CN111537318A - Metallographic phase display method of copper-gallium alloy - Google Patents
Metallographic phase display method of copper-gallium alloy Download PDFInfo
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- CN111537318A CN111537318A CN202010240403.9A CN202010240403A CN111537318A CN 111537318 A CN111537318 A CN 111537318A CN 202010240403 A CN202010240403 A CN 202010240403A CN 111537318 A CN111537318 A CN 111537318A
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- 229910000807 Ga alloy Inorganic materials 0.000 title claims abstract description 103
- CDZGJSREWGPJMG-UHFFFAOYSA-N copper gallium Chemical compound [Cu].[Ga] CDZGJSREWGPJMG-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 57
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003518 caustics Substances 0.000 claims abstract description 33
- 230000007797 corrosion Effects 0.000 claims abstract description 27
- 238000005260 corrosion Methods 0.000 claims abstract description 27
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000007664 blowing Methods 0.000 claims abstract description 5
- 238000011010 flushing procedure Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims description 69
- 238000005498 polishing Methods 0.000 claims description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000010432 diamond Substances 0.000 claims description 7
- 238000007517 polishing process Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052733 gallium Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 16
- 229910010271 silicon carbide Inorganic materials 0.000 description 16
- 239000000080 wetting agent Substances 0.000 description 9
- 239000004744 fabric Substances 0.000 description 8
- 238000005507 spraying Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material 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)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a metallographic display method of a copper-gallium alloy, which comprises the following steps: immersing the polished copper-gallium alloy sample into a metallographic corrosive agent for corrosion, flushing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the sample by blowing, and observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, wherein the metallographic corrosive agent is a mixed solution prepared by adopting alkali metal hydroxide, ammonia water and hydrogen peroxide according to a certain proportion. According to the metallographic display method of the copper-gallium alloy, provided by the invention, the mixed solution prepared from the alkali metal hydroxide, the ammonia water and the hydrogen peroxide according to a certain proportion is used as the metallographic corrosive agent, so that the technical problems that the prior art is complex in process, the corrosive agent is high in risk and the display effect cannot be guaranteed can be effectively solved.
Description
Technical Field
The invention relates to the technical field of preparation of metallographic copper-gallium alloy samples, in particular to a metallographic display method of copper-gallium alloy.
Background
The Copper Indium Gallium Selenide (CIGS) thin-film solar cell has the advantages of low preparation cost, high photoelectric conversion efficiency and good device stability, and is one of the novel solar cells with the most application prospect. At present, the preparation method of the CIGS thin-film solar cell is mainly a magnetron sputtering method, and the CIG precursor thin film is mostly formed by sputtering a copper-gallium alloy target and an indium (or copper-indium) target in the process, and then selenization treatment is carried out. The parameters of the target material such as grain size, grain orientation and the like have very important influence on the physical property, the mechanical property, the photoelectric property and the like of the CIGS thin film. In order to obtain a CIGS thin film with high performance, it is important to characterize and control the grain size and grain orientation of the sputtering target.
The internal structure of the metal material is directly and closely related to the material properties such as hardness, strength, ductility and the like, and metallographic observation is the most direct and effective method for researching the internal structure of the metal material. The metallographic phase refers to chemical components of metal or alloy and physical and chemical states of various components in the metal or alloy, and the metallographic phase display is a common technology for observing the internal structure of the metal and the alloy thereof, and the basic principle is that different structure phases are displayed by utilizing the difference of corrosion resistance of phases in the metal and corrosion resistance of crystal grains and grain boundaries to the same corrosion solution. The characterization technology has the characteristics of simplicity and feasibility, and is widely applied to material science research.
In the metallographic sample preparation process, if the grinding and polishing process and the corrosive agent are not properly selected, clear and obvious metallographic structure pictures cannot be obtained, at present, the existing metallographic corrosive agent for metals generally adopts a strong acid salt solution, although the scheme of adopting the strong acid salt solution can obtain clear metallographic structure pictures for metals, the process is complex and pollutes the environment, as the scheme adopting the strong acid salt solution has the defects of high oxidizability, high corrosivity, high volatility, high safety risk to operators and the like, the industry begins to use the alkaline solution scheme with low corrosive risk as the metallic phase corrosive, however, the display effect is always unsatisfactory by using the conventional alkaline solution scheme as a metallographic corrosive agent for metals, therefore, a metallographic corrosive agent which has relatively simple process, low corrosive agent risk and ideal display effect is urgently needed in the industry.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a metallographic display method of a copper-gallium alloy.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a metallographic display method of a copper-gallium alloy, which comprises the following steps: immersing the polished copper-gallium alloy sample into a metallographic corrosive agent for corrosion, flushing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the sample by blowing, and observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, wherein the metallographic corrosive agent is a mixed solution prepared by adopting alkali metal hydroxide, ammonia water and hydrogen peroxide according to a certain proportion.
As a further improvement of the invention, the ratio of the alkali metal hydroxide, the ammonia water and the hydrogen peroxide in the metallographic corrosive agent is 1g to 20mL to 50 mL.
As a further improvement of the invention, before polishing the copper-gallium alloy test sample, the method also comprises the following steps: preparing a copper-gallium alloy test sample, and carrying out three links of coarse grinding, fine grinding and polishing on the copper-gallium alloy test sample for treatment.
As a further improvement of the invention, the alkali metal hydroxide is potassium hydroxide or sodium hydroxide.
As a further improvement of the invention, the duration of the corrosion is 20 s-300 s.
As a further improvement of the invention, the abrasive paper is used as water-based abrasive paper with the mesh number of 320-800 # in the coarse grinding process, and the rotating speed in the coarse grinding process is 200-800 r/min.
As a further improvement of the invention, the abrasive paper is water-based abrasive paper with the mesh number of 1000-2000 # in the fine grinding process, and the rotating speed in the fine grinding process is 300-800 r/min.
As a further improvement of the invention, the polishing agent used in the polishing process is a diamond polishing agent.
As a further improvement of the invention, the purity of copper in the prepared copper-gallium alloy sample is not lower than 4N, and the purity of gallium is not lower than 4N.
As a further improvement of the invention, the copper-gallium alloy sample is provided with copper composed of the following raw materials in percentage by weight: 50.0% -75.0%; gallium: 25.0% -50.0%.
According to the metallographic display method of the copper-gallium alloy, provided by the invention, the mixed solution prepared from the alkali metal hydroxide, the ammonia water and the hydrogen peroxide according to a certain proportion is used as the metallographic corrosive agent, so that the technical problems that the prior art is complex in process, the corrosive agent is high in risk and the display effect cannot be guaranteed can be effectively solved.
Drawings
FIG. 1 is a metallographic structure image of a copper-gallium alloy sample obtained in example 1 of the present invention.
FIG. 2 is a metallographic structure image of a Cu-Ga alloy sample obtained in comparative example 1 of the present invention.
FIG. 3 is a metallographic structure image of a Cu-Ga alloy sample obtained in comparative example 2 of the present invention.
FIG. 4 is a metallographic structure image of a Cu-Ga alloy sample obtained in comparative example 3 of the present invention.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a metallographic display method of a copper-gallium alloy, which comprises the following steps:
and preparing a copper-gallium alloy sample.
In this embodiment, the purity of copper in the prepared copper-gallium alloy sample is not lower than 4N, the purity of gallium is not lower than 4N, and the copper in the copper-gallium alloy sample is composed of the following raw materials by weight percent: 50.0% -75.0%; gallium: 25.0% -50.0%.
And carrying out coarse grinding on the copper-gallium alloy test sample.
In the embodiment, coarse silicon carbide water-based abrasive paper and mechanical polishing equipment are adopted to perform coarse grinding on the copper-gallium alloy sample, the mesh number of the coarse silicon carbide abrasive paper adopted in the coarse grinding process is 320# to 800# water-based abrasive paper, the rotating speed in the coarse grinding process is 200 r/min to 800 r/min, in the coarse grinding process, the mesh number of the abrasive paper is changed every time, the grinding surface of the copper-gallium alloy sample is rotated by 90 degrees until the surface of the copper-gallium alloy sample is smooth and the scratch direction is consistent, and the copper-gallium alloy sample is cleaned after the coarse grinding is completed.
And (4) carrying out accurate grinding on the copper-gallium alloy test sample after the coarse grinding.
In the embodiment, fine silicon carbide water-based abrasive paper and mechanical polishing equipment are adopted to accurately polish the copper-gallium alloy sample, the mesh number of coarse silicon carbide abrasive paper adopted in the accurate grinding process is 1000# -2000 # water-based abrasive paper, the rotating speed in the coarse grinding process is 300 r/min-800 r/min, in the accurate grinding process, the mesh number of the abrasive paper is changed every time, the grinding surface of the copper-gallium alloy sample is rotated by 90 degrees until the surface of the copper-gallium alloy sample is smooth and has no obvious coarse scratch, and the copper-gallium alloy sample is cleaned after the accurate grinding is finished.
And polishing the finely ground copper-gallium alloy sample.
In the embodiment, a diamond polishing agent and a mechanical polishing device are used for polishing the copper-gallium alloy sample, the particle size of powder of the polishing agent is 0.25-3 mu m, the polishing speed is 200-600 r/min, wetting agents used in the processes of coarse grinding, fine grinding and polishing are all water, and the copper-gallium alloy sample is cleaned after polishing.
Immersing the polished copper-gallium alloy sample into a metallographic corrosive agent for corrosion, flushing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the sample by blowing, and observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, wherein the metallographic corrosive agent is a mixed solution prepared by adopting alkali metal hydroxide, ammonia water and hydrogen peroxide according to a certain proportion.
In the embodiment, the metallographic corrosive agent is a mixed solution prepared by alkali metal hydroxide, ammonia water and hydrogen peroxide according to a certain proportion, the proportion of the alkali metal hydroxide, the ammonia water and the hydrogen peroxide in the metallographic corrosive agent is 1g:20mL:50mL, the corrosive agent is dipped by a cotton swab and wiped on the surface of the copper-gallium alloy sample for corrosion, the duration of the corrosion is 20 s-300 s, and after the corrosion is finished, the surface of the copper-gallium alloy sample is washed by ultrapure water and dried.
For further understanding of the present invention, the method and effects of the present invention will be described in further detail with reference to specific examples. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1.
The embodiment provides a metallographic corrosive agent which adopts alkali metal hydroxide, 25% concentration ammonia water and 30% concentration hydrogen peroxide in a ratio of 1g to 20mL to 50mL, and comprises the following steps:
(1) coarse grinding: in the coarse grinding process, water is used as a wetting agent, 320# SiC water-based abrasive paper is installed on a metallographic polishing machine, the surface of a copper-gallium alloy sample is polished at the rotating speed of 600 r/min for 5 min until the whole surface is bright, then the 600# SiC water-based abrasive paper is replaced, the copper-gallium alloy sample is rotated by 90 degrees and is continuously polished at the rotating speed of 500 r/min for 3 min until the surface is flat and the scratch direction is consistent, and the copper-gallium alloy sample is cleaned after the coarse grinding is finished.
(2) Fine grinding: and in the fine grinding process, water is used as a wetting agent, the copper-gallium alloy test sample after the coarse grinding is rotated by 90 degrees, fine grinding is carried out by using 2000# SiC water-based abrasive paper, the rotating speed is 350 r/min, the grinding duration is 5 min, the copper-gallium alloy test sample is ground until the surface is flat and has no obvious coarse scratch, and the copper-gallium alloy test sample is cleaned after the fine grinding is finished.
(3) Polishing: wetting the polishing cloth by water, spraying a layer of diamond polishing agent on the polishing cloth, rotating the copper-gallium alloy sample after finishing fine grinding by 90 degrees, polishing at the rotating speed of 400 r/min, and dripping water and spraying the polishing agent uninterruptedly. And (4) the polishing process takes about 8 min, and after the polishing is finished, the copper-gallium alloy sample is sequentially cleaned and dried by using absolute ethyl alcohol and ultrapure water.
(4) And (3) corrosion: the method comprises the steps of taking alkali metal hydroxide, ammonia water with the concentration of 25% and hydrogen peroxide with the concentration of 30% as a metallographic corrosive agent according to the proportion of 1g to 20mL to 50mL, stirring the metallographic corrosive agent uniformly, dipping a medical cotton swab in corrosive liquid to wipe the surface of a copper-gallium alloy sample for corrosion for 50 s, washing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the sample by blowing, observing the surface of the corroded copper-gallium alloy sample with a metallographic microscope to obtain a metallographic structure image, wherein the result is shown in figure 1, the grain boundary contour of each part of the surface of the whole image is clear, and the difference between each phase is obvious.
Comparative example 1.
This example provides the use of water, 30% strength hydrogen peroxide and 28% strength ammonia in a ratio of 4:3:6 as the metallographic etchant, comprising the steps of:
(1) coarse grinding: in the coarse grinding process, water is used as a wetting agent, 320# SiC water-based abrasive paper is installed on a metallographic polishing machine, the surface of a copper-gallium alloy sample is polished at the rotating speed of 600 r/min for 5 min until the whole surface is bright, then the 600# SiC water-based abrasive paper is replaced, the copper-gallium alloy sample is rotated by 90 degrees and is continuously polished at the rotating speed of 500 r/min for 3 min until the surface is flat and the scratch direction is consistent, and the copper-gallium alloy sample is cleaned after the coarse grinding is finished.
(2) Fine grinding: and in the fine grinding process, water is used as a wetting agent, the copper-gallium alloy test sample after the coarse grinding is rotated by 90 degrees, fine grinding is carried out by using 2000# SiC water-based abrasive paper, the rotating speed is 350 r/min, the grinding duration is 5 min, the copper-gallium alloy test sample is ground until the surface is flat and has no obvious coarse scratch, and the copper-gallium alloy test sample is cleaned after the fine grinding is finished.
(3) Polishing: wetting the polishing cloth by water, spraying a layer of diamond polishing agent on the polishing cloth, rotating the copper-gallium alloy sample after finishing fine grinding by 90 degrees, polishing at the rotating speed of 400 r/min, and dripping water and spraying the polishing agent uninterruptedly. And (4) the polishing process takes about 8 min, and after the polishing is finished, the copper-gallium alloy sample is sequentially cleaned and dried by using absolute ethyl alcohol and ultrapure water.
(4) And (3) corrosion: the method comprises the steps of taking water, 30% of hydrogen peroxide and 28% of ammonia water in a ratio of 4:3:6 as a metallographic corrosive agent, stirring the metallographic corrosive agent uniformly, dipping a medical cotton swab in corrosive liquid to wipe the surface of a copper-gallium alloy sample for corrosion for 50 s, flushing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, blow-drying, observing the surface of the corroded copper-gallium alloy sample with a metallographic microscope to obtain a metallographic structure image, wherein the result is shown in figure 2, the grain boundary contours of a plurality of places on the surface are not completely shown, and the grain surface color of part of the places is black.
Comparative example 2.
The embodiment provides a metallographic corrosive agent which adopts potassium hydroxide and 30% hydrogen peroxide in a ratio of 1g to 50ml, and comprises the following steps:
(1) coarse grinding: in the coarse grinding process, water is used as a wetting agent, 400# SiC water-based abrasive paper is installed on a metallographic polishing machine, the surface of a copper-gallium alloy sample is polished at the rotating speed of 500 r/min, the polishing duration is 5 min, the whole surface is polished to be bright, then the 800# SiC water-based abrasive paper is replaced, the copper-gallium alloy sample is rotated by 90 degrees, the polishing is continued at the rotating speed of 500 r/min, the polishing duration is 3 min, the surface is polished to be flat, the scratch direction is consistent, and the copper-gallium alloy sample is cleaned after the coarse grinding is finished.
(2) Fine grinding: and in the fine grinding process, water is used as a wetting agent, the copper-gallium alloy test sample after the coarse grinding is rotated by 90 degrees, fine grinding is carried out by 1500# SiC water-based abrasive paper, the rotating speed is 400 r/min, the grinding duration is 5 min, the copper-gallium alloy test sample is ground until the surface is flat and has no obvious coarse scratch, and the copper-gallium alloy test sample is cleaned after the fine grinding is finished.
(3) Polishing: wetting polishing cloth by water, spraying a layer of diamond polishing agent on the polishing cloth, rotating the copper-gallium alloy sample after finishing fine grinding by 90 degrees, polishing at the rotating speed of 350 r/min, and dripping water and spraying the polishing agent uninterruptedly. And (4) the polishing process takes about 8 min, and after the polishing is finished, the copper-gallium alloy sample is sequentially cleaned and dried by using absolute ethyl alcohol and ultrapure water.
(4) And (3) corrosion: the method comprises the steps of taking potassium hydroxide and 30% hydrogen peroxide in a ratio of 1g to 50ml as metallographic corrosive agents, stirring the metallographic corrosive agents uniformly, dipping medical cotton swabs in corrosive liquid to wipe the surface of a copper-gallium alloy sample for corrosion for 50 s, washing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the surface of the copper-gallium alloy sample, observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, and obtaining a result shown in figure 3, wherein the surface is uneven in color, and the whole surface can only be subjected to phase separation, but an obvious grain boundary profile cannot be seen.
Comparative example 3.
This example provides the use of potassium hydroxide and 25% strength ammonia in a ratio of 1g to 20ml as a metallographic etchant comprising the steps of:
(1) coarse grinding: in the coarse grinding process, water is used as a wetting agent, 320# SiC water-based abrasive paper is installed on a metallographic polishing machine, the surface of a copper-gallium alloy sample is polished at the rotating speed of 400 r/min for 5 min until the whole surface is bright, then 800# SiC water-based abrasive paper is replaced, the copper-gallium alloy sample is rotated by 90 degrees and is continuously polished at the rotating speed of 450 r/min for 3 min until the surface is flat and the scratch direction is consistent, and the copper-gallium alloy sample is cleaned after the coarse grinding is finished.
(2) Fine grinding: and in the fine grinding process, water is used as a wetting agent, the copper-gallium alloy test sample after the coarse grinding is rotated by 90 degrees, fine grinding is carried out by using 2000# SiC water-based sand paper, the rotating speed is 400 r/min, the grinding duration is 5 min, the copper-gallium alloy test sample is ground until the surface is flat and has no obvious coarse scratch, and the copper-gallium alloy test sample is cleaned after the fine grinding is finished.
(3) Polishing: wetting the polishing cloth by water, spraying a layer of diamond polishing agent on the polishing cloth, rotating the copper-gallium alloy sample after finishing fine grinding by 90 degrees, polishing at the rotating speed of 400 r/min, and dripping water and spraying the polishing agent uninterruptedly. And (4) the polishing process takes about 8 min, and after the polishing is finished, the copper-gallium alloy sample is sequentially cleaned and dried by using absolute ethyl alcohol and ultrapure water.
(4) And (3) corrosion: the method comprises the steps of taking potassium hydroxide and 25% ammonia water in a ratio of 1g to 20ml as metallographic corrosive agents, stirring the metallographic corrosive agents uniformly, dipping medical cotton swabs in corrosive liquid to wipe the surface of a copper-gallium alloy sample for corrosion for 50 s, washing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the surface of the copper-gallium alloy sample, observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, and obtaining a result shown in figure 4, wherein the surface can only be subjected to phase separation, and obvious grain boundary contours cannot be seen.
According to the metallographic display method of the copper-gallium alloy, provided by the invention, the mixed solution prepared from the alkali metal hydroxide, the ammonia water and the hydrogen peroxide according to a certain proportion is used as the metallographic corrosive agent, so that the technical problems that the prior art is complex in process, the corrosive agent is high in risk and the display effect cannot be guaranteed can be effectively solved.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (10)
1. A metallographic display method of a copper-gallium alloy is characterized by comprising the following steps:
immersing the polished copper-gallium alloy sample into a metallographic corrosive agent for corrosion, flushing the surface of the copper-gallium alloy sample with ultrapure water after the corrosion is finished, drying the sample by blowing, and observing the surface of the corroded copper-gallium alloy sample by using a metallographic microscope to obtain a metallographic structure image, wherein the metallographic corrosive agent is a mixed solution prepared by adopting alkali metal hydroxide, ammonia water and hydrogen peroxide according to a certain proportion.
2. The method of claim 1, wherein the ratio of alkali metal hydroxide, ammonia water and hydrogen peroxide in the metallographic etchant is 1g:20mL:50 mL.
3. The method of claim 1, wherein prior to polishing the copper gallium alloy coupon, further comprising the steps of:
preparing a copper-gallium alloy test sample, and carrying out three links of coarse grinding, fine grinding and polishing on the copper-gallium alloy test sample for treatment.
4. The method of claim 1, wherein the alkali metal hydroxide is potassium hydroxide or sodium hydroxide.
5. The method of claim 1, wherein the duration of the etching is 20 s to 300 s.
6. The method as claimed in claim 3, wherein the coarse grinding process uses water-based sand paper with a mesh size of 320-800 #, and the rotation speed during the coarse grinding process is 200-800 r/min.
7. The method according to claim 3, wherein the abrasive paper used in the fine grinding process is water-based abrasive paper with a mesh number of 1000-2000 #, and the rotation speed in the fine grinding process is 300-800 r/min.
8. The method of claim 3, wherein the polishing agent used in the polishing process is a diamond polishing agent.
9. The method according to claim 3, wherein the purity of copper in the prepared copper-gallium alloy sample is not lower than 4N, and the purity of gallium is not lower than 4N.
10. The method according to claim 3, wherein the copper in the prepared copper-gallium alloy test sample is composed of the following raw materials in percentage by weight: 50.0% -75.0%; gallium: 25.0% -50.0%.
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