. 2(a) indicates a low resolvability of the sample; the unsolved area proportion in fig. 2(b) is obviously reduced, so that the electron backscatter diffraction resolvable rate of the sample can be effectively improved by processing the sample by the method provided by the invention from the comparison result of fig. 2(a) and fig. 2 (b); furthermore, as shown in fig. 2(c) and 2(d), stress profiles are given, and a large number of high stress regions are observed in fig. 2(c), indicating that very large stresses exist at the surface of the sample; and the proportion of the high stress area in fig. 2(d) is obviously reduced, and most of the high stress area is a low stress area, so that the surface stress layer of the sample processed by the method can be effectively reduced.
Other embodiments of the present invention than the preferred embodiments described above will be apparent to those skilled in the art from the present invention, and various changes and modifications can be made therein without departing from the spirit of the present invention as defined in the appended claims.
Claims (8)
1. A method for improving the surface quality of a plastic metal electron back scattering diffraction sample is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: sample preparation: obtaining a cylindrical sample along the radial direction of the metal;
step two: polishing: carrying out surface polishing treatment on the radial section of the sample obtained in the step one;
step three: mechanical polishing: performing surface mechanical polishing treatment on the sample polished in the step two;
step four: electrolytic polishing: performing surface electrolytic polishing treatment on the sample subjected to the mechanical polishing treatment in the step three;
step five: ion etching: and carrying out surface ion etching treatment on the sample subjected to the four-point solution polishing treatment.
2. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 1, wherein the method comprises the following steps: the sample in the step one is cut by wire cut electrical discharge machining, and the height of the sample is equal to 10 mm.
3. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 1, wherein the method comprises the following steps: and carrying out surface grinding treatment on the sample in the step two through SiC sand paper.
4. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 3, wherein the method comprises the following steps: the surface grinding times of the sample are four times, and the surface granularity of SiC sand paper used in the four times of grinding is different.
5. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 1, wherein the method comprises the following steps: and the sample in the third step is subjected to surface mechanical polishing treatment by using an MgO aqueous solution, wherein the MgO aqueous solution comprises MgO powder and water, and the volume ratio of the MgO powder to the water is 1: 4.
6. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 1, wherein the method comprises the following steps: and performing surface electrolytic polishing treatment on the sample in the fourth step through a perchloric acid alcohol mixed solution, wherein the perchloric acid alcohol mixed solution comprises perchloric acid and alcohol, the volume ratio of the perchloric acid to the alcohol is 1:9, the electrolytic polishing voltage is 12-16V, the current is 0.5-2.0A, the electrolytic polishing time is 40-80 s, and the electrolytic polishing temperature is 0 ℃.
7. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 6, wherein the method comprises the following steps: the electropolishing temperature was controlled by placing a beaker containing a mixed perchloric acid alcohol solution in a container containing an ice-water mixture.
8. The method for improving the surface quality of the plastic metal electron back scattering diffraction sample according to claim 1, wherein the method comprises the following steps: and performing surface ion etching treatment on the sample in the fifth step through an ion thinning instrument, wherein the ion thinning instrument comprises an instrument ion etching gun, the current of the instrument ion etching gun is 1.0-1.5 mA, the voltage is 3.5-4.5 kV, the tilting angle is 10-15 degrees, and the etching time is 30-60 min.
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| CN115615784A (en) * | 2022-11-15 | 2023-01-17 | 广东风华高新科技股份有限公司 | Sample processing method for representing MLCC barium titanate ceramic grains |
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| CN115615784A (en) * | 2022-11-15 | 2023-01-17 | 广东风华高新科技股份有限公司 | Sample processing method for representing MLCC barium titanate ceramic grains |
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