CN117447999A - Metallographic etching liquid for gallium arsenide polycrystal and metallographic etching method thereof - Google Patents
Metallographic etching liquid for gallium arsenide polycrystal and metallographic etching method thereof Download PDFInfo
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- CN117447999A CN117447999A CN202311441242.XA CN202311441242A CN117447999A CN 117447999 A CN117447999 A CN 117447999A CN 202311441242 A CN202311441242 A CN 202311441242A CN 117447999 A CN117447999 A CN 117447999A
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- metallographic
- water
- gallium arsenide
- hydrogen peroxide
- metallographic etching
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- 238000005530 etching Methods 0.000 title claims abstract description 61
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910001218 Gallium arsenide Inorganic materials 0.000 title claims abstract description 42
- 239000007788 liquid Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 32
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 32
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 abstract description 18
- 239000013078 crystal Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 description 13
- 230000007797 corrosion Effects 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 9
- 238000010587 phase diagram Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000003822 epoxy resin Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (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)
- ing And Chemical Polishing (AREA)
Abstract
The invention relates to the field of semiconductor materials, in particular to a metallographic etching solution for gallium arsenide polycrystal and a metallographic etching method thereof. The invention provides a metallographic etching solution for gallium arsenide polycrystal, which comprises the following components: ammonia, hydrogen peroxide and water; the mass concentration of the ammonia water is 25-28 wt%; the mass concentration of the hydrogen peroxide is 20-30wt%; the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1: (1-2). The metallographic etching liquid of the gallium arsenide polycrystal is obtained by mixing ammonia water, hydrogen peroxide and water, can etch the gallium arsenide polycrystal, can observe the metallographic structure of the gallium arsenide polycrystal from a microscope, can see obvious crystal boundaries and tissue crystal grains, and can measure the size and the grain size of the crystal grains so as to judge the uniformity and the quality of materials, thereby evaluating the quality of the prepared materials, clamping the materials with poor quality in the current process, and preventing the materials from flowing to the next process, thereby increasing the production cost.
Description
Technical Field
The invention relates to the field of semiconductor materials, in particular to a metallographic etching solution for gallium arsenide polycrystal and a metallographic etching method thereof.
Background
The structure of the material has close relation with the performance of the material, and metallographic observation is the most direct and effective method for researching the internal structure of the metal material. The metallographic phase display is a common technology for observing the internal structure of metals and alloys thereof, the basic principle is that the corrosion resistance difference of each phase in the metals and between crystal grains and crystal boundaries to the same corrosion solution is utilized to display different structure phases, and the characterization technology has the characteristics of simplicity and easy implementation and is widely applied to material science research.
The metallographic morphology of the material can reflect the structure and defects of a material matrix phase to a certain extent, so that the quality of the prepared material is evaluated, the material with poor quality is clamped in the current process, and the material is prevented from flowing to the next process, so that the production cost is increased. But no metallographic etching solution with good effect on gallium arsenide polycrystal exists at present.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is a metallographic etching solution and a metallographic etching method for gallium arsenide polycrystal, the metallographic etching solution provided by the invention can etch gallium arsenide polycrystal, and the metallographic structure of gallium arsenide polycrystal can be observed from a microscope, and obvious crystal boundary and structural crystal grains can be seen.
The invention provides a metallographic etching solution for gallium arsenide polycrystal, which comprises ammonia water, hydrogen peroxide and water; the mass concentration of the ammonia water is 25-28 wt%; the mass concentration of the hydrogen peroxide is 20-30wt%; the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1: (1-2).
The corrosive liquid provided by the invention is obtained by mixing ammonia water, hydrogen peroxide and pure water. In one embodiment, the corrosive liquid comprises ammonia water with the mass concentration of 25wt%, hydrogen peroxide with the mass concentration of 27.5wt% and water; the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1:1 or 2:1:2.
the invention also provides a metallographic etching method of the gallium arsenide polycrystal, which comprises the following steps: metallographic etching is carried out on gallium arsenide polycrystal by using metallographic etching liquid; the metallographic etching liquid is the same as the metallographic etching liquid of the gallium arsenide polycrystal, and is not repeated.
When the metallographic etching liquid of the gallium arsenide polycrystal is used for etching the gallium arsenide polycrystal, the etching degree can be judged through observation of a gallium arsenide polycrystal sample, so that the etching degree can be controlled conveniently, and over-etching or under-etching is prevented. In some embodiments of the invention, the time for etching the gallium arsenide polycrystalline metallographic phase by the metallographic etching liquid is 60-180 s. In some embodiments of the invention, the temperature of the gallium arsenide polycrystalline metallographic phase etched by the metallographic phase etching liquid is 0-20 ℃.
Before the metallographic etching liquid is used for metallographic etching of gallium arsenide polycrystal, the method further comprises the steps of sequentially embedding, grinding and polishing the gallium arsenide polycrystal. In one embodiment of the invention, the mounting is: placing gallium arsenide polycrystal into a mould, wherein the mass ratio is 4:1, mixing the epoxy resin and the curing agent, curing in a mold and taking out; the gallium arsenide polycrystal has the size of 20mm multiplied by 10mm, and the size is more convenient for embedding, thereby being convenient for operation. In one embodiment of the invention, the polishing is: and sequentially grinding the gallium arsenide polycrystal after the mounting by using sand paper of P180, P360, P500, P1200 and P2500, wherein the grinding is carried out for 5-25 min at a rotating speed of 10-300 r/min each time. In one embodiment of the invention, the polishing is: polishing agents of 15 mu m, 6 mu m and 0.25 mu m are sequentially used for fine polishing of the polished gallium arsenide polycrystal, so that the surface of the gallium arsenide polycrystal is bright and shows obvious mirror surface and no scratch. And cleaning and drying the polished gallium arsenide polycrystal surface polishing solution, and then corroding the gallium arsenide polycrystal metallographic phase by using the metallographic phase corrosion solution.
The invention provides a metallographic etching solution for gallium arsenide polycrystal and a metallographic etching method thereof. The invention provides a metallographic etching solution for gallium arsenide polycrystal, which comprises the following components: ammonia, hydrogen peroxide and water; the mass concentration of the ammonia water is 25-28 wt%; the mass concentration of the hydrogen peroxide is 20-30wt%; the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1: (1-2). The metallographic etching liquid of the gallium arsenide polycrystal is obtained by mixing ammonia water, hydrogen peroxide and water, can etch the gallium arsenide polycrystal, can observe the metallographic structure of the gallium arsenide polycrystal from a microscope, can see obvious crystal boundaries and tissue crystal grains, and can measure the size and the grain size of the crystal grains so as to judge the uniformity and the quality of materials, thereby evaluating the quality of the prepared materials, clamping the materials with poor quality in the current process, and preventing the materials from flowing to the next process, thereby increasing the production cost.
Drawings
FIG. 1 is a golden phase diagram of a sample after corrosion in this example;
FIG. 2 is a golden phase diagram of the sample after etching in this example;
FIG. 3 is a golden phase diagram of the sample after corrosion in this comparative example.
Detailed Description
The invention discloses a metallographic etching solution and a metallographic etching method for gallium arsenide polycrystal. Those skilled in the art can, with the benefit of this disclosure, suitably modify the process parameters to achieve this. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.
The specific embodiment of the application is carried out according to the following five stages (a) - (e):
(a) The first stage: sample-mounting treatment
Cutting gallium arsenide polycrystal into square sample with size of 20mm×20mm×10 mm; the size is more convenient for embedding, thereby being convenient for operation;
placing the cut sample in a mould, and mixing epoxy resin and a curing agent according to the mass ratio of the epoxy resin: curing agent = 4: and 1, mixing and pouring the mixture into a die, and taking out after solidification.
(b) And a second stage: polishing
The polishing was performed sequentially using P180, P360, P500, P1200 and P2500 sandpaper, each time at a rotation speed of 250r/min for 20min depending on the polishing conditions.
(c) And a third stage: polishing
Polishing the polished sample with polishing agents of 15 μm, 6 μm and 0.25 μm in sequence, wherein the surface of the sample is bright, and has obvious mirror surface and no scratch;
(d) Fourth stage: cleaning, drying, etching and rinsing
And (3) cleaning the polished sample surface with clear water, thoroughly washing off the polishing solution on the surface, then wiping the water-washed sample block with alcohol, drying the sample surface with hot air by using a blower, corroding the sample dried with hot air by using the corresponding metallographic corrosive liquid, washing with pure water after corrosion, and drying with the blower.
(e) Fifth stage: and observing the grain boundary of the tissue on the surface of the treated sample by a metallographic microscope.
The invention is further illustrated by the following examples:
example 1
The embodiment provides a metallographic etching solution, which comprises the following components in percentage by volume: ammonia water: hydrogen peroxide: pure water=2:1:2, wherein the mass percentage concentration of the ammonia water is 25wt%, and the mass percentage concentration of the hydrogen peroxide is 27.5wt%. The preparation method of the metallographic corrosive liquid comprises the following steps: firstly, weighing 20mL of pure water by using a cup, pouring the pure water into a beaker with 150mL of capacity, respectively weighing 10mL of hydrogen peroxide and 20mL of ammonia water, slowly pouring the pure water into the beaker, and stirring the pure water by using a glass rod to uniformly mix the pure water to obtain the metallographic corrosive liquid.
In the fourth stage, the sample dried by hot air is corroded by the metallographic corrosive liquid, specifically, the polished surface of the sample is immersed in the corrosive liquid for 60-180 s and then taken out, the corroded sample is rinsed by pure water for 1 min, and then the sample is dried by a blower.
The grain boundaries of the structure on the surface of the treated sample were observed by a microscope, as shown in fig. 1, and fig. 1 is a golden phase diagram of the sample after corrosion in this example. The corresponding grain boundaries and structure can be clearly seen from FIG. 1
Example 2
The difference between this example and example 1 is that the volume ratio of the metallographic etchant is: ammonia water: hydrogen peroxide: pure water=2:1:1, wherein the mass percentage concentration of the ammonia water is 25wt%, and the mass percentage concentration of the hydrogen peroxide is 27.5wt%. The preparation method of the metallographic corrosive liquid comprises the following steps: firstly, measuring 10mL of pure water by using a measuring cup, pouring the pure water into a beaker with 150mL of capacity, respectively measuring 10mL of hydrogen peroxide and 20mL of ammonia water, slowly pouring the pure water into the beaker, and stirring the pure water by using a glass rod to uniformly mix the pure water and the ammonia water to obtain the metallographic corrosive liquid.
In the fourth stage, the sample dried by hot air is corroded by the metallographic etching solution, specifically, the polished surface of the sample is immersed in the etching solution for 120s and then taken out, the corroded sample is rinsed by pure water for 1 minute, and then the sample is dried by a blower.
The grain boundaries of the structure on the surface of the treated sample were observed by a microscope, as shown in fig. 2, and fig. 2 is a golden phase diagram of the sample after corrosion in this example. The corresponding grain boundaries and organized grains can be clearly seen from fig. 2.
Comparative example 1
The comparative example provides a metallographic etching solution, the volume ratio of the metallographic etching solution is as follows: ammonia water: hydrogen peroxide: pure water=2:1:2, wherein the mass percentage concentration of the ammonia water is 25wt%, and the mass percentage concentration of the hydrogen peroxide is 27.5wt%. The preparation method of the metallographic corrosive liquid comprises the following steps: firstly, weighing 20mL of pure water by using a cup, pouring the pure water into a beaker with 150mL of capacity, respectively weighing 10mL of hydrogen peroxide and 20mL of ammonia water, slowly pouring the pure water into the beaker, and stirring the pure water by using a glass rod to uniformly mix the pure water to obtain the metallographic corrosive liquid.
In the fourth stage, the sample dried by hot air is corroded by the metallographic corrosive liquid, specifically, the polished surface of the sample is immersed in the corrosive liquid for 120 seconds and then taken out, the corroded sample is rinsed by pure water for 1 minute, and then the sample is dried by a blower.
The grain boundaries of the structure on the surface of the treated sample were observed under a microscope, as shown in fig. 3, and fig. 3 is a golden phase diagram of the sample after corrosion in this comparative example. The corresponding grain boundaries and organized grains cannot be seen from fig. 3.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. A metallographic etching solution for gallium arsenide polycrystal, which is characterized by comprising: ammonia, hydrogen peroxide and water;
the mass concentration of the ammonia water is 25-28 wt%;
the mass concentration of the hydrogen peroxide is 20-30wt%;
the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1: (1-2).
2. The metallographic etching solution according to claim 1, wherein the metallographic etching solution comprises ammonia water with a mass concentration of 25wt%, hydrogen peroxide with a mass concentration of 27.5wt% and water.
3. The metallographic etching solution according to claim 2, wherein the volume ratio of the ammonia water, the hydrogen peroxide solution and the water is 2:1:1.
4. the metallographic etching solution according to claim 2, wherein the volume ratio of the ammonia water, the hydrogen peroxide solution and the water is 2:1:2.
5. a metallographic etching method of gallium arsenide polycrystal, which is characterized by comprising the following steps: metallographic etching is carried out on gallium arsenide polycrystal by using metallographic etching liquid;
the metallographic etching solution comprises: ammonia, hydrogen peroxide and water;
the mass concentration of the ammonia water is 25-28 wt%;
the mass concentration of the hydrogen peroxide is 20-30wt%;
the volume ratio of the ammonia water to the hydrogen peroxide to the water is 2:1: (1-2).
6. The metallographic etching method according to claim 5, wherein the metallographic etching liquid comprises ammonia water with a mass concentration of 25wt%, hydrogen peroxide with a mass concentration of 27.5wt% and water.
7. The metallographic etching method according to claim 6, wherein the volume ratio of the ammonia water, the hydrogen peroxide solution and the water is 2:1:1.
8. the metallographic etching method according to claim 6, wherein the volume ratio of the ammonia water, the hydrogen peroxide solution and the water is 2:1:2.
9. the method according to claim 5, wherein the time for etching the gallium arsenide polycrystal metallographic phase with the metallographic etching liquid is 60-180 s.
10. The method according to claim 5, wherein the temperature of etching the gallium arsenide polycrystal metallographic phase with the metallographic etching liquid is 0-20 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311441242.XA CN117447999A (en) | 2023-11-01 | 2023-11-01 | Metallographic etching liquid for gallium arsenide polycrystal and metallographic etching method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311441242.XA CN117447999A (en) | 2023-11-01 | 2023-11-01 | Metallographic etching liquid for gallium arsenide polycrystal and metallographic etching method thereof |
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| Publication Number | Publication Date |
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| CN117447999A true CN117447999A (en) | 2024-01-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311441242.XA Pending CN117447999A (en) | 2023-11-01 | 2023-11-01 | Metallographic etching liquid for gallium arsenide polycrystal and metallographic etching method thereof |
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| CN (1) | CN117447999A (en) |
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2023
- 2023-11-01 CN CN202311441242.XA patent/CN117447999A/en active Pending
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