CN112592663A - Nano-diamond polishing solution for processing SiC substrate and preparation method thereof - Google Patents
Nano-diamond polishing solution for processing SiC substrate and preparation method thereof Download PDFInfo
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- CN112592663A CN112592663A CN202011523862.4A CN202011523862A CN112592663A CN 112592663 A CN112592663 A CN 112592663A CN 202011523862 A CN202011523862 A CN 202011523862A CN 112592663 A CN112592663 A CN 112592663A
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- 238000005498 polishing Methods 0.000 title claims abstract description 76
- 239000000758 substrate Substances 0.000 title claims abstract description 36
- 239000002113 nanodiamond Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 18
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 68
- 239000010432 diamond Substances 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 63
- 239000002245 particle Substances 0.000 claims abstract description 60
- 239000000375 suspending agent Substances 0.000 claims abstract description 39
- 239000002270 dispersing agent Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 22
- 239000000314 lubricant Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 44
- 239000006185 dispersion Substances 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 17
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 16
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 16
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 15
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 15
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- 229920002396 Polyurea Polymers 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- 235000012216 bentonite Nutrition 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 229960001631 carbomer Drugs 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 239000001540 sodium lactate Substances 0.000 claims description 2
- 229940005581 sodium lactate Drugs 0.000 claims description 2
- 235000011088 sodium lactate Nutrition 0.000 claims description 2
- 238000002525 ultrasonication Methods 0.000 claims 2
- 238000000227 grinding Methods 0.000 abstract description 5
- 239000006061 abrasive grain Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000006748 scratching Methods 0.000 description 4
- 230000002393 scratching effect Effects 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention discloses a nano-diamond polishing solution for processing a SiC substrate and a preparation method thereof, belonging to the technical field of ultra-precision grinding and polishing, wherein the polishing solution is prepared from the following raw materials in parts by weight: 50-85 parts of water; 0.5-15 parts of diamond micro powder; 0.1-5 parts of a dispersant; 0.1-5 parts of a suspending agent; 1-40 parts of a lubricant; 0.001-0.1 part of defoaming agent, the granularity of diamond micro powder is 10-1000nm, the number ratio of wear-resistant abrasive particles to round abrasive particles in the diamond micro powder is 1-15:1, and round abrasive particles with the roundness Fc more than 0.950 are round abrasive particles; fc is more than or equal to 0.900 and less than or equal to 0.950, and the wear-resistant abrasive particles are prepared. The polishing solution is formed by controlling the appearance of diamond micro powder, so that the polishing efficiency is improved by the wear-resistant abrasive particles, and meanwhile, the surface damage layer and the roughness are repaired by the aid of the round abrasive particles, so that the polishing scratch is controlled.
Description
Technical Field
The invention belongs to the field of ultra-precision grinding and polishing, and particularly relates to a nano-diamond polishing solution for processing a SiC substrate and a preparation method thereof.
Background
SiC, as a representative of third generation semiconductor materials, has formed a global material, device, and application industry chain. Because of excellent performance in high temperature, high frequency, radiation resistance and high power application, the material is widely applied to core industries such as national defense and military provision, 5G mobile communication, energy internet, new energy automobiles, rail transit and the like. The new generation of 'gold racetrack' in the semiconductor industry drives the reputations of 'green energy devices' and the like of the energy revolution, and particularly catalyzes the hot spot of 'getting SiC from the world'.
The purpose of polishing is to remove mechanically damaged layers such as scratches and pits of the previous grinding and to reduce the surface roughness of the workpiece. The depth of the mechanical damage layer and the surface roughness are related to the granularity of the abrasive in the grinding fluid adopted in the previous process. Generally, it is necessary to remove 3 times of the thickness of the abrasive grain size in the grinding fluid of the previous process to completely remove the mechanically damaged layer caused by the previous process. That is, if the previous polishing is performed using a 3um diamond polishing liquid, the remaining 9um is removed in the subsequent polishing, so that the mechanical damage layer caused by the polishing can be completely eliminated.
Typically, nano-SiO is used for polishing2Polishing solution, nano SiO2The Mohs hardness is about 6.8, the Mohs hardness of the SiC substrate is about 9.5, the abrasive hardness is far lower than the hardness of a workpiece, and the polishing efficiency is low, so that the polishing time is often required to be several hours, and the bottleneck for limiting the time of the whole processing technology is realized. In order to rapidly obtain a high-quality SiC substrate, the invention relates to a nano-diamond polishing solution which can be used for nano SiO2The pre-polishing process quickly optimizes the wafer surface roughness and surface damage layer to reduce the overall polishing time. However, since the mohs hardness of diamond is 10, which is slightly higher than the hardness of the SiC substrate, the polishing performance of the nano-diamond polishing solution needs to be strictly controlled to avoid the generation of polishing scratches.
Disclosure of Invention
The invention relates to a nano-diamond polishing solution for processing a SiC substrate and a preparation method thereof, which can be used for nano-SiO2The working procedure before polishing can effectively control polishing scratch and simultaneously can quickly optimize the surface roughness and the surface damage layer of the wafer so as to reduceOverall polishing time.
Based on the purpose, the invention adopts the following technical scheme:
a nano-diamond polishing solution for processing a SiC substrate comprises the following raw materials in parts by weight:
50-85 parts of water; 0.5-15 parts of diamond micro powder; 0.1-5 parts of a dispersant; 0.1-5 parts of a suspending agent; 1-40 parts of a lubricant; 0.001-0.1 part of defoaming agent.
The diamond micro powder is one or a mixture of more of single crystal diamond micro powder, polycrystal-like diamond micro powder or polycrystal diamond micro powder, and the granularity of the diamond micro powder is 10-1000 nm.
The number ratio of the wear-resistant abrasive particles to the round abrasive particles in the diamond micro powder is 1-15. Wear-resistant abrasive particles and round abrasive particles are selected in a key mode, the wear-resistant abrasive particles are used for improving polishing efficiency, and the round abrasive particles are used for repairing a surface damage layer and roughness to avoid scratches.
And analyzing the particle number ratio of the wear-resistant abrasive particles to the round particles by using a KBKL-II type particle size image analyzer. Wherein: roundness Fc = equivalent circumference of particle projection area/actual circumference of particle projection, Fc > 0.950 is round abrasive grain; fc is more than or equal to 0.900 and less than or equal to 0.950, and the wear-resistant abrasive particles are prepared.
The dispersing agent is selected from one or a mixture of more than two of sodium citrate, sodium lactate, triethanolamine, alkyl ammonium oxide, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether and alkylolamide in any proportion.
The suspending agent is one or a mixture of more than two of hydroxyethyl cellulose, sodium carboxymethylcellulose, bentonite, sodium alginate, sodium polyacrylate, polyacrylamide, polyurethane resin, carbomer resin and modified polyurea in any proportion.
The lubricant is one or a mixture of more than two of ethylene glycol, glycerol, diethylene glycol, polyethylene glycol, polyvinylpyrrolidone and polyethylene oxide in any proportion.
The defoaming agent is an organic silicon defoaming agent.
The preparation method of the nano-diamond polishing solution for processing the SiC substrate comprises the following steps:
s1, uniformly mixing 10-20wt% of water with a dispersant to form a dispersant solution;
s2, slowly adding diamond micro powder into the dispersing agent solution under the stirring condition, and performing ultrasonic-assisted dispersion to form diamond micro powder dispersion liquid;
s3, adding the suspending agent into the residual water, and fully stirring and dissolving the mixture uniformly to form a suspending agent solution;
and S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding the lubricant and the defoaming agent, and uniformly stirring.
Wherein the power during ultrasonic treatment is 400-600W, and the ultrasonic treatment time is 60-120 minutes.
The nano diamond polishing solution can be used for nano SiO2The working procedure before polishing can effectively inhibit the generation of scratches and simultaneously can quickly optimize the surface quality of the wafer.
The invention has the beneficial effects that:
the invention provides a preparation process and a use method of a nano-diamond polishing solution, wherein the polishing solution is formed by controlling the appearance of diamond micro-powder, so that the polishing efficiency is improved by wear-resistant abrasive particles, and meanwhile, a surface damage layer and roughness are repaired by virtue of round abrasive particles, thereby realizing the control of polishing scratches.
Drawings
FIG. 1 is a picture of the appearance of the nano-diamond micro-powder particles of example 4 magnified 100 times;
fig. 2 is an evaluation picture of the osm type profile analysis system detecting scratches and gouges on the surface of a wafer; wherein: the scratch is the abrasive grain diameter less than or equal to 3 times of the depth, can be effectively removed through the subsequent CMP polishing, and is repairable; the scratch is the abrasive grain diameter which is more than 3 times of the depth, can not be removed in the subsequent CMP process, and is relatively unrepairable;
FIG. 3 is a 100-fold magnified photograph of a SiC substrate sheet polished with the polishing solution of comparative example 1;
FIG. 4 is a 100 times magnified view of a SiC substrate wafer polished with the polishing solution of example 4;
FIG. 5 is a photograph of a SiC substrate sheet polished with the polishing solution of comparative example 3, at a magnification of 100.
Detailed Description
The modified sodium polyacrylate in the following examples is a sodium polyacrylate modified by Bick chemical DISPERBYK2010 type, and the modified polyurea is a modified polyurea by Bick chemical BYK420 type.
Example 1
A nano-diamond polishing solution for processing a SiC substrate comprises the following components: 500g of water, 15g of diamond micro powder, 3g of fatty alcohol-polyoxyethylene ether (dispersing agent), 25g of hydroxyethyl cellulose (suspending agent), 25g of modified sodium polyacrylate (suspending agent), 75g of glycol (lubricating agent) and 0.5g of organic silicon defoaming agent.
The preparation method of the polishing solution comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution;
s2, slowly adding 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 1 into the dispersing agent solution under the stirring condition, and using 500W ultrasonic wave to assist and disperse for 90min until the diamond micro powder is completely and uniformly dispersed to form diamond micro powder dispersion liquid;
s3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, fully stirring at 1500rpm, and stirring for 4 hours until the materials are uniformly dissolved to form a suspending agent solution;
and S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 2
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, 100g of water and 3g of sodium citrate are uniformly mixed to form a dispersant solution.
S2, under the stirring condition, 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 3 is slowly added into the dispersing agent solution, and the ultrasonic wave of 500W is utilized to assist and disperse for 90min, so that the diamond micro powder dispersing liquid is formed.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 3
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, adding 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 6 slowly into the dispersing agent solution, and dispersing for 90min by using 500W ultrasonic wave to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 4
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 8 is slowly added into the dispersing agent solution, and the ultrasonic wave of 500W is utilized to assist and disperse for 90min, so that the diamond micro powder dispersing liquid is formed.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 5
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, adding 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 10 into the dispersing agent solution slowly, and dispersing for 90min by using 500W ultrasonic wave to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 6
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, adding 15g of 600nm diamond micro powder with the ratio of the number of wear-resistant abrasive particles to the number of round abrasive particles being 12 slowly into the dispersing agent solution, and dispersing for 90min by using 500W ultrasonic wave to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 7
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, slowly adding 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 15 into the dispersing agent solution under the stirring condition, and performing auxiliary dispersion for 90min by using 500W ultrasonic waves to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 8
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of sodium citrate to form a dispersant solution;
s2, slowly adding 15g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 8 into the dispersing agent solution under the stirring condition, and performing auxiliary dispersion for 90min by using 500W ultrasonic waves to form diamond micro powder dispersion liquid;
s3, adding 25g of sodium alginate and modified polyurea into 400g of water respectively, and fully stirring and dissolving uniformly to form a suspending agent solution;
and S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 5g of K90 type polyvinylpyrrolidone and 0.5g of organic silicon defoamer, and uniformly stirring.
Example 9
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, slowly adding 5g of 600nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 18 into the dispersing agent solution under the stirring condition, and performing auxiliary dispersion for 90min by using 500W ultrasonic waves to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 10
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, slowly adding 15g of 900nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 8 into the dispersing agent solution, and using 500W ultrasonic wave to assist and disperse for 60min to form the diamond micro powder dispersing liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Example 11
A preparation method of nano-diamond polishing solution for processing a SiC substrate comprises the following steps:
s1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, under the stirring condition, 15g of 100nm diamond micro powder with the ratio of the number of the wear-resistant abrasive particles to the number of the round abrasive particles being 8 is slowly added into the dispersing agent solution, and 500W ultrasonic wave is utilized to assist and disperse for 120min, so that the diamond micro powder dispersing liquid is formed.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Comparative example 1
S1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, slowly adding 15g of wear-resistant abrasive grain diamond micro powder with the particle size of 600nm into the dispersing agent solution under the stirring condition, and performing ultrasonic wave auxiliary dispersion for 90min by using 500W to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Comparative example 2
S1, uniformly mixing 100g of water and 3g of fatty alcohol-polyoxyethylene ether to form a dispersing agent solution.
S2, slowly adding 15g of round abrasive grain diamond micro powder with the particle size of 600nm into the dispersing agent solution under the stirring condition, and performing ultrasonic wave auxiliary dispersion for 90min by using 500W to form diamond micro powder dispersion liquid.
S3, adding 25g of hydroxyethyl cellulose and 25g of modified sodium polyacrylate into 400g of water, and fully stirring and dissolving uniformly to form a suspending agent solution.
And S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding 75g of ethylene glycol and 0.5g of organic silicon defoaming agent, and uniformly stirring.
Comparative example 3
Dupont SR330 type nano SiO2And (4) polishing solution.
A4-inch diameter and 440 μm SiC substrate sheet was polished using the polishing liquids of the above examples and comparative examples. Using a ZYP400 type polisher, a Suba600 type polishing pad, at a pressure of 200g/cm2The rotating speed is 40rpm, the diamond polishing solution flow is 5ml/min, and the polishing time is 1.5 h; nano SiO2The flow rate of the polishing solution was 300ml/min, the polishing time was 3 hours, and scratches were detected by using a dialsipect.osm morphology subsystem, and the determination criteria are shown in fig. 2a and 2b (enlarged by 100 times), respectively. The specific results are as follows:
TABLE 1 comparison table of polishing solution application properties
As can be seen from Table 1: nano SiO2The polishing efficiency of the polishing solution is 0.78 um/h; diamond polishing solution prepared by completely adopting circular abrasive particlesThe efficiency is about 2.46 um/h; when the ratio of the wear-resistant abrasive particles to the round abrasive particles reaches 8, the efficiency reaches 7.98um/h, and the scratching condition is good; when the wear-resistant abrasive grain/round abrasive grain ratio reaches 10, the efficiency reaches 8.69um/h, but repairable scratches appear; when the ratio of the wear-resistant abrasive particles to the round abrasive particles reaches 18, the efficiency reaches 9.01um/h, but scratches are increased and occur along with irreparable scratches; the polishing efficiency of the diamond polishing solution prepared by completely adopting the wear-resistant abrasive particles is about 9.21um/h, but the diamond polishing solution is seriously scratched and is basically in a full-sheet scratching state. Therefore, the wear-resistant abrasive grain/round abrasive grain ratio is preferably 1-15, more preferably 6-12, and most preferably 6-8, and the diamond micro-powder particle size is preferably 600nm, which takes the efficiency improvement and the scratch control into consideration.
Photographs of the polished SiC substrates of comparative example 1, example 4 and comparative example 3 are shown in fig. 3, fig. 4 and fig. 5, and it can be seen from table 1 that the results of scratching and/or scratching are consistent with the data in table 1.
The method for preparing the nano diamond polishing solution by preferably selecting the wear-resistant abrasive particles and the round abrasive particles is also suitable for preparing the nano super-hard abrasive polishing solution for various substrate materials such as sapphire substrates, silicon substrates, gallium arsenide, gallium nitride, indium phosphide and the like.
Although the present invention has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the true spirit and scope of the present invention, which is intended to be covered by the claims.
Claims (7)
1. The nano-diamond polishing solution for processing the SiC substrate is characterized by comprising the following raw materials in parts by weight:
50-85 parts of water; 0.5-15 parts of diamond micro powder; 0.1-5 parts of a dispersant; 0.1-5 parts of a suspending agent; 1-40 parts of a lubricant; 0.001-0.1 part of defoaming agent, the granularity of diamond micro powder is 10-1000nm, the ratio of the number of wear-resistant abrasive particles to the number of round abrasive particles is 1-15:1, wherein the round abrasive particles are round abrasive particles with the roundness Fc more than 0.950; fc is more than or equal to 0.900 and less than or equal to 0.950, and the wear-resistant abrasive particles are prepared.
2. The nano-diamond polishing solution for processing the SiC substrate as recited in claim 1, wherein the dispersing agent is one or a mixture of two or more of sodium citrate, sodium lactate, triethanolamine, alkyl ammonium oxide, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene ether and alkylolamide in any proportion.
3. The nano-diamond polishing solution for processing the SiC substrate according to claim 1, wherein the suspending agent is one or a mixture of two or more of hydroxyethyl cellulose, sodium carboxymethyl cellulose, bentonite, sodium alginate, sodium polyacrylate, polyacrylamide, polyurethane resin, carbomer resin and modified polyurea in any proportion.
4. The nanodiamond polishing solution for processing an SiC substrate according to claim 1, wherein the lubricant is one or a mixture of two or more of ethylene glycol, glycerol, diethylene glycol, polyethylene glycol, polyvinylpyrrolidone, and polyethylene oxide at any ratio.
5. The nanodiamond polishing solution for SiC substrate processing according to claim 1, wherein the defoaming agent is an organic silicon defoaming agent.
6. The method for preparing a nanodiamond polishing solution for SiC substrate processing according to any one of claims 1 to 5, characterized by the steps of:
s1, uniformly mixing 10-20wt% of water with a dispersant to form a dispersant solution;
s2, slowly adding diamond micro powder into the dispersing agent solution under the stirring condition, and performing ultrasonic-assisted dispersion to form diamond micro powder dispersion liquid;
s3, adding the suspending agent into the residual water, and fully stirring and dissolving the mixture uniformly to form a suspending agent solution;
and S4, uniformly mixing the diamond micro powder dispersion liquid and the suspending agent solution, sequentially adding the lubricant and the defoaming agent, and uniformly stirring.
7. The method for preparing a nanodiamond polishing solution for processing an SiC substrate according to claim 6, characterized in that the power during ultrasonication is 400 to 600W and the ultrasonication time is 60 to 120 minutes.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265224A (en) * | 2021-04-29 | 2021-08-17 | 郑州磨料磨具磨削研究所有限公司 | Spray type diamond grinding fluid and preparation method thereof |
| CN113913154A (en) * | 2021-04-27 | 2022-01-11 | 北京利研科技有限公司 | Efficient suspension auxiliary agent and preparation and application thereof |
| CN114231251A (en) * | 2021-12-27 | 2022-03-25 | 河南联合精密材料股份有限公司 | Diamond grinding fluid for coarse grinding of silicon carbide wafer and preparation method thereof |
| CN114736654A (en) * | 2022-04-28 | 2022-07-12 | 浙江奥首材料科技有限公司 | Spherical abrasive, preparation method and application thereof, and sapphire grinding fluid containing spherical abrasive |
| CN115725242A (en) * | 2022-12-09 | 2023-03-03 | 郑州磨料磨具磨削研究所有限公司 | High-efficiency low-damage diamond grinding fluid and preparation method thereof |
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| CN115873508A (en) * | 2022-12-26 | 2023-03-31 | 博力思(天津)电子科技有限公司 | SiC substrate polishing solution with high removal rate and low surface roughness and polishing process |
| CN115926747A (en) * | 2022-12-08 | 2023-04-07 | 郑州磨料磨具磨削研究所有限公司 | Concentrated aqueous grinding aid and preparation method thereof |
| CN116144270A (en) * | 2023-02-20 | 2023-05-23 | 湖南三安半导体有限责任公司 | Polishing solution and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031560A (en) * | 2013-03-07 | 2014-09-10 | 天津市乾宇超硬科技有限公司 | Water-based diamond polishing solution used for crystal processing |
| JP5853117B1 (en) * | 2014-06-30 | 2016-02-09 | 花王株式会社 | Polishing liquid composition for magnetic disk substrate |
| CN111548737A (en) * | 2020-06-04 | 2020-08-18 | 湖南圣高机械科技有限公司 | Diamond grinding fluid and preparation method thereof |
-
2020
- 2020-12-22 CN CN202011523862.4A patent/CN112592663B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031560A (en) * | 2013-03-07 | 2014-09-10 | 天津市乾宇超硬科技有限公司 | Water-based diamond polishing solution used for crystal processing |
| JP5853117B1 (en) * | 2014-06-30 | 2016-02-09 | 花王株式会社 | Polishing liquid composition for magnetic disk substrate |
| CN111548737A (en) * | 2020-06-04 | 2020-08-18 | 湖南圣高机械科技有限公司 | Diamond grinding fluid and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 梁庆瑞等: "金刚石微粉对SiC机械抛光的影响研究", 《人工晶体学报》 * |
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| CN113265224B (en) * | 2021-04-29 | 2021-11-30 | 郑州磨料磨具磨削研究所有限公司 | Spray type diamond grinding fluid and preparation method thereof |
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