CN110405649B - Sol-gel polishing pellet added with soluble filler with water-resistant coating and preparation method thereof - Google Patents
Sol-gel polishing pellet added with soluble filler with water-resistant coating and preparation method thereof Download PDFInfo
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- CN110405649B CN110405649B CN201910716724.9A CN201910716724A CN110405649B CN 110405649 B CN110405649 B CN 110405649B CN 201910716724 A CN201910716724 A CN 201910716724A CN 110405649 B CN110405649 B CN 110405649B
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- 238000005498 polishing Methods 0.000 title claims abstract description 91
- 239000008188 pellet Substances 0.000 title claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000945 filler Substances 0.000 title claims abstract description 27
- 238000000576 coating method Methods 0.000 title claims abstract description 21
- 239000011248 coating agent Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 10
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 33
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 33
- 238000000227 grinding Methods 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 15
- -1 phenolic aldehyde Chemical class 0.000 claims abstract description 12
- 238000009966 trimming Methods 0.000 claims abstract 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 239000003292 glue Substances 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 229910003460 diamond Inorganic materials 0.000 claims description 19
- 239000010432 diamond Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000011265 semifinished product Substances 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
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- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000000080 wetting agent Substances 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 6
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- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
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- JZZIHCLFHIXETF-UHFFFAOYSA-N dimethylsilicon Chemical compound C[Si]C JZZIHCLFHIXETF-UHFFFAOYSA-N 0.000 claims description 4
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- 238000009499 grossing Methods 0.000 claims description 4
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- 238000007873 sieving Methods 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910001610 cryolite Inorganic materials 0.000 claims description 3
- 239000002612 dispersion medium Substances 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical group [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 241000252203 Clupea harengus Species 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 235000019514 herring Nutrition 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 238000010257 thawing Methods 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000004846 water-soluble epoxy resin Substances 0.000 claims description 2
- 239000002344 surface layer Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 239000007767 bonding agent Substances 0.000 abstract description 5
- 235000015895 biscuits Nutrition 0.000 abstract description 4
- 239000006187 pill Substances 0.000 description 37
- 239000000463 material Substances 0.000 description 14
- 229910052732 germanium Inorganic materials 0.000 description 8
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 230000003746 surface roughness Effects 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 6
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- 239000010410 layer Substances 0.000 description 6
- 229910001018 Cast iron Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 5
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- 239000005543 nano-size silicon particle Substances 0.000 description 4
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- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/009—Tools not otherwise provided for
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention discloses a self-trimming polishing pellet added with a water-resistant coating soluble filler and a preparation method thereof. The grinding tool made of the mixed resin liquid gel of polyvinyl alcohol and phenolic aldehyde utilizes the physical gel capability of polyvinyl alcohol to form a gel biscuit, the polyvinyl alcohol is sintered and carbonized at high temperature, water-soluble resin is solidified to be used as a bonding agent for polishing the pellet, a large number of capillary through micropores are generated after the polyvinyl alcohol is carbonized, the absorption capability to water is strong, soluble aluminum nitride with a water-resistant coating is added, after the water-resistant coating of aluminum nitride particles on the surface layer of the pellet is ground off, the aluminum nitride is hydrolyzed, the strength is reduced, the effect of self-sharpening the surface layer is achieved, and the water-resistant coating of the aluminum nitride inside the pellet is protected, so that the overall strength of the pellet is ensured.
Description
Technical Field
The invention belongs to the field of precision machining grinding and polishing, and relates to a sol-gel polishing pellet added with a water-resistant coating soluble filler and a preparation method thereof.
Background
In optical machining, generally, after one-pass refining and two-pass super-refining in high-speed refining, although the surface shape is smooth and regular, it is not completely transparent and the surface shape is not required, and the element is polished to achieve the required surface finish, at this time, high-speed refining by a polishing sheet is required, and polishing is a main process after the refining. The purpose of polishing is therefore: (1) removing the finely ground destructive layer to meet the specified appearance limit requirement; (2) and (5) finishing the surface shape to reach the curvature radius R value specified by the drawing, so that the requirement of the local tolerance of the aperture is met.
However, the traditional method for manufacturing the grinding tool is powder mixing → sieving → drying → pressing → sintering, so that the problem of phase agglomeration is easy to occur, and how to reduce the internal defects of the grinding tool with abrasive particles and ensure the uniformity of the grinding tool tissue is an urgent problem to be solved, because the uniformity of the internal tissue directly influences the polishing performance. Meanwhile, the traditional grinding tool has the problem that the grinding tool is passivated after being used for a long time, so that the polishing pill needs to be designed to have the self-sharpening function.
The invention patent with the publication number of 106944939B discloses a self-sharpening superhard superfine grinding tool pellet added with soluble resin materials and a preparation method thereof, the soluble resin materials on the surface layer of the grinding tool are dissolved by grinding fluid, pores are formed among binding agents, and the purposes of reducing the strength of the binding agents and the holding force of the binding agents on peripheral abrasive particles are achieved, so that the purpose of automatically and controllably sharpening the grinding tool on line is achieved, but the method is easy to dissolve the resin generated inside the pellet, and the strength is reduced; the invention patent with publication number 106956222B discloses a porous sponge composite diamond grinding pill sheet adopting a rubber bonding agent and a preparation method thereof, wherein a rubber elastic composite complex containing continuous pores and composite particles are combined into a whole to form a pill sheet with a spongy fine continuous pore tissue, and the surface shape is difficult to ensure due to low rubber hardness; the invention patent with the publication number of 104944956A discloses a preparation method of a polycrystalline nano-diamond grinding tool based on gel reaction, and the method adopts polyacrylonitrile for gelling, has high hardness and is suitable for a grinding stage; the invention patent publication 108081159a discloses a method for forming a polyvinyl acetal resin abrasive organogel that is not suitable for aqueous systems, and that is not carbonized to form capillary pores with a single resin.
In order to solve the problems of phase agglomeration, capillary pore formation and self-sharpening of the diamond polishing pill, the invention adopts composite resin gel molding, one resin is sintered and cured, and the other resin is carbonized to generate capillary micropores; the water-resistant coating filler is added, and the strength of the matrix is ensured under the condition of realizing the surface dissolubility and self-sharpening.
Disclosure of Invention
The invention adopts composite resin to prepare polishing pill, firstly, a polishing pill biscuit is formed by a polyvinyl alcohol low-temperature gel method, then, water-soluble resin is solidified to be used as a polishing pill bonding agent by sintering, and the polyvinyl alcohol is carbonized and decomposed to form through capillary micropores, and the process has the advantages that: (1) the components of the polishing pill prepared by the sol-gel method are uniformly distributed without agglomeration, and the method is suitable for preparing precise polishing pills; (2) the pill tablet is internally provided with a large number of through capillary micropores, which is beneficial to enhancing the adsorption potential energy, improving the friction force and removing chips. And meanwhile, the aluminum nitride powder with the water-resistant coating is added, the aluminum nitride powder on the surface is subjected to frictional decomposition, and under the action of improving self-sharpening performance, the internal water-resistant aluminum nitride powder is used as a filler and is not decomposed, so that the strength of the polished pill is ensured.
In order to achieve the purpose, the invention adopts the following technical scheme:
step 1: preparing water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface;
step 2: dispersing diamond powder, water-resistant aluminum nitride powder, electrolytic copper powder, a filler and an additive in water to prepare a suspension;
and step 3: under the condition of 90 ℃ water bath, dissolving polyvinyl alcohol in a mixed solvent of water and ethanol to obtain polyvinyl alcohol glue, adding water-soluble resin liquid into the polyvinyl alcohol glue to obtain mixed glue, wherein the weight ratio of the polyvinyl alcohol glue to the water-soluble resin liquid in the mixed glue is 1: 1-6, adding the mixed glue into the suspension prepared in the step 2, and mixing to obtain glue-containing slurry; the ethanol has the function of preventing water from crystallizing at low temperature;
and 4, step 4: pouring the slurry containing the colloid into a mold, freezing for 1-3 hours at the temperature of-25 to-15 ℃, naturally drying for 5-10 hours after thawing, taking out a blank from the mold, performing densification treatment, drying for 24-48 hours at the temperature of 45-65 ℃, and then sintering to prepare a polished pellet semi-finished product with micro pores;
and 5: and (4) pasting the semi-finished product of the polishing pellet on a base plate for surface smoothing treatment to obtain the polishing pellet, and further polishing the workpiece.
Further, the step 1 specifically comprises:
mixing 1-10 parts by weight of aluminum nitride powder and 50 parts by weight of absolute ethyl alcohol, and uniformly stirring at 40 ℃ to obtain an aluminum nitride ethanol dispersion liquid; dropwise adding 3-6 parts of tetraethoxysilane diluted by 30 parts of absolute ethyl alcohol, 4-6 parts of ammonia water diluted by 30 parts of absolute ethyl alcohol and 5 parts of water into the aluminum nitride ethanol dispersion liquid at the dropping speed of 1-2 drops/second, then carrying out gel reaction for 6 hours at the temperature of 35-45 ℃, carrying out vacuum filtration, washing the product for 3 times by using absolute ethyl alcohol, naturally drying the obtained product for 12-24 hours at the room temperature, then calcining for 2 hours at the temperature of 300 ℃, cooling, and then sieving by using a 200-mesh sieve to obtain the water-resistant aluminum nitride powder with the silicon dioxide film layer on the surface; the aluminum nitride can be hydrolyzed in water, the hydrolysis speed of the aluminum nitride can be adjusted under the alkaline or acidic condition, the aluminum nitride inside the polishing pill can be prevented from being hydrolyzed by coating a layer of silicon dioxide, and the aluminum nitride on the surface layer of the polishing pill is wiped off by the coated silicon dioxide film under the friction action to cause the hydrolysis of the aluminum nitride on the surface layer, so that the binding force is reduced, and the self-sharpening effect is achieved;
further, the step 2 specifically comprises:
adding 5-10 parts by weight of 0.5-5 micron diamond powder, 1-3 parts by weight of water-resistant aluminum nitride powder, 10-30 parts by weight of 200-1000 mesh electrolytic copper powder, 5-10 parts by weight of filler and 0.5-2 parts by weight of additive into 20-50 parts by weight of water, and dispersing by using a planetary ball mill, wherein a dispersion medium is zirconium oxide microspheres to prepare a suspension; the filler is any one or more of copper-coated graphite, talcum powder, cryolite, cerium oxide, aluminum oxide powder, calcium carbonate, calcium oxide, zinc oxide, barium sulfate, magnesium oxide, molybdenum disulfide and silicon carbide; the additive is prepared by mixing a wetting agent, a dispersing agent, an organic silicon defoaming agent and a dimethyl silicon oil release agent, wherein the addition amount of the wetting agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dispersing agent is 0.1-1.5 wt% of the dry weight of the paste containing the glue, the addition amount of the organic silicon defoaming agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dimethyl silicon oil release agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the wetting agent is any one of alkyl sulfate, sulfonate, fatty acid ester sulfate, carboxylic acid soap and phosphate ester anionic surfactant or polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene segmented copolymer nonionic surfactant, and the dispersing agent is phosphate ester dispersing agent, ethoxy compound dispersing agent, polyacrylate dispersing agent, polyester dispersing agent, any one of polyether dispersant, polyolefin dispersant, sodium carbonate, sodium orthophosphate, polyethyleneimine or herring oil.
Further, in the step 3, the weight ratio of water to ethanol in the polyvinyl alcohol glue is 3-10: 1, the solid content of polyvinyl alcohol is 5-15 wt%; the water-soluble resin solution is one or more of water-soluble polyimide resin solution, water-soluble epoxy resin solution and water-soluble phenolic resin solution, and the solid content of the water-soluble resin solution is 40-60 wt%; the dry weight of the mixed glue accounts for 5-15 wt% of the dry weight of the glue-containing slurry;
further, the mold in the step 4 is cylindrical, square or polygonal; the densification treatment is cold isostatic pressing, and the pressure is 5-50 MPa; the sintering is specifically that the blank body is placed in an oven, the temperature is firstly raised to 75 ℃ and is kept for 60min, then the temperature is raised to 115 ℃ and is kept for 90min, then the temperature is raised to 150-180 ℃ and is kept for 60min, and finally the temperature is raised to 180-230 ℃ and is kept for 30 min. After sintering, the polyvinyl alcohol glue is thermally decomposed and carbonized to form uniform capillary micropores, the function of gel blank forming is completed, at the moment, the water-soluble resin is thermally cured to play the role of a pellet resin binding agent, and the polished pellet semi-finished product with fine pores is prepared.
Further, in the step 5, the surface smoothing treatment is to stick the semi-finished product of the polishing pill on a base plate, the base plate is placed on a plane grinding machine, the surface of the semi-finished product of the polishing pill is ground to be flat by a #100 ceramic-based grinding wheel, the polishing solution is acidic polishing solution, alkaline polishing solution or water, the acidic polishing solution and the alkaline grinding solution are respectively prepared by adding an acidic pH regulator or an alkaline pH regulator into the water, the acidic pH regulator is dilute hydrochloric acid, the pH value regulating range is 2-6, the alkaline pH regulator is potassium hydroxide, the pH value regulating range of the alkaline polishing solution is 8-12, the dissolving capacity of the soluble aluminum nitride filler is improved, and the self-sharpening effect of the pill is enhanced.
The polishing pill obtained by the preparation method is used for polishing a workpiece, and the processing method comprises the steps of sticking the workpiece on a ceramic base plate by using wax, sticking the polishing pill on a cast iron plate, placing the cast iron plate on the base plate of a plane polishing machine, clamping the ceramic base plate by using a clamp at the rotating speed of 50-150 rpm, pneumatically pressurizing by using the clamp at the pressure of 1-20 Mpa at the polishing temperature of 30-38 ℃ for 10-30 min.
The invention has the following beneficial effects: the traditional gel grinding tool adopts glue direct gel as a binding agent to consolidate the grinding material, and the grinding tool is manufactured by mixing the liquid gel of the polyvinyl alcohol and the water-soluble resin, so that the internal defects of the grinding tool with the abrasive particles are reduced, and the uniformity of the grinding tool tissue is ensured. The two resins have different functions in the process of forming the polishing pill, firstly, a gel blank is formed by utilizing the low-temperature physical gelling capacity of polyvinyl alcohol, the polyvinyl alcohol is sintered and carbonized at high temperature, meanwhile, the water-soluble resin is solidified to be used as a bonding agent of the polishing pill, a large number of capillary micropores are generated after the polyvinyl alcohol is carbonized, compared with a hole generated by directly forming powder and adding a pore-forming agent, the capillary micropores generated in the pill by the method are through micropores, have strong water absorption capacity, and are beneficial to improving the friction force, storing polishing solution and discharging chips.
Traditional abrasive tools improve self-sharpening by adding "soluble", "decomposable" or "electrolytic" fillers, which swell and do not guarantee selective self-sharpening of the surface material, which have the disadvantage of a complex process. According to the invention, the aluminum nitride soluble powder filler with the water-resistant nano silicon dioxide coating coated on the surface is added, silicon dioxide on the surface of the aluminum nitride on the surface layer of the pill is worn, the aluminum nitride is hydrolyzed by polishing solution, the surface bonding strength is reduced, the passivated abrasive material falls off, and a new abrasive material is exposed, so that the self-sharpening property is maintained; because the capillary micropores in the polishing pill have water absorption capacity, the aluminum nitride coated with the water-resistant nano silicon dioxide coating in the pill can avoid direct hydrolysis and maintain the strength of the pill matrix, and therefore, the polishing pill has the advantages of stable internal structure and good surface self-sharpening property.
Drawings
FIG. 1 is a schematic view of the internal structure of a sol-gel polishing pellet;
FIG. 2 SEM surface topography of the sol-gel polished pellet prepared in example 1;
FIG. 3 is a schematic view of a polishing mode;
FIG. 4 is a graph of the surface topography of a polished germanium mirror white light interference surface of a polished pellet prepared in example 1;
FIG. 5 is a graph of material removal rate versus polishing time for gel polishing pellets and hot press polishing pellets;
FIG. 6 shows the surface roughness and material removal rate of a germanium plane lens after being processed by polishing pills under the condition of different diamond abrasive content;
FIG. 7 is a graph showing the relationship between the pH of the polishing liquid and the wear rate of the polishing pellet.
Detailed Description
The invention provides a sol-gel polishing pellet added with a soluble filler with a water-resistant coating and a preparation method thereof, wherein the internal structure schematic diagram of the sol-gel polishing pellet is shown in figure 1. The grinding tool is manufactured by using polyvinyl alcohol and water-soluble resin liquid gel, the problem of uneven powder forming and dispersion is avoided, a gel biscuit is formed by utilizing the physical gel capability of the polyvinyl alcohol, the sintering and carbonization are carried out, the sintering and curing temperature of the water-soluble resin is also the carbonization temperature of the polyvinyl alcohol, a large number of through capillary micropores are generated after the carbonization of the polyvinyl alcohol, the gel biscuit has good water absorption capability, an aluminum nitride soluble powder filler with a water-resistant nano silicon dioxide coating coated on the surface is added, the silicon dioxide on the surface of the aluminum nitride on the surface layer of the pill piece is worn, the aluminum nitride is hydrolyzed by polishing solution, the surface bonding strength is reduced, the passivated grinding material falls off, and new grinding material is; the aluminum nitride coated with the water-resistant nano silicon dioxide coating in the pellet can avoid direct hydrolysis, maintain the strength of the pellet substrate, effectively reduce the consumption of the abrasive and improve the service life and the utilization rate of the abrasive in the polishing tool.
Example 1:
step 1: preparation of aluminum nitride powder with water-resistant film layer on surface
Mixing 100g of aluminum nitride powder with the grain diameter of 1 micron and 1kg of absolute ethyl alcohol by weight, uniformly stirring, and heating to 40 ℃ under the condition of water bath to obtain an aluminum nitride ethanol dispersion liquid; simultaneously adding 80g of tetraethyl orthosilicate (TEOS) diluted by 600g of absolute ethyl alcohol, 100g of ammonia water diluted by 600g of absolute ethyl alcohol and 100g of water into the aluminum nitride ethanol dispersion liquid, controlling the dropping speed to be 2 drops/second, reacting at 40 ℃ for 6 hours after the dropping is finished, stopping the reaction, carrying out vacuum filtration, washing the product for 3 times by using absolute ethyl alcohol, naturally drying the obtained product at room temperature for 12 hours, calcining at 300 ℃ for 2 hours after the drying, cooling, and sieving by a 200-mesh sieve to obtain silicon dioxide coated aluminum nitride powder; since the silica has water resistance, the aluminum nitride powder having a water-resistant film layer on the surface is obtained; step 2: preparing a suspension: according to weight, 300g of diamond powder with the particle size of 2.5 microns, 100g of silicon dioxide coated aluminum nitride powder, 500g of electrolytic copper powder with the particle size of 400 meshes, 50g of copper-coated graphite, 50g of cryolite powder, 80g of zinc oxide, 150g of barium sulfate, 70g of aluminum oxide powder, 15g of polyoxyethylene alkylphenol ether wetting agent, 20g of polyethylene imine, 10g of organic silicon defoamer and 10g of dimethyl silicone oil release agent are added into 1200g of water, the mixture is dispersed by using a planetary ball mill after mixing, and zirconium oxide microspheres with the particle size of 3mm are selected as dispersion media to prepare suspension.
And step 3: preparing a sizing agent containing glue: under the condition of 90 ℃ water bath, 10g of polyvinyl alcohol is dissolved in a mixed solvent of 80g of water and 10g of ethanol to obtain 100g of polyvinyl alcohol glue with the solid content of 10 wt%; adding 300g of water-soluble polyimide resin liquid with the solid content of 40 wt% into the polyvinyl alcohol glue to obtain 400g of mixed glue, adding the mixed glue into the suspension prepared in the step 2 while stirring, and dispersing for 1 hour by using a planetary ball mill after mixing and stirring to obtain glue-containing slurry;
and 4, step 4: preparing a polishing pill with fine pores: pouring 15g of the prepared slurry containing the colloid into a cylindrical mold with the diameter of 12mm, freezing for 2 hours at the temperature of-15 ℃, naturally drying for 10 hours after unfreezing, taking out a blank body from the mold, carrying out cold isostatic pressing under the condition of 20MPa, putting into an oven for baking for 24 hours at the temperature of 45 ℃, drying, heating the pellet blank body to 180 ℃ for sintering, wherein the temperature rise curve is that the temperature is firstly raised to 75 ℃ for 1 hour, then raised to 115 ℃ for 1.5 hours, then raised to 180 ℃ for 1 hour, finally raised to 230 ℃ for 30 minutes, polyvinyl alcohol glue is thermally decomposed to form uniform capillary micropores, water-soluble polyimide resin is solidified to prepare a polished pellet semi-finished product with a rough surface, then a surface of the polished pellet semi-finished product is ground to be flat by using a flat grinder to obtain a polished pellet finished product, and the prepared sol-gel polished pellet is shown in figure 2, and the diamond is diamond, The filler and the electrolytic copper powder are uniformly distributed in the polishing pellet. The tensile strength of the obtained polishing pellet tablet reaches 25MPa, the hardness reaches 60 (Shore hardness), and the elongation at break is 150%.
Example 2:
polishing and processing the germanium plane lens:
a schematic diagram of a polishing mode is shown in fig. 3, a germanium plane lens with the diameter of 100mm is pasted on a ceramic base disc by wax, the plane lens is firstly ground by a diamond polishing solution with the diameter of 10 microns and a silicon carbide grinding disc, the surface roughness reaches 25nm, a pellet prepared in example 1 is pasted on a cast iron disc, the diameter of the cast iron disc is 200mm, the surface of the pellet is flattened on a plane grinder, the vertical error is less than 2 microns, the cast iron disc is placed on the plane polisher base disc, the ceramic base disc is clamped by a clamp, the rotation speed of the polishing disc is 100rpm, the clamp is pneumatically pressurized, the pressure is 5Mpa, an acid polishing solution is added on the surface of the pellet in the polishing process, the pH value is 5, the flow is 100ml/min, the pH value is adjusted to be 5 by adding an acid pH regulator, namely dilute hydrochloric acid into water, the dissolving capacity of soluble aluminum nitride filler is improved, the polishing temperature is controlled at 30 ℃, and the polishing time is, after polishing, white light observation and analysis are carried out on the surface of the germanium planar lens, the surface appearance is as shown in figure 4, and the surface roughness reaches 7.716 nm.
Example 3:
the operation is basically the same as that of the example 1, except that in the step 2, the amount of the silicon dioxide coated aluminum nitride powder is increased to 150g, the strength of the pellet matrix can be still maintained under the dry condition after sintering, the tensile strength reaches 25Mpa, the breaking strength is 60Mpa, the elongation at break is 145%, after soaking in water for 1 hour, the tensile strength is 23Mpa, the breaking strength is 55Mpa, and after drying, the weight is weighed and reduced by 0.5 g; after 2 hours, the tensile strength is 22Mpa, the breaking strength is 53Mpa, the strength is not obviously reduced, and after drying, the weight is weighed and reduced by 0.4 g.
After the surface of the pill is rubbed, the original weight of the pill is weighed, the pill is soaked in water for 1 hour, the integral tensile strength of the pill is 23Mpa, the breaking strength is 55Mpa, after drying, the weight is weighed, the weight is reduced by 1g, and the surface of the pill is favorable for hydrolysis of the surface layer aluminum nitride after the surface of the pill is rubbed.
Example 4:
the operation is substantially the same as that of example 1, except that the amount of the 10 wt% polyvinyl alcohol glue in the mixed glue in step 3 is increased to 200g, and since the polyvinyl alcohol is carbonized after being sintered, a large number of capillary micropores with good water absorption capacity can be generated, the friction is enhanced, the removal efficiency is improved, but the wear rate is also improved.
As a comparative experiment, the operation was substantially the same as that of example 1 except that the water-soluble polyimide resin solution was added to 500g, and after curing, the polishing pellet had a large amount of resin binder, improved abrasion resistance, reduced effect of aluminum nitride as a hydrolyzable filler, and had a surface glazing phenomenon and a reduced removal force after 5 hours of use.
Example 5:
in the present example, a comparative experiment was performed on the gel polishing pellet in example 1 and a commercially available 2.5 μm diamond polishing pellet, the polishing process was substantially the same as that of example 2, the commercially available pellet was subjected to a powder mixing-hot pressing process, and the change of the material removal rate with time was observed in the experiment, as shown in fig. 5, it can be seen from the figure that, in the initial stage, the hot pressing pellet had a higher material removal rate than the gel pellet, because of the resin network structure inside the gel pellet, the strength of the gel pellet was higher under the condition of having an equivalent amount of resin binder, the abrasive was difficult to fall off, after a long time of polishing use, the aluminum nitride filler on the surface of the gel pellet was hydrolyzed, the binding force was reduced, the abrasive fell off, the pellet was self-sharpened, and the stability of material removal was maintained, so the gel polishing pellet had the characteristics of high strength and stable material removal rate.
Example 6:
the purpose of this implementation was to test the effect of different diamond grit sizes on the efficiency of lapping and polishing in the polishing pellets.
The operation was substantially the same as in example 1, except that polishing pellets having diamond grit sizes of W0.5, W1.5, W2.5, W3.5, W5, and W7 were prepared, the germanium flat lens was polished on a nanopolli 100 lapping and polishing machine, and the surface roughness and material removal rate of the germanium flat lens after processing by the gel diamond pellets under the conditions of different diamond grit contents were measured, as shown in fig. 6, it can be seen from the figure that the surface roughness and material removal rate after processing the workpiece were both improved with the increase in the diamond grit size, different surface roughnesses could be obtained by selecting different diamond grit sizes, and the polishing efficiency decreased at a fast rate with the diamond grit size of less than 2.5 μm, and the surface quality did not change significantly.
Example 7:
in this example, the pH of the polishing solution was changed based on example 2, and the effect of the pH on the wear rate of the pellets was observed. It can be seen from FIG. 7 that increasing the pH of the polishing slurry increases the wear rate of the polished pellet because the pH increases and the hydrolysis rate of aluminum nitride increases, which is beneficial to the self-sharpening of the polished pellet, but too high a wear rate is not beneficial to the maintenance of the surface shape of the pellet.
Example 8:
the operation is basically the same as that of the embodiment 1, except that the water-soluble polyimide resin is changed into the water-soluble phenolic resin, in the step 3, the sintering temperature is changed into 180 ℃, the sintering temperature rise curve is that the temperature is firstly raised to 75 ℃ and preserved for 1 hour, then raised to 115 ℃ and preserved for 1.5 hours, and finally raised to 180 ℃ and preserved for 30 minutes, so that the phenolic resin bonding agent polishing pill piece is obtained, the tensile strength of the obtained polishing pill piece reaches 22MPa, the hardness reaches 56 (Shore hardness), and the surface roughness of the polishing germanium plane mirror can reach below 10 nm.
Claims (7)
1. A method for preparing self-trimming polished pellets to which a soluble filler having a water-resistant coating is added, characterized by comprising the steps of:
step 1: preparing water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface;
step 2: dispersing diamond powder, water-resistant aluminum nitride powder, electrolytic copper powder, a filler and an additive in water to prepare a suspension;
and step 3: under the condition of 90 ℃ water bath, dissolving polyvinyl alcohol in a mixed solvent of water and ethanol to obtain polyvinyl alcohol glue, adding water-soluble resin liquid into the polyvinyl alcohol glue to obtain mixed glue, wherein the weight ratio of the polyvinyl alcohol glue to the water-soluble resin liquid in the mixed glue is 1: 1-6, adding the mixed glue into the suspension prepared in the step 2, and mixing to obtain glue-containing slurry;
and 4, step 4: pouring the slurry containing the rubber into a mold, freezing for 1-3 hours at the temperature of-25 to-15 ℃, naturally drying for 5-10 hours after thawing, taking out a blank from the mold, performing densification treatment, drying for 24-48 hours at the temperature of 45-65 ℃, and then sintering to prepare a semi-finished product of the polishing pellet with the micro pores;
and 5: and (4) pasting the semi-finished product of the polishing pellet on a base plate for surface smoothing treatment to obtain the polishing pellet, and further polishing the workpiece.
2. The method for preparing self-trimming polished pellet added with soluble filler with water-resistant coating according to claim 1, wherein the step 1 is specifically as follows:
mixing 1-10 parts by weight of aluminum nitride powder and 50 parts by weight of absolute ethyl alcohol, and uniformly stirring at 40 ℃ to obtain an aluminum nitride ethanol dispersion liquid; dropwise adding 3-6 parts of tetraethoxysilane diluted by 30 parts of absolute ethyl alcohol, 4-6 parts of ammonia water diluted by 30 parts of absolute ethyl alcohol and 5 parts of water into the aluminum nitride ethanol dispersion liquid at the dropping speed of 1-2 drops/second, then carrying out gel reaction for 6 hours at the temperature of 35-45 ℃, carrying out vacuum filtration, washing the product for 3 times by using the absolute ethyl alcohol, naturally drying the obtained product for 12-24 hours at the room temperature, then calcining for 2 hours at the temperature of 300 ℃, cooling and then sieving by using a 200-mesh sieve to obtain the water-resistant aluminum nitride powder with the silicon dioxide film layer on the surface.
3. The method for preparing self-trimming polished pellet added with soluble filler with water-resistant coating according to claim 1, wherein the step 2 is specifically as follows:
adding 5-10 parts by weight of 0.5-5 micron diamond powder, 1-3 parts by weight of water-resistant aluminum nitride powder, 10-30 parts by weight of 200-1000 mesh electrolytic copper powder, 5-10 parts by weight of filler and 0.5-2 parts by weight of additive into 20-50 parts by weight of water, and dispersing by using a planetary ball mill, wherein a dispersion medium is zirconium oxide microspheres to prepare a suspension; the filler is any one or more of copper-coated graphite, talcum powder, cryolite, cerium oxide, aluminum oxide powder, calcium carbonate, calcium oxide, zinc oxide, barium sulfate, magnesium oxide, molybdenum disulfide and silicon carbide; the additive is prepared by mixing a wetting agent, a dispersing agent, an organic silicon defoaming agent and a dimethyl silicon oil release agent, wherein the addition amount of the wetting agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dispersing agent is 0.1-1.5 wt% of the dry weight of the paste containing the glue, the addition amount of the organic silicon defoaming agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the addition amount of the dimethyl silicon oil release agent is 0.1-1 wt% of the dry weight of the paste containing the glue, the wetting agent is any one of alkyl sulfate, sulfonate, fatty acid ester sulfate, carboxylic acid soap and phosphate ester anionic surfactant or polyoxyethylene alkylphenol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene polyoxypropylene segmented copolymer nonionic surfactant, and the dispersing agent is phosphate ester dispersing agent, ethoxy compound dispersing agent, polyacrylate dispersing agent, polyester dispersing agent, any one of polyether dispersant, polyolefin dispersant, sodium carbonate, sodium orthophosphate, polyethyleneimine or herring oil.
4. The method for preparing self-trimming polishing pellets added with the soluble filler with the water-resistant coating according to claim 1, wherein the weight ratio of water to ethanol in the polyvinyl alcohol glue in the step 3 is 3-10: 1, and the solid content of the polyvinyl alcohol is 5-15 wt%; the water-soluble resin solution is one or more of water-soluble polyimide resin solution, water-soluble epoxy resin solution and water-soluble phenolic resin solution, and the solid content of the water-soluble resin solution is 40-60 wt%; the dry weight of the mixed glue accounts for 5-15 wt% of the dry weight of the glue-containing slurry.
5. The method for preparing self-trimming polished pellets with soluble fillers added with water-resistant coatings according to claim 1, wherein the mold in step 4 is cylindrical, square or polygonal; the densification treatment is cold isostatic pressing, and the pressure is 5-50 MPa; the sintering is specifically that the blank body is placed in an oven, the temperature is firstly raised to 75 ℃ and is kept for 60min, then the temperature is raised to 115 ℃ and is kept for 90min, then the temperature is raised to 150-180 ℃ and is kept for 60min, and finally the temperature is raised to 180-230 ℃ and is kept for 30 min.
6. The method according to claim 1, wherein the surface smoothing treatment in step 5 is performed by attaching the semi-finished product of the polishing pellet to a base plate, placing the base plate on a flat grinder, and grinding the surface of the semi-finished product of the polishing pellet with a 100 # ceramic-based grinding wheel, wherein the polishing solution is an acidic polishing solution, an alkaline polishing solution or water, the acidic polishing solution and the alkaline polishing solution are prepared by adding an acidic pH regulator or an alkaline pH regulator to water, respectively, the acidic pH regulator is dilute hydrochloric acid, the pH value is 2-6, the alkaline pH regulator is potassium hydroxide, and the alkaline polishing solution has a pH value of 8-12.
7. A self-trimming polished pellet added with a soluble filler having a water-resistant coating prepared by the method of any one of claims 1 to 6.
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| US6669747B2 (en) * | 2002-02-15 | 2003-12-30 | Master Chemical Corporation | Grinding wheel with titanium aluminum nitride and hard lubricant coatings |
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| CN101905439B (en) * | 2009-06-04 | 2012-07-04 | 宋健民 | Polishing pad with internal in-situ generated gap and gap generating method |
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| CN106956212B (en) * | 2017-03-17 | 2018-12-04 | 衢州学院 | A kind of aluminium nitride chip polishing method using chemical polishing solution and ceramic polished disk |
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