CN110618149A - Preparation method of magnesium alloy EBSD sample - Google Patents
Preparation method of magnesium alloy EBSD sample Download PDFInfo
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- CN110618149A CN110618149A CN201910988922.0A CN201910988922A CN110618149A CN 110618149 A CN110618149 A CN 110618149A CN 201910988922 A CN201910988922 A CN 201910988922A CN 110618149 A CN110618149 A CN 110618149A
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- magnesium alloy
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
Abstract
The invention belongs to the technical field of detection sample preparation, and particularly relates to a preparation method of a magnesium alloy EBSD sample, which comprises the following steps: (1) mechanically polishing the surface of a magnesium alloy sample; (2) preparing an electrolytic polishing solution, and performing electrolytic polishing on the magnesium alloy sample after mechanical polishing; (3) carrying out OPS polishing on the magnesium alloy sample after electrolytic polishing; (4) and (4) cleaning and drying the magnesium alloy sample polished by the OPS in the step (3) to obtain a magnesium alloy EBSD sample. The method can effectively remove the surface stress layer and the oxide layer of the magnesium alloy, and the obtained magnesium alloy EBSD sample has a smooth and clean surface and a high calibration rate; and has low cost, simple preparation and high efficiency.
Description
Technical Field
The invention belongs to the technical field of detection sample preparation, and particularly relates to a preparation method of a magnesium alloy EBSD sample.
Background
Magnesium alloys have poor room temperature plastic formability due to less independent slip systems. In recent years, much magnesium alloy research focuses on the development of novel wrought magnesium alloys (particularly rare earth magnesium alloys), the development of special magnesium alloy section bar production processes (such as asynchronous rolling, EBSD and the like) and the development of special magnesium alloy forming processes (such as warm stamping and warm hydraulic stamping) and the like, and relates to the research on magnesium alloy plastic forming mechanism. The plastic deformation mechanism is usually studied on a microscopic scale, and an electron back-scattered diffraction-EBSD (electron back scattering diffraction-EBSD) system mounted on a Scanning Electron Microscope (SEM) is one of the most effective methods for doing the above.
The EBSD technology mainly has the following characteristics in 3 aspects: (1) the analysis precision of the crystal structure is high, and the technology becomes a new method for identifying the phase of a micro-area after X-ray diffraction and neutron diffraction at present; (2) is a technology for analyzing the crystal orientation micro-zone texture in a standard way; (3) high acquisition speed (100 points can be measured per second) and automatic acquisition of line distribution and surface distribution data on the sample. Therefore, the technology has the characteristics of micro-area analysis of a transmission electron microscope method and statistical analysis of a large-area of a sample by X-ray diffraction (or neutron diffraction) on the crystal structure and orientation analysis.
For magnesium alloy, pure electrolytic polishing, the existing electrolyte has high cost and complex configuration, for example, when AC2 electrolyte is used for preparing a sample, the calibration rate can meet the requirement, but the price is extremely high, reaches 5000 yuan/liter, and the production is completely stopped at present. And the EBSD sample prepared by pure OPS polishing has low efficiency, and takes more than half an hour for one sample. The polishing time for preparing the EBSD sample by pure OPS polishing is difficult to grasp, and if the time is too long, the second phase in the alloy is easy to fall off, so that the calibration rate is influenced; if the time is too short, the stress layer cannot be removed, and the calibration rate is also reduced.
Disclosure of Invention
In order to overcome the defects of high preparation cost and low quality of a magnesium alloy EBSD sample in the prior art, the invention provides a preparation method of the magnesium alloy EBSD sample. The method can effectively remove the surface stress layer and the oxide layer of the magnesium alloy, and the obtained magnesium alloy EBSD sample has a smooth and clean surface and a high calibration rate.
The invention is realized by the following technical scheme:
a preparation method of a magnesium alloy EBSD sample comprises the following steps:
(1) mechanically polishing the surface of a magnesium alloy sample;
(2) preparing an electrolytic polishing solution, and performing electrolytic polishing by taking the magnesium alloy sample after mechanical polishing as an anode;
(3) carrying out OPS polishing on the magnesium alloy sample after electrolytic polishing;
(4) and (4) cleaning and drying the magnesium alloy sample polished by the OPS in the step (3) to obtain a magnesium alloy EBSD sample.
Preferably, the mechanical grinding in step (1) is coarse grinding and then fine grinding, wherein the fine grinding needs to be carried out by using sand paper with a size of more than 2000 meshes.
Preferably, the electrolytic polishing solution in step (2) contains the following components per liter: 50-100mL of perchloric acid, and the balance of absolute ethyl alcohol, wherein the temperature of the electrolytic polishing solution is 0 ℃.
Preferably, the conditions of the electropolishing in step (2) are: the polishing voltage is 5-10V, and the polishing time is 8-15 s. If the voltage range is exceeded or the polishing time is too long, the alloy is easy to corrode; if the polishing time is too short or the voltage range is lower than the voltage range, the alloy stress layer cannot be effectively removed, and the calibration rate is influenced under the two conditions, so that the experimental result is influenced.
Preferably, the OPS polishing solution used for OPS polishing in the step (3) is a silica suspension with the volume fraction of 25-35%; the rotation speed of the polishing machine is 100-.
Preferably, the cleaning in the step (4) is carried out by ultrasonic cleaning with absolute ethyl alcohol.
The invention has the beneficial effects that:
(1) the method combines the electrolytic polishing and the OPS polishing, firstly uses the electrolytic polishing to carry out electrolytic erosion on the magnesium alloy sample as the anode, improves the micro-geometrical structure of the surface of the magnesium alloy, and reduces the micro-roughness of the metal surface, thereby ensuring that the surface of the magnesium alloy is smooth. And then removing the oxide layer on the surface of the magnesium alloy after electrolytic polishing by using OPS polishing, wherein the OPS polishing does not generate a stress layer while removing the oxide layer on the surface of the magnesium alloy, so that the surface of the magnesium alloy is bright, and a better calibration rate can be obtained.
(2) The electrolytic polishing solution prepared by the method has the advantages of low raw material price, simple preparation, short sample preparation time, high efficiency and high calibration rate.
Drawings
FIG. 1 is a pole drawing of an EBSD sample of an extruded Mg-1Al-0.3Ca-0.3Mn alloy in example 1 of the present invention;
FIG. 2 is a polar view of an EBSD sample of an extruded Mg-3Al-1Zn-1Ca alloy in example 2 of the present invention;
FIG. 3 is a pole figure of an EBSD sample of an extruded Mg-5Li-3Zn alloy in example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples, but is not limited thereto.
Example 1
In this example, the magnesium alloy sample is an extruded Mg-1Al-0.3Ca-0.3Mn alloy, and the specific steps for preparing the magnesium alloy EBSD sample are as follows:
(1) the surface of a magnesium alloy sample is roughly ground and then finely ground, wherein the fine grinding is carried out by adopting 2000 abrasive paper;
(2) preparing an electrolytic polishing solution according to 5% perchloric acid and 95% absolute ethyl alcohol by volume fraction;
(3) placing the prepared electrolytic polishing solution in a refrigerator and freezing to 0 ℃;
(4) connecting the magnesium alloy sample obtained in the step (1) as an anode, and taking a stainless steel plate as a cathode, and carrying out electrolytic polishing, wherein the polishing voltage is 10V, and the polishing electrolysis time is 10 s;
(5) after polishing electrolysis is finished, performing OPS polishing on the magnesium alloy sample subjected to polishing electrolysis in OPS polishing solution, wherein the polishing time is 5min, and the rotating speed of a polishing machine is 150 r/min;
wherein the OPS polishing solution is a silicon dioxide suspension with the volume fraction of 30%;
(6) and (3) placing the magnesium alloy sample after OPS polishing in absolute ethyl alcohol for ultrasonic cleaning until no polishing paste exists on the surface of the sample, and finally drying to obtain a magnesium alloy EBSD sample, namely a Mg-1Al-0.3Ca-0.3Mn alloy EBSD sample.
FIG. 1 is a polar diagram of an EBSD sample of the extruded Mg-1Al-0.3Ca-0.3Mn alloy of the present example, which has a calibration ratio of 88.9%.
Example 2
In this example, the magnesium alloy sample is an extruded Mg-3Al-1Zn-1Ca alloy, and the specific steps for preparing the magnesium alloy EBSD sample are as follows:
(1) the surface of a magnesium alloy sample is roughly ground and then finely ground, wherein the fine grinding is carried out by adopting 2000 abrasive paper;
(2) preparing an electrolytic polishing solution according to 10% perchloric acid and 90% absolute ethyl alcohol by volume fraction;
(3) placing the prepared electrolytic polishing solution in a refrigerator and freezing to 0 ℃;
(4) connecting the magnesium alloy sample obtained in the step (1) as an anode, and taking a stainless steel plate as a cathode, and carrying out electrolytic polishing, wherein the polishing voltage is 5V, and the polishing electrolysis time is 15 s;
(5) after polishing electrolysis is finished, performing OPS polishing on the magnesium alloy sample subjected to polishing electrolysis in OPS polishing solution, wherein the polishing time is 10min, and the rotating speed of a polishing machine is 150 r/min;
wherein the OPS polishing solution is a silica suspension with the volume fraction of 35%;
(6) and (3) placing the magnesium alloy sample after OPS polishing in absolute ethyl alcohol for ultrasonic cleaning until no polishing paste exists on the surface of the sample, and finally drying to obtain the magnesium alloy EBSD sample, namely the Mg-3Al-1Zn-1Ca alloy EBSD sample.
FIG. 2 is a polar diagram of EBSD of the extruded Mg-3Al-1Zn-1Ca alloy of this example, with a calibration rate of 85.2%.
Example 3
In this embodiment, the magnesium alloy sample is an extruded Mg-5Li-3Zn alloy, and the specific steps for preparing the magnesium alloy EBSD sample are as follows:
(1) the surface of a magnesium alloy sample is roughly ground and then finely ground, wherein the fine grinding is carried out by adopting 2000 abrasive paper;
(2) preparing an electrolytic polishing solution according to 5% perchloric acid and 95% absolute ethyl alcohol by volume fraction;
(3) placing the prepared electrolytic polishing solution in a refrigerator and freezing to 0 ℃;
(4) connecting the magnesium alloy sample obtained in the step (1) as an anode, and taking a stainless steel plate as a cathode, and carrying out electrolytic polishing, wherein the polishing voltage is 10V, and the polishing electrolysis time is 15 s;
(5) after polishing electrolysis is finished, performing OPS polishing on the magnesium alloy sample subjected to polishing electrolysis in OPS polishing solution, wherein the polishing time is 10min, and the rotating speed of a polishing machine is 200 r/min;
wherein the OPS polishing solution is a silica suspension with a volume fraction of 25%;
(6) and (3) placing the magnesium alloy sample after OPS polishing in absolute ethyl alcohol for ultrasonic cleaning until no polishing paste exists on the surface of the sample, and finally drying to obtain the magnesium alloy EBSD sample, namely the Mg-5Li-3Zn alloy EBSD sample.
FIG. 3 is a polar diagram of the EBSD of the Mg-5Li-3Zn alloy after extrusion in the present example, with a calibration ratio of 92.4%.
Comparative example 1
In this example, a magnesium alloy EBSD sample was also prepared from an extruded Mg-5Li-3Zn alloy sample, and the preparation method was substantially the same as in example 3, except that step (5) in example 3 was omitted, and the magnesium alloy sample after electropolishing was directly washed and dried. The calibration rate was found to be 75.2%.
Comparative example 2
In this example, a magnesium alloy EBSD sample was prepared from an extruded Mg-5Li-3Zn alloy sample by substantially the same method as in example 3 except that steps (2), (3) and (4) in example 3 were omitted. The calibration rate of the obtained magnesium alloy EBSD sample is 73.0 percent through testing.
Claims (6)
1. The preparation method of the magnesium alloy EBSD sample is characterized by comprising the following steps:
(1) mechanically polishing the surface of a magnesium alloy sample;
(2) preparing an electrolytic polishing solution, and performing electrolytic polishing on the magnesium alloy sample after mechanical polishing;
(3) carrying out OPS polishing on the magnesium alloy sample after electrolytic polishing;
(4) and (4) cleaning and drying the magnesium alloy sample polished by the OPS in the step (3) to obtain a magnesium alloy EBSD sample.
2. The method for preparing the magnesium alloy EBSD sample according to the claim 1, wherein the mechanical grinding in the step (1) is coarse grinding and then fine grinding, wherein the fine grinding needs to be carried out by using sand paper with a grain size of more than 2000 meshes.
3. The method for preparing the magnesium alloy EBSD sample according to the claim 1, wherein each liter of the electrolytic polishing solution in the step (2) comprises the following components in percentage by weight: 50-100mL of perchloric acid, and the balance of absolute ethyl alcohol, wherein the temperature of the electrolytic polishing solution is 0 ℃.
4. The method for preparing the magnesium alloy EBSD sample according to the claim 1, wherein the conditions of the electrolytic polishing in the step (2) are as follows: the polishing voltage is 5-10V, and the polishing time is 8-15 s.
5. The method for preparing the magnesium alloy EBSD sample according to the claim 1, wherein the OPS polishing solution used for OPS polishing in the step (3) is a silica suspension with the volume fraction of 25-35%; the rotation speed of the polishing machine is 100-.
6. The method for preparing the magnesium alloy EBSD sample according to the claim 1, wherein the cleaning in the step (4) is carried out by ultrasonic cleaning with absolute ethyl alcohol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113670962A (en) * | 2021-08-23 | 2021-11-19 | 河海大学 | Method for preparing high-calibration-rate pure magnesium EBSD sample at room temperature |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102383176A (en) * | 2010-09-03 | 2012-03-21 | 中国科学院金属研究所 | Preparation method of magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof |
| US20170074755A1 (en) * | 2012-11-13 | 2017-03-16 | Ues, Inc. | Automated high speed metallographic system |
| CN107541768A (en) * | 2017-08-30 | 2018-01-05 | 北京科技大学 | A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples |
| CN108106913A (en) * | 2017-11-20 | 2018-06-01 | 东北大学 | A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN109855931A (en) * | 2018-12-20 | 2019-06-07 | 河钢股份有限公司 | A kind of preparation method of austenitic alloy EBSD sample |
| WO2019174151A1 (en) * | 2018-03-13 | 2019-09-19 | 西南石油大学 | Hot-bending x90 structure and performance evaluation method |
-
2019
- 2019-10-17 CN CN201910988922.0A patent/CN110618149A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102383176A (en) * | 2010-09-03 | 2012-03-21 | 中国科学院金属研究所 | Preparation method of magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof |
| US20170074755A1 (en) * | 2012-11-13 | 2017-03-16 | Ues, Inc. | Automated high speed metallographic system |
| CN107541768A (en) * | 2017-08-30 | 2018-01-05 | 北京科技大学 | A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples |
| CN108106913A (en) * | 2017-11-20 | 2018-06-01 | 东北大学 | A kind of method of Al-Si alloys OPS polishing sample preparations for EBSD tests |
| WO2019174151A1 (en) * | 2018-03-13 | 2019-09-19 | 西南石油大学 | Hot-bending x90 structure and performance evaluation method |
| CN109855931A (en) * | 2018-12-20 | 2019-06-07 | 河钢股份有限公司 | A kind of preparation method of austenitic alloy EBSD sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
Non-Patent Citations (2)
| Title |
|---|
| CHEN, YJ: "Microstructure evolution in magnesium alloy AZ31 during cyclic extrusion compression", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 宋广胜: "AZ31镁合金棒材循环扭转变形及其对力学性能的影响", 《材料工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113670962A (en) * | 2021-08-23 | 2021-11-19 | 河海大学 | Method for preparing high-calibration-rate pure magnesium EBSD sample at room temperature |
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Application publication date: 20191227 |