CN115537904A - Method for obtaining metallographic structure of aluminum alloy by utilizing two-stage electrolyte electrolysis - Google Patents
Method for obtaining metallographic structure of aluminum alloy by utilizing two-stage electrolyte electrolysis Download PDFInfo
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- CN115537904A CN115537904A CN202211155377.5A CN202211155377A CN115537904A CN 115537904 A CN115537904 A CN 115537904A CN 202211155377 A CN202211155377 A CN 202211155377A CN 115537904 A CN115537904 A CN 115537904A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 66
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 47
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 13
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005498 polishing Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000005260 corrosion Methods 0.000 claims description 7
- 230000007797 corrosion Effects 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910000881 Cu alloy Inorganic materials 0.000 claims 1
- 229910000676 Si alloy Inorganic materials 0.000 claims 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims 1
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001887 electron backscatter diffraction Methods 0.000 abstract 1
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010587 phase diagram Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 206010027146 Melanoderma Diseases 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/18—Polishing of light metals
- C25F3/20—Polishing of light metals of aluminium
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
Abstract
The invention relates to a method for polishing and corroding aluminum alloy by using a two-stage electrolyte, which aims at aluminum alloy with a metallographic structure, such as wrought aluminum alloy and heat-treated aluminum alloy, which is difficult to obtain by using a common treatment method. The proportion of the two-stage electrolyte is as follows: first-stage: perchloric acid 20% -25% methanol 75% -80%, second stage: 10-15% of perchloric acid and 85-90% of ethanol alcohol. According to the invention, the pretreated aluminum alloy is electrolyzed, and the pretreated aluminum alloy is sequentially put into the secondary electrolyte for electrolysis, so that a metallographic phase suitable for observation through OM is obtained. Each electrolyte can be used independently, and the electrolyte of the first grade can be used for removing larger scratches on the surface of the aluminum alloy so as to make the surface smoother. The second stage electrolyte may be used for the electrolyte of a general as-cast aluminum alloy, and the aluminum alloy treated with the second stage electrolyte may be used for an EBSD pattern.
Description
Technical Field
Novel proportion of aluminum alloy electrolyte and method for obtaining metallographic structure through electrolysis
Background
The aluminum alloy has the characteristics of high specific strength and high cost performance, is widely applied to various fields, and is not poor in the application of high-tech fields such as aviation, aerospace, military and the like. The method has great influence on the production and life of people, so the research on the aluminum alloy becomes abnormal and important, in the daily research on the aluminum alloy, the microstructure of the aluminum alloy is observed, the polishing corrosion treatment is required to be carried out on the surface of the aluminum alloy, and the electrolytic polishing corrosion is a better mode and has the advantages of simplicity, rapidness and outstanding effect. However, some aluminum alloys tend to have grain boundaries that become fine due to deformation or heat treatment, making it difficult to etch out the crystal phase. And the proper proportion of the electrolyte and the corrosion method are helpful for corroding a crystal phase structure suitable for observation.
Disclosure of Invention
The invention relates to a method for performing electrolytic polishing corrosion on aluminum alloy which is particularly difficult to polish and corrode by using a two-stage electrolyte and obtaining a metallographic structure.
The first-stage electrolyte is prepared from perchloric acid 20-25% methanol 75-80% and voltage 20-25v. The method has the effects of removing scratches still existing after the surface of the aluminum alloy is polished, enabling the surface to be brighter and smoother and creating conditions for subsequent further electrolytic corrosion.
The secondary electrolysis proportion is 10 percent of perchloric acid and 90 percent of methanol, and the voltage is 20-25v. The function of the aluminum alloy is equivalent to that of corrosive liquid, so that the surface of the aluminum alloy can show the appearance of a metallographic phase, and the metallographic structure can be observed better.
The step-by-step polishing corrosion by using the electrolyte needs to be carried out by rotating and stirring a rotor so as to bring bubbles on the surface of the aluminum alloy away and reduce black spots and air holes on the surface. The rotating speed in the first-stage electrolyte is 4-5r/s, and the rotating speed in the second-stage electrolyte is 3r/s.
The electrolyte occupies 2/3-3/4 of the container, and a beaker with the capacity of 500ml is used as the container of the electrolyte, so that the rotor can fully exert the effect.
The lead block size is 50mm multiplied by 50mm, and the electrolyte is 1/2 of the lead block.
The current can reach 1.5A in the first-stage electrolyte and 0.2A in the second-stage electrolyte, and both can be carried out at room temperature.
The electrolysis time in the first-stage electrolyte is 5-20s, and the electrolysis time in the second-stage electrolyte is 10-15s.
The electrolyte does not contain nitric acid, and is beneficial to environmental protection.
The electrolyte is stored in a dark environment.
The primary and secondary electrolyte can be used for multiple purposes, each electrolyte can be used independently, and the primary electrolyte can be used for removing large scratches on the surface of the aluminum alloy so that the surface is smoother. The secondary electrolyte can be used as an electrolytic polishing corrosive liquid for easily corroding aluminum alloy with a metallographic phase, and the electrolyzed aluminum alloy can be used as an EBSD (Electron Back scattered diffraction) pattern.
Drawings
FIG. 1 is a schematic view of aluminum alloy electrolysis
FIG. 2 is a phase diagram of an aluminum alloy electrolyzed using the two-stage aluminum alloy electropolishing solution of example 1.
FIG. 3 is a phase diagram of an aluminum alloy electrolyzed using the two-stage aluminum alloy electropolishing solution of example 2.
FIG. 4 is a phase diagram of an aluminum alloy subjected to electrolytic polishing using the aluminum alloy electrolytic polishing liquid of example 7.
Detailed Description
My invention is next illustrated by several specific examples.
Example 1
The example adopts two-stage electrolyte mixture ratio as follows: primary electrolyte perchloric acid 20% methanol 80%; the secondary electrolyte perchloric acid is 10% and ethanol is 90%.
And (3) connecting the pre-ground aluminum alloy (which is ground to 2000 meshes by using sand paper and then polished to be bright in surface) into an anode, wherein a cathode is a lead block.
The beaker with the rotor is placed on a magnetic stirring device, the voltage is adjusted to 25v, the rotating speed is 4r/s, and then the magnetic stirring device is started. Putting lead blocks and aluminum alloy into primary electrolyte for electrolysis for 10s, taking out, washing the surface with alcohol, soaking in alcohol for 1min, clamping with forceps, blowing the surface with a blower, observing on an optical microscope, and repeating the above operations until no scratch, black spot or bubble is generated on the surface.
The aluminum alloy treated by the primary electrolyte is soaked in the secondary electrolyte for 5s in the same way, the rotating speed of the rotor is 3r/s at the voltage of 25v, and the electrolysis time is 15s.
Example 2
The process was essentially the same as the electrolyte formulation and operation of example 1, except that the electrolysis time in the primary electrolyte was changed to 15 seconds.
Example 3
The process was essentially the same as the formulation and operation of the electrolyte of example 1, except that the electrolysis time in the secondary electrolyte was changed to 10 seconds.
Example 4
The electrolyte is prepared by the following steps: the same procedure as in example 1 was repeated except that 80% of methanol was used as the primary electrolyte and 85% of ethanol was used as the secondary electrolyte, respectively, as perchloric acid and 15% of ethanol were used.
Example 5
The proportion of the electrolyte is the same as that of example 4, the electrolyte is electrolyzed in the primary electrolyte for 15s, the rotating speed of the rotor is 4r/s, the voltage is 20V, and the electrolyte is electrolyzed in the secondary electrolyte for 5s, the rotating speed of the rotor is 3r/s, and the voltage is 25V. The other operations were the same as in example 1.
Example 6
The electrolysis is carried out for 10s in the secondary electrolyte, and the other operations and the proportion of the electrolyte are the same as those of the example 5.
Example 7
Preparing electrolyte perchloric acid 20% methanol 80%, and performing rotor rotation speed 4r/s, voltage 25v, current 1.5A and room temperature.
Example 8
The electrolyte is prepared by 90 percent of perchloric acid 10 percent ethanol, the rotor rotating speed is 3r/s, the voltage is 25v, the current can reach 0.2A-0.4A, and the temperature is room temperature.
And electrolyzing the aluminum alloy with a smooth and easily corroded surface after mechanical polishing for 10s.
The experiments show that the two-stage electrolyte is very suitable for aluminum alloys (various deformed aluminum alloys and heat-treated aluminum alloys) which are difficult to corrode crystal boundaries, and the electrolyte of each stage can be used independently to achieve different effects.
Claims (3)
1. An aluminum alloy electrolyte is characterized by being a two-stage electrolyte. And each electrolyte can be independently used to exert different effects, the primary electrolyte can remove deep scratches on the surface of the pretreated aluminum alloy, and the secondary electrolyte can be used as an electrolytic polishing solution for common cast aluminum alloys.
2. The formula is as follows: first-stage: perchloric acid 20-25% and methanol 75-80%; and (2) second stage: 10-15% of perchloric acid and 85-90% of ethanol. The surface of the aluminum alloy is pretreated before electrolysis (sand paper is ground to 2000 meshes, and then mechanical polishing is carried out until the surface presents a mirror surface). The area of the aluminum alloy polished surface is 16mm2-40mm2. The method is mainly used for metallographic corrosion of the aluminum-copper alloy and the aluminum-silicon alloy in the deformation state and the heat treatment state. Connecting an aluminum alloy with a positive electrode, connecting a negative electrode with a lead block, placing electrolyte put into a rotor on a magnetic stirrer, opening the magnetic stirrer to rotate the rotor so as to fully eliminate a large number of bubbles on the surface of the aluminum alloy, wherein the voltage in the first-stage electrolyte is 20-25v, the electrolysis time is 10-20s, immediately washing the rotor with alcohol after taking out, drying the washed bubbles after 1-2 minutes in the alcohol by using a blower, observing whether bubbles or black spots exist on the surface, continuously carrying out electrolysis if bubbles and black spots exist until the surface is bright and no bubbles exist, and then carrying out second-stage electrolysis, wherein the voltage in the second-stage electrolyte is 20-25v, and the electrolysis time is 5-15s.
3. According to the patent claim 2, the rotor speed in the primary electrolyte is 4-5r/s, the rotor speed in the secondary electrolyte is 3-4r/s, and the requirement for the electrolyte is that the shelf life is one month (or when the solution becomes red), and the electrolyte should be re-proportioned after the solution becomes red.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211155377.5A CN115537904A (en) | 2022-09-22 | 2022-09-22 | Method for obtaining metallographic structure of aluminum alloy by utilizing two-stage electrolyte electrolysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211155377.5A CN115537904A (en) | 2022-09-22 | 2022-09-22 | Method for obtaining metallographic structure of aluminum alloy by utilizing two-stage electrolyte electrolysis |
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| CN202211155377.5A Pending CN115537904A (en) | 2022-09-22 | 2022-09-22 | Method for obtaining metallographic structure of aluminum alloy by utilizing two-stage electrolyte electrolysis |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128759A (en) * | 1992-10-13 | 1994-05-10 | Nippon Steel Corp | Corrosive liquid revealing metallic structure of aluminum alloy and revealing method |
| CN107462456A (en) * | 2016-06-03 | 2017-12-12 | 宁波江丰电子材料股份有限公司 | Method for displaying metallographic structure |
| CN110208264A (en) * | 2019-06-17 | 2019-09-06 | 新疆众和股份有限公司 | A kind of method for making sample of high-purity aluminium busbar metallographic sample |
| CN110835778A (en) * | 2019-11-21 | 2020-02-25 | 哈尔滨工业大学 | Aluminum alloy electrolytic polishing solution and electrolytic polishing method |
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2022
- 2022-09-22 CN CN202211155377.5A patent/CN115537904A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06128759A (en) * | 1992-10-13 | 1994-05-10 | Nippon Steel Corp | Corrosive liquid revealing metallic structure of aluminum alloy and revealing method |
| CN107462456A (en) * | 2016-06-03 | 2017-12-12 | 宁波江丰电子材料股份有限公司 | Method for displaying metallographic structure |
| CN110208264A (en) * | 2019-06-17 | 2019-09-06 | 新疆众和股份有限公司 | A kind of method for making sample of high-purity aluminium busbar metallographic sample |
| CN110835778A (en) * | 2019-11-21 | 2020-02-25 | 哈尔滨工业大学 | Aluminum alloy electrolytic polishing solution and electrolytic polishing method |
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