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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- aluminum nitride
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- 238000005498 polishing Methods 0.000 title claims abstract description 100
- 239000008188 pellet Substances 0.000 title claims abstract description 92
- 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 28
- 239000011248 coating agent Substances 0.000 title claims abstract description 19
- 238000000576 coating method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 46
- 239000003292 glue Substances 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 32
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 32
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 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 28
- 239000007788 liquid Substances 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 20
- 239000002270 dispersing agent Substances 0.000 claims description 19
- 239000010432 diamond Substances 0.000 claims description 18
- 229910003460 diamond Inorganic materials 0.000 claims description 18
- 239000011148 porous material Substances 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- -1 polyoxyethylene Polymers 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000080 wetting agent Substances 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 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
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 229920001296 polysiloxane Polymers 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 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
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 239000009719 polyimide resin Substances 0.000 claims description 4
- 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
- 238000009694 cold isostatic pressing 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
- 229940008099 dimethicone Drugs 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 3
- 239000002612 dispersion medium Substances 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
- 239000003921 oil 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
- 238000010979 pH adjustment Methods 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 239000011265 semifinished product Substances 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
- 238000010257 thawing Methods 0.000 claims description 3
- 239000011787 zinc oxide Substances 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
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 229920001400 block copolymer Polymers 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
- 238000000280 densification Methods 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 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
- 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
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 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
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000000344 soap Substances 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
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 125000005526 alkyl sulfate group Chemical group 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 239000011230 binding agent Substances 0.000 abstract description 9
- 230000007062 hydrolysis Effects 0.000 abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 7
- 238000003763 carbonization Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- TWYVVGMYFLAQMU-UHFFFAOYSA-N gelgreen Chemical compound [I-].[I-].C1=C(N(C)C)C=C2[N+](CCCCCC(=O)NCCCOCCOCCOCCCNC(=O)CCCCC[N+]3=C4C=C(C=CC4=CC4=CC=C(C=C43)N(C)C)N(C)C)=C(C=C(C=C3)N(C)C)C3=CC2=C1 TWYVVGMYFLAQMU-UHFFFAOYSA-N 0.000 abstract description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 239000003082 abrasive agent Substances 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 229910052732 germanium Inorganic materials 0.000 description 8
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 8
- 230000003746 surface roughness Effects 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 229910001018 Cast iron Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000003002 pH adjusting agent Substances 0.000 description 4
- 239000006187 pill Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
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- 230000007774 longterm Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
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- 150000008051 alkyl sulfates Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
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- 239000002113 nanodiamond Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
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- 238000003980 solgel method Methods 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- 229920002554 vinyl polymer Polymers 0.000 description 1
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
本发明公开了一种添加具有耐水涂层可溶填料的自修整抛光丸片及其制备方法,使用耐水氮化铝粉末与金刚石微粉、电解铜粉、填料、添加剂混合,加入聚乙烯醇、水、乙醇、水溶性树脂制备得到的混合胶水,得到浆料。通过聚乙烯醇和酚醛混合树脂液凝胶制作的磨具利用了聚乙烯醇具有的物理凝胶能力,形成凝胶素坯,高温下聚乙烯醇烧结碳化,水溶性树脂固化作为抛光丸片结合剂,聚乙烯醇碳化后产生大量毛细贯通微孔,对水的吸收能力强,添加了具有耐水涂层的可溶氮化铝,丸片表层氮化铝颗粒耐水涂层磨去后,氮化铝水解,强度下降,具有表层自修锐的作用,而丸片内部氮化铝耐水涂层保护,保证丸片整体强度。
The invention discloses a self-dressing polishing pellet with water-resistant coating soluble filler and a preparation method thereof. , ethanol, and the mixed glue prepared from the water-soluble resin to obtain a slurry. The abrasive tool made of polyvinyl alcohol and phenolic mixed resin lyogel utilizes the physical gel ability of polyvinyl alcohol to form a gel green body. At high temperature, polyvinyl alcohol is sintered and carbonized, and the water-soluble resin is cured as a polishing pellet binder. , After carbonization of polyvinyl alcohol, a large number of capillary through-holes are generated, which has a strong ability to absorb water. Soluble aluminum nitride with a water-resistant coating is added. After the water-resistant coating of the aluminum nitride particles on the surface of the pellet is removed, Hydrolysis reduces the strength, and has the effect of self-sharpening of the surface layer, and the inner aluminum nitride water-resistant coating of the pellets is protected to ensure the overall strength of the pellets.
Description
技术领域technical field
本发明属于精密加工研磨抛光领域,涉及一种添加具有耐水涂层可溶填料的溶胶凝胶抛光丸片及其制备方法。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.
背景技术Background technique
光学加工中,一般在高速精磨中,经过了一道精磨,二道超精磨之后,虽然具有一定光滑和规则的表面形状,但它还不完全透明而且表面形状也不是所要求的,还需要对元件进行抛光,来达到需要的表面光洁度,这时候就需要用抛光片进行高速精磨,抛光是精磨以后的一个主要工序。因此抛光的目的即为:(1)去除精磨的破坏层达到规定的外观限度要求;(2)精修面形,达到图面规定的曲率半径R值,满足光圈局部允差的要求。In optical processing, generally in high-speed fine grinding, after one fine grinding and two super fine grinding, although it has a certain smooth and regular surface shape, it is not completely transparent and the surface shape is not required. The components need to be polished to achieve the required surface finish. At this time, high-speed fine grinding with a polishing sheet is required. Polishing is a major process after fine grinding. Therefore, the purpose of polishing is to: (1) remove the finely ground damage layer to meet the specified appearance limit requirements; (2) finely trim the surface shape to achieve the specified curvature radius R value of the drawing surface and meet the requirements of the local tolerance of the aperture.
但是传统磨具制作方法为粉料混合→过筛→干燥→压制→烧结,容易出现物相团聚的问题,如何减少磨粒磨具内部缺陷、保证磨具组织的均匀性是一个迫在眉睫要解决的问题,因为内部组织的均匀性直接影响抛光性能。同时传统磨具存在长时间使用,磨具发生钝化的问题,因此,需要设计抛光丸片具有自修锐的功能。However, the traditional abrasive tool manufacturing method is powder mixing → sieving → drying → pressing → sintering, which is prone to the problem of phase agglomeration. How to reduce the internal defects of the abrasive tool and ensure the uniformity of the abrasive tool structure is an urgent problem to be solved. problem, because the uniformity of the internal structure directly affects the polishing performance. At the same time, the traditional abrasive tool has the problem of passivation after long-term use. Therefore, it is necessary to design the polishing pellet with the function of self-sharpening.
公开号为106944939B的发明专利公开了一种添加可溶性树脂材料的自修锐超硬微细磨具丸片及其制备方法,通过研磨液溶解磨具表层的“可溶性”树脂材料,在结合剂间形成孔隙,起到降低粘结剂强度和其对周围磨粒的把持力,从而达到自动在线可控修锐磨具的目的,但是该方法容易对丸片内部产生树脂溶解,导致强度下降;公开号为106956222B的发明专利公开了一种采用橡胶结合剂的多孔海绵复合金刚石研磨丸片及其制备方法,含有连续气孔的橡胶弹性复合配合物与复合颗粒结合为一体具有海绵状细小连续气孔组织的丸片,由于橡胶硬度低,面型难以保证;公开号为104944956A的发明专利公开了一种基于凝胶反应的多晶纳米金刚石磨具制备方法,该方法采用聚丙烯晴进行凝胶,硬度高,适用于研磨阶段;公开号为108081159A的发明专利公开了一种聚乙烯醇缩醛树脂磨具有机凝胶成型方法,该凝胶方法无法适用于水性体系,同时采用单一树脂,无法碳化形成毛细微孔。Invention patent publication No. 106944939B discloses a self-sharpening superhard micro abrasive pellet with soluble resin material and a preparation method thereof. The "soluble" resin material on the surface of the abrasive tool is dissolved by the grinding liquid, and pores are formed between the binders. , which can reduce the strength of the binder and its holding force on the surrounding abrasive particles, so as to achieve the purpose of automatic online controllable sharpening of abrasive tools, but this method is easy to dissolve the resin inside the pellet, resulting in a decrease in strength; the publication number is The invention patent of 106956222B discloses a porous sponge composite diamond grinding pellet using a rubber binder and a preparation method thereof. The rubber elastic composite compound containing continuous pores and the composite particles are combined into a pellet with a sponge-like fine continuous pore structure. , due to the low rubber hardness, the surface shape is difficult to guarantee; the invention patent publication No. 104944956A discloses a preparation method of polycrystalline nano-diamond abrasive tool based on gel reaction, the method uses polyacrylonitrile for gel, high hardness, suitable for In the grinding stage; the invention patent publication No. 108081159A discloses a polyvinyl acetal resin grinding method for organogel molding, the gel method cannot be applied to water-based systems, and a single resin is used at the same time, which cannot be carbonized to form micropores .
为解决金刚石抛光丸片物相团聚、造毛细孔、自修锐的问题,本发明采用复合树脂凝胶成型,一种树脂烧结固化,另一种树脂碳化产生毛细微孔;添加耐水涂层填料,在实现表面可溶自锐的条件下,基体强度得到保证。In order to solve the problems of phase agglomeration, capillary formation and self-sharpening of diamond polishing pellets, the present invention adopts composite resin gel molding, one resin is sintered and solidified, and the other resin is carbonized to generate capillary pores; adding water-resistant coating filler, Under the condition that the surface is soluble and self-sharpening, the matrix strength is guaranteed.
发明内容SUMMARY OF THE INVENTION
本发明采用复合树脂制备抛光丸片,首先通过聚乙烯醇低温凝胶方法成形抛光丸片素坯,再通过烧结,使水溶性树脂固化作为抛光丸片结合剂,而聚乙烯醇碳化分解,形成贯通式毛细微孔,该工艺优势有:(1)溶胶-凝胶法制备的抛光丸片成分分布均匀、没有团聚,适合精密抛光丸片的制备;(2)丸片内部有大量贯通的毛细微孔,有利于增强吸附势能,提高摩擦力,同时有利于排屑。同时添加具有耐水涂层的氮化铝粉末,在表层氮化铝粉末摩擦分解,提高自锐性的作用下,内部耐水氮化铝粉末作为填料,不分解,保证抛光丸片强度。In the present invention, composite resin is used to prepare polishing pellets. First, the polishing pellets are formed by a polyvinyl alcohol low-temperature gel method, and then sintered to solidify the water-soluble resin as a polishing pellet binding agent, and the polyvinyl alcohol is carbonized and decomposed to form Through capillary pores, the advantages of this process are: (1) The polishing pellets prepared by the sol-gel method have uniform distribution of components and no agglomeration, which is suitable for the preparation of precision polishing pellets; (2) There are a large number of through capillaries inside the pellets. The micropores are beneficial to enhance the adsorption potential energy, improve the friction force, and at the same time facilitate chip removal. At the same time, the aluminum nitride powder with water-resistant coating is added. Under the action of friction decomposition of the surface aluminum nitride powder to improve self-sharpening, the internal water-resistant aluminum nitride powder is used as a filler, which does not decompose and ensures the strength of the polishing pellet.
为实现上述目的,本发明采用如下技术方案:To achieve the above object, the present invention adopts the following technical solutions:
步骤1:制备表面具有二氧化硅膜层的耐水氮化铝粉末;Step 1: prepare a water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface;
步骤2:将金刚石粉末、耐水氮化铝粉末、电解铜粉、填料、添加剂分散在水中,制备得到悬浮液;Step 2: disperse diamond powder, water-resistant aluminum nitride powder, electrolytic copper powder, filler and additives in water to prepare a suspension;
步骤3:在90℃水浴条件下,将聚乙烯醇溶于水和乙醇的混合溶剂中得到聚乙烯醇胶水,在聚乙烯醇胶水中添加水溶性树脂液得到混合胶水,所述混合胶水中的聚乙烯醇胶水与水溶性树脂液的重量比为1:1~6,将混合胶水加入到步骤2制备的悬浮液中,混合得到含胶浆料;乙醇的作用是防止水在低温条件下发生水结晶现象;Step 3: Dissolving polyvinyl alcohol in a mixed solvent of water and ethanol under the condition of a 90° C. water bath to obtain polyvinyl alcohol glue, adding water-soluble resin liquid to the polyvinyl alcohol glue to obtain a mixed glue, in which the mixed glue is The weight ratio of the polyvinyl alcohol glue to the water-soluble resin liquid is 1:1 to 6, and the mixed glue is added to the suspension prepared in step 2, and mixed to obtain a glue-containing slurry; the function of ethanol is to prevent the occurrence of water under low temperature conditions water crystallization;
步骤4:将含胶浆料倒入模具中,置于-25~-15℃温度下冷冻1~3小时,解冻后自然干燥5~10小时,从模具中取出坯体,致密化处理,在45~65℃条件下干燥24~48小时,然后烧结,制备得到具有微细毛孔的抛光丸片半成品;Step 4: Pour the glue-containing slurry into the mold, freeze it at a temperature of -25 to -15 ° C for 1 to 3 hours, and dry it naturally for 5 to 10 hours after thawing. Drying at 45-65°C for 24-48 hours, and then sintering to prepare semi-finished polishing pellets with fine pores;
步骤5:将抛光丸片半成品贴在基盘上进行表面修平处理,得到抛光丸片,进一步对工件进行抛光加工。Step 5: The semi-finished product of the polishing pellet is attached to the base plate for surface leveling treatment to obtain the polishing pellet, and the workpiece is further polished.
进一步的,所述的步骤1具体为:Further, the step 1 is specifically:
按重量计,将1~10份氮化铝粉末和50份无水乙醇混合,在40℃条件下搅拌均匀,得到氮化铝乙醇分散液;将30份无水乙醇稀释的3~6份正硅酸乙酯以及用30份无水乙醇稀释的4~6份氨水和5份水滴加到氮化铝乙醇分散液中,滴加速度为1~2滴/秒,然后在35~45℃条件下凝胶反应6小时,真空抽滤,用无水乙醇洗涤产物3次,将得到的产物置于室温条件下自然干燥12~24小时,然后在300℃条件下煅烧2小时,冷却后过200目筛,得到表面具有二氧化硅膜层的耐水氮化铝粉末;氮化铝可在水中发生水解,在碱性或酸性条件下,可调节氮化铝水解速度,包覆一层二氧化硅可防止抛光丸片内部氮化铝发生水解,而抛光丸片表面层氮化铝在摩擦作用下,包覆的二氧化硅膜擦拭去除,引起表层氮化铝水解,结合力下降,达到自锐的效果;By weight, 1-10 parts of aluminum nitride powder and 50 parts of anhydrous ethanol are mixed, and stirred evenly at 40 ° C to obtain an ethanol dispersion of aluminum nitride; Ethyl silicate, 4-6 parts of ammonia water and 5 parts of water diluted with 30 parts of absolute ethanol are added dropwise to the ethanol dispersion of aluminum nitride at a rate of 1-2 drops/second, and then at 35-45 °C The gel was reacted for 6 hours, vacuum filtered, the product was washed with absolute ethanol 3 times, the obtained product was dried at room temperature for 12 to 24 hours, then calcined at 300 ° C for 2 hours, and passed through 200 mesh after cooling. sieve to obtain a water-resistant aluminum nitride powder with a silicon dioxide film layer on the surface; aluminum nitride can be hydrolyzed in water, under alkaline or acidic conditions, the hydrolysis speed of aluminum nitride can be adjusted, and a layer of silicon dioxide can be To prevent the hydrolysis of aluminum nitride inside the polishing pellet, and under the action of friction, the coated silicon dioxide film on the surface of the polishing pellet is wiped off, causing the surface aluminum nitride to hydrolyze, and the bonding force decreases, achieving self-sharpening. Effect;
进一步的,所述步骤2具体为:Further, the step 2 is specifically:
按重量计,将5~10份0.5~5微米的金刚石粉末、1~3份耐水氮化铝粉末、10~30份200~1000目的电解铜粉、5~10份填料和0.5~2份添加剂加入到20~50份水中,采用行星式球磨机进行分散,分散介质选用氧化锆微球,制备得到悬浮液;所述的填料为铜包石墨、滑石粉、冰晶石、氧化铈、铝氧粉、碳酸钙、氧化钙、氧化锌、硫酸钡、氧化镁、二硫化钼、碳化硅中的任意一种或者几种;所述的添加剂由湿润剂、分散剂、有机硅消泡剂和二甲基硅油脱模剂混合得到,湿润剂添加量为含胶浆料干重0.1~1wt%,分散剂添加量为含胶浆料干重0.1~1.5wt%,有机硅消泡剂添加量为含胶浆料干重0.1~1wt%,二甲基硅油脱模剂添加量为含胶浆料干重0.1~1wt%,所述的润湿剂选用烷基硫酸盐、磺酸盐、脂肪酸、脂肪酸酯硫酸盐、羧酸皂类、磷酸酯阴离子型表面活性剂,或者聚氧乙烯烷基酚醚、聚氧乙烯脂肪醇醚、聚氧乙烯聚氧丙烯嵌段共聚物非离子型表面活性剂中的任意一种,所述的分散剂为磷酸酯型分散剂、乙氧基化合物分散剂、聚丙烯酸酯型分散剂、聚酯型分散剂、聚醚型分散剂、聚烯烃类分散剂、碳酸钠、正磷酸钠、聚乙烯亚胺或鲱鱼油中的任意一种。By weight, 5-10 parts of 0.5-5 micron diamond powder, 1-3 parts of water-resistant aluminum nitride powder, 10-30 parts of 200-1000 mesh electrolytic copper powder, 5-10 parts of filler and 0.5-2 parts of additives Add into 20-50 parts of water, disperse by planetary ball mill, and use zirconia microspheres as dispersion medium to prepare a suspension; the fillers are copper-coated graphite, talc powder, cryolite, cerium oxide, aluminum oxide powder, Any one or more of calcium carbonate, calcium oxide, zinc oxide, barium sulfate, magnesium oxide, molybdenum disulfide, silicon carbide; the additive is composed of wetting agent, dispersant, silicone defoamer and dimethyl The silicone oil release agent is mixed to obtain, the addition amount of the wetting agent is 0.1-1 wt% of the dry weight of the glue-containing slurry, the added amount of the dispersant is 0.1-1.5 wt% of the dry weight of the glue-containing slurry, and the addition amount of the silicone defoamer is 0.1-1.5 wt% of the glue-containing slurry. The dry weight of the slurry is 0.1-1 wt%, the addition amount of the dimethicone release agent is 0.1-1 wt% of the dry weight of the glue-containing slurry, and the wetting agent is selected from alkyl sulfates, sulfonates, fatty acids, fatty acids Ester sulfate, carboxylic acid soap, phosphate anionic surfactant, or polyoxyethylene alkyl phenol ether, polyoxyethylene fatty alcohol ether, polyoxyethylene polyoxypropylene block copolymer nonionic surfactant Any one of the dispersants, the dispersants are phosphate ester type dispersants, ethoxylate dispersants, polyacrylate type dispersants, polyester type dispersants, polyether type dispersants, polyolefin type dispersants, carbonic acid Any of sodium, sodium orthophosphate, polyethyleneimine or herring oil.
进一步的,步骤3中所述聚乙烯醇胶水中的水与乙醇的重量比为3~10:1,聚乙烯醇固含量为5~15wt%;所述的水溶性树脂液是水溶性聚酰亚胺树脂液、水溶性环氧树脂液,水溶性酚醛树脂液中的一种或者几种,水溶性树脂液固含量为40~60wt%;混合胶水干重占含胶浆料干重比为5~15wt%;Further, in step 3, the weight ratio of water and ethanol in the polyvinyl alcohol glue is 3-10:1, and the polyvinyl alcohol solid content is 5-15wt%; the water-soluble resin liquid is a water-soluble polyamide One or more of imine resin liquid, water-soluble epoxy resin liquid, and water-soluble phenolic resin liquid, the solid content of the water-soluble resin liquid is 40-60 wt%; the ratio of the dry weight of the mixed glue to the dry weight of the glue-containing slurry is 5~15wt%;
进一步的,步骤4中所述的模具为圆柱形,正方形或者多边形;所述的致密化处理是冷等静压,压强为5~50MPa;所述的烧结具体为将所述坯体放在烘箱中,首先升温到75℃保温60min,再升温到115℃保温90min,再升温到150~180℃保温60min,最后升温到180~230℃保温30min。烧结后,聚乙烯醇胶发生热分解碳化形成均匀的毛细微孔,完成了凝胶成坯的功能,此时水溶性树脂热固化,起到丸片树脂结合剂的作用,制备得到具有微细毛孔的抛光丸片半成品。Further, the mold described in
进一步的,步骤5中所述表面修平处理是将抛光丸片半成品贴在基盘上,将基盘放在平面磨床上用#100号的陶瓷基砂轮将抛光丸片半成品表面磨平,抛光液为酸性抛光液、碱性抛光液或者水,所述酸性磨削液和碱性磨削液分别通过在水中添加酸性pH调节剂或者碱性pH调节剂制备得到,酸性pH调节剂为稀盐酸,pH值调节范围为2~6,碱性pH调节剂为氢氧化钾,碱性抛光液pH值调节范围为8~12,提高对可溶氮化铝填料的溶解能力,增强丸片自修锐效果。Further, the surface leveling treatment described in
使用本发明的制备方法得到的抛光丸片对工件进行抛光加工,所述加工方法为将工件用蜡黏贴在陶瓷基盘上,抛光丸片黏贴在铸铁盘上放置在平面抛光机基盘上,抛光盘转速为50~150rpm,陶瓷基盘用夹具夹紧,夹具气动加压,压力为1~20Mpa,抛光温度为30~38℃,抛光时间为10~30min。The workpiece is polished by using the polishing pellets obtained by the preparation method of the present invention, and the processing method is that the workpiece is pasted on the ceramic base plate with wax, and the polishing pellets are pasted on the cast iron plate and placed on the base plate of a plane polishing machine. The rotating speed of the polishing disc is 50-150rpm, the ceramic base plate is clamped with a clamp, the clamp is pneumatically pressurized, the pressure is 1-20Mpa, the polishing temperature is 30-38°C, and the polishing time is 10-30min.
本发明具备的有益效果:传统凝胶磨具采用胶水直接凝胶作为结合剂固结磨料,本发明通过聚乙烯醇和水溶性树脂混合液凝胶制作磨具,减少磨粒磨具内部缺陷、保证磨具组织的均匀性。两种树脂在抛光丸片成型过程中的作用不同,首先利用聚乙烯醇具有的低温物理凝胶能力,形成凝胶素坯,高温下聚乙烯醇烧结碳化,同时水溶性树脂固化作为抛光丸片结合剂,聚乙烯醇碳化后产生大量毛细微孔,相比直接粉末成型添加造孔剂产生的孔为闭孔,本方法在丸片中产生的毛细微孔是贯通微孔,对水的吸收能力强,有利于提高摩擦力、抛光液的储存和排屑。The present invention has the beneficial effects: traditional gel abrasives use glue direct gel as a binding agent to consolidate abrasives, and the present invention uses polyvinyl alcohol and water-soluble resin mixed liquid gel to make abrasives, reducing the internal defects of abrasive abrasives and ensuring The uniformity of the abrasive structure. The two resins have different roles in the molding process of polishing pellets. First, the low-temperature physical gelling ability of polyvinyl alcohol is used to form a gel china, and the polyvinyl alcohol is sintered and carbonized at high temperature, and at the same time, the water-soluble resin is cured as a polishing pellet. Binder, after carbonization of polyvinyl alcohol, a large number of capillary pores are generated. Compared with direct powder molding, the pores generated by adding pore-forming agent are closed pores. Strong ability, which is beneficial to improve friction, storage of polishing liquid and chip removal.
传统磨具通过添加“可溶”、“可分解”或“可电解”填料提高自锐性,“可溶”和“可分解”填料会发生溶胀现象,且并不能保证表面材料的选择性自锐,“可电解”填料具有工艺复杂的缺点。本发明添加了表面涂覆有耐水纳米二氧化硅涂层的氮化铝可溶粉末填料,丸片表层氮化铝表面的二氧化硅磨损,氮化铝被抛光液水解,表面结合强度下降,钝化磨料脱落,新的磨料露出来,保持自锐性;由于抛光丸片中的毛细微孔具有吸水能力,丸片里面涂覆有耐水纳米二氧化硅涂层的氮化铝可避免直接水解,保持丸片基体的强度,因此,该抛光丸片具有内部结构稳定,表面自锐性好的优点。Traditional abrasives improve self-sharpening by adding "soluble", "decomposable" or "electrolytic" fillers. Sharp, "electrolyzable" fillers have the disadvantage of complex processes. The invention adds the aluminum nitride soluble powder filler coated with water-resistant nano-silica coating on the surface, the silicon dioxide on the surface of the aluminum nitride on the surface of the pellet wears, the aluminum nitride is hydrolyzed by the polishing liquid, and the surface bonding strength decreases, The passivation abrasive falls off, and the new abrasive is exposed to maintain self-sharpening; because the capillary pores in the polishing pellets have water absorption capacity, the aluminum nitride coated with a water-resistant nano-silica coating on the pellets can avoid direct hydrolysis , to maintain the strength of the pellet matrix, therefore, the polished pellet has the advantages of stable internal structure and good surface self-sharpening.
附图说明Description of drawings
图1溶胶凝胶抛光丸片内部结构示意图;Fig. 1 is a schematic diagram of the internal structure of a sol-gel polishing pellet;
图2实施例1制备得到的溶胶凝胶抛光丸片SEM表面形貌图;Fig. 2 SEM surface topography of the sol-gel polishing pellet prepared in Example 1;
图3抛光方式示意图;Figure 3 is a schematic diagram of a polishing method;
图4实施例1制备得到的抛光丸片抛光锗平面镜白光干涉表面形貌图;The topography of the white light interference surface of the polishing pellet polished germanium plane mirror prepared in Fig. 4 embodiment 1;
图5凝胶抛光丸片和热压抛光丸片材料去除率和抛光时间关系图;Figure 5. The relationship between the material removal rate and polishing time of gel polishing pellets and hot pressing polishing pellets;
图6不同金刚石磨料含量条件下抛光丸片对锗平面镜头加工后的表面粗糙度和材料去除率;Fig. 6 Surface roughness and material removal rate of germanium flat lens processed by polishing pellets under different diamond abrasive content conditions;
图7抛光液pH值和抛光丸片磨损率关系图。Figure 7. Relationship between pH value of polishing solution and polishing pellet wear rate.
具体实施方式Detailed ways
本发明提供了一种添加具有耐水涂层可溶填料的溶胶凝胶抛光丸片及其制备方法,溶胶凝胶抛光丸片内部结构示意图如图1所示。使用聚乙烯醇和水溶性树脂液凝胶制作磨具,避免了粉末成型分散不均匀的问题,利用聚乙烯醇具有的物理凝胶能力,形成凝胶素坯,烧结碳化,水溶性树脂烧结固化温度也是聚乙烯醇碳化温度,聚乙烯醇碳化后产生大量贯通的毛细微孔,具有良好的吸水能力,且添加了表面涂覆有耐水纳米二氧化硅涂层的氮化铝可溶粉末填料,丸片表层氮化铝表面的二氧化硅磨损,氮化铝被抛光液水解,表面结合强度下降,钝化磨料脱落,新的磨料露出来,保持自锐性;丸片里面涂覆有耐水纳米二氧化硅涂层的氮化铝可避免直接水解,保持丸片基体的强度,可以有效降低磨料的消耗量,提高抛光工具中磨料的使用寿命和利用率。The present invention provides a sol-gel polishing pellet added with a water-resistant coating soluble filler and a preparation method thereof. The schematic diagram of the internal structure of the sol-gel polishing pellet is shown in FIG. 1 . The use of polyvinyl alcohol and water-soluble resin lyogel to make abrasive tools avoids the problem of uneven powder molding and dispersion, and uses the physical gel ability of polyvinyl alcohol to form a gel green body, sintering carbonization, and water-soluble resin sintering and curing temperature It is also the carbonization temperature of polyvinyl alcohol. After carbonization of polyvinyl alcohol, a large number of through capillary pores are produced, which has good water absorption capacity, and aluminum nitride soluble powder filler coated with water-resistant nano-silica coating on the surface is added. The silicon dioxide on the surface of the aluminum nitride on the surface of the chip is worn, the aluminum nitride is hydrolyzed by the polishing liquid, the surface bonding strength decreases, the passivation abrasive falls off, and the new abrasive is exposed to maintain self-sharpening; The silicon oxide-coated aluminum nitride can avoid direct hydrolysis, maintain the strength of the pellet matrix, effectively reduce the consumption of abrasives, and improve the service life and utilization of abrasives in polishing tools.
实施例1:Example 1:
步骤1:制备表面具有耐水膜层的氮化铝粉末Step 1: Preparation of aluminum nitride powder with a water-resistant film on the surface
按重量计,取100g粒径为1微米氮化铝粉末和1kg无水乙醇混合,搅拌均匀,水浴条件下,升温至40℃,得到氮化铝乙醇分散液;同时将600g无水乙醇稀释的80g正硅酸乙酯(TEOS),以及600g无水乙醇稀释的100g氨水和100g水滴加到氮化铝乙醇分散液中,滴加速度控制为2滴/秒,滴加完毕后,在40℃下反应6小时后,停止反应,真空抽滤,用无水乙醇洗涤产物3次,再将得到的产物置于室温条件下自然干燥12小时,干燥后放在300℃条件下煅烧2小时,冷却后,过200目筛,即得到二氧化硅包覆的氮化铝粉末;,由于二氧化硅具备耐水性,因此得到了表面具有耐水膜层的氮化铝粉末;步骤2:制备悬浮液:按重量计,取300g粒径为2.5微米金刚石粉末、100g二氧化硅包覆的氮化铝粉末、500g粒度为400目电解铜粉、50g铜包石墨、50g冰晶石粉、80g氧化锌、150g硫酸钡、70g铝氧粉、15g聚氧乙烯烷基酚醚湿润剂、20g聚乙烯亚胺、10g有机硅消泡剂和10g二甲基硅油脱模剂加入到1200g水中,混合后使用行星式球磨机进行分散,分散介质选用粒径3mm氧化锆微球,制备得到悬浮液。By weight, take 100 g of aluminum nitride powder with a particle size of 1 micron and mix with 1 kg of absolute ethanol, stir evenly, and heat up to 40 ° C under water bath conditions to obtain aluminum nitride ethanol dispersion; 80g of tetraethyl orthosilicate (TEOS), 100g of ammonia water and 100g of water diluted with 600g of absolute ethanol were added dropwise to the aluminum nitride ethanol dispersion, and the dropping rate was controlled to 2 drops/sec. After 6 hours of reaction, the reaction was stopped, vacuum filtered, and the product was washed three times with absolute ethanol, and then the obtained product was naturally dried at room temperature for 12 hours. After drying, it was calcined at 300 ° C for 2 hours. After cooling , pass through a 200-mesh sieve to obtain silica-coated aluminum nitride powder; because silica has water resistance, an aluminum nitride powder with a water-resistant film layer on the surface is obtained; Step 2: Prepare the suspension: press By weight, taking 300g particle size is 2.5 micron diamond powder, 100g silicon dioxide coated aluminum nitride powder, 500g particle size is 400 mesh electrolytic copper powder, 50g copper-coated graphite, 50g cryolite powder, 80g zinc oxide, 150g barium sulfate , 70g aluminum oxide powder, 15g polyoxyethylene alkyl phenol ether wetting agent, 20g polyethyleneimine, 10g silicone defoamer and 10g dimethicone oil release agent were added to 1200g water, and mixed with a planetary ball mill. For dispersion, the dispersion medium is selected from zirconia microspheres with a particle size of 3 mm to prepare a suspension.
步骤3:制备含胶浆料:在90℃水浴条件下,将10g聚乙烯醇溶于80g水和10g乙醇的混合溶剂中得到100g固含量为10wt%聚乙烯醇胶水;再向聚乙烯醇胶水中添加300g固含量为40wt%的水溶性聚酰亚胺树脂液,得到400g混合胶水,再将混合胶水边搅拌边加入到步骤2制备的悬浮液中,混合搅拌后,使用行星式球磨机进行分散1小时,得到含胶浆料;Step 3: Preparation of glue-containing slurry: under the condition of a water bath at 90°C, dissolve 10 g of polyvinyl alcohol in a mixed solvent of 80 g of water and 10 g of ethanol to obtain 100 g of polyvinyl alcohol glue with a solid content of 10 wt %; Add 300g of water-soluble polyimide resin liquid with a solid content of 40wt% to obtain 400g of mixed glue, and then add the mixed glue to the suspension prepared in step 2 while stirring, after mixing and stirring, use a planetary ball mill to disperse 1 hour to obtain glue-containing slurry;
步骤4:制备具有微细毛孔的抛光丸片:将制得的含胶浆料各取15g倒入直径为12mm的圆柱形模具中,置于-15℃温度下冷冻2小时,解冻后自然干燥10小时,从模具中取出坯体,在20MPa条件下冷等静压,放入烘箱中45℃条件下烘24小时,烘干后,丸片坯体升温到180℃烧结,升温曲线是首先升温到75℃保温1小时,再升温到115℃保温1.5小时,再升温到180℃保温1小时,最后升温到230℃保温30min,聚乙烯醇胶热分解形成均匀的毛细微孔,水溶性聚酰亚胺树脂固化,制备得到表面粗糙的抛光丸片半成品,再用平面磨床将抛光丸片半成品表面磨平,得到抛光丸片成品,制备得到的溶胶凝胶抛光丸片SEM如图2所示,金刚石、填料和电解铜粉在抛光丸片中分布均匀。获得的抛光丸片拉伸强度达到了25MPa,硬度达到了60(邵尔硬度),断裂伸长率为150%。Step 4: Preparation of polishing pellets with fine pores: Pour 15g of the prepared glue-containing slurry into a cylindrical mold with a diameter of 12mm, freeze at -15°C for 2 hours, and naturally dry for 10 hours after thawing. hours, take out the green body from the mold, cold isostatic pressing under the condition of 20MPa, put it in an oven and bake it at 45℃ for 24 hours. After drying, the pellet green body is heated to 180℃ for sintering. 75 °C for 1 hour, then heated to 115 °C for 1.5 hours, then heated to 180 °C for 1 hour, and finally heated to 230 °C for 30 minutes, the polyvinyl alcohol glue was thermally decomposed to form uniform capillary pores, water-soluble polyimide The amine resin is cured to prepare a semi-finished polishing pellet with a rough surface, and then the surface of the semi-finished polishing pellet is ground with a surface grinder to obtain a finished polishing pellet. The SEM of the prepared sol-gel polishing pellet is shown in Figure 2. The diamond , filler and electrolytic copper powder are evenly distributed in the polishing pellets. The obtained polishing pellets have a tensile strength of 25 MPa, a hardness of 60 (Shore hardness), and an elongation at break of 150%.
实施例2:Example 2:
锗平面镜头抛光加工:Polishing of germanium plane lens:
抛光方式示意图如图3所示,将直径100mm的锗平面镜头用蜡黏贴在陶瓷基盘上,先用10微米金刚石抛光液配合碳化硅研磨盘对对平面镜头进行研磨,表面粗糙度达到25nm,将实施例1制备得到的丸片黏贴在铸铁盘上,铸铁盘直径200mm,丸片表面在平面磨床上修平,垂直误差小于2微米,铸铁盘放置在平面抛光机基盘上,陶瓷基盘用夹具夹紧,抛光盘转速为100rpm,夹具气动加压,压力为5Mpa,抛光过程中在丸片表面加酸性抛光液,pH值为5,流量为100ml/min,通过水中添加酸性pH调节剂稀盐酸调节pH值为5,提高对可溶氮化铝填料的溶解能力,抛光温度控制在30℃,抛光时间为20min,抛光完成后对锗平面镜头进行表面白光观察分析,表面形貌如图4所示,表面粗糙度达到了7.716nm。The schematic diagram of the polishing method is shown in Figure 3. The germanium plane lens with a diameter of 100mm is pasted on the ceramic substrate with wax. First, the plane lens is ground with a 10-micron diamond polishing liquid and a silicon carbide grinding disk, and the surface roughness reaches 25nm. , the pellets prepared in Example 1 were pasted on a cast iron disc, the diameter of the cast iron disc was 200 mm, the surface of the pellets was flattened on a plane grinder, the vertical error was less than 2 microns, the cast iron disc was placed on the base plate of the plane polisher, and the ceramic base The disc is clamped with a clamp, the polishing disc rotation speed is 100rpm, the clamp is pneumatically pressurized, and the pressure is 5Mpa. During the polishing process, an acid polishing solution is added to the surface of the pellet, the pH value is 5, and the flow rate is 100ml/min. The pH is adjusted by adding acid in water. Dilute hydrochloric acid was used to adjust the pH to 5 to improve the solubility of soluble aluminum nitride fillers. The polishing temperature was controlled at 30 °C and the polishing time was 20 min. After polishing, the germanium plane lens was observed and analyzed by white light on the surface. As shown in Figure 4, the surface roughness reaches 7.716nm.
实施例3:Example 3:
操作与实施例1基本相同,不同之处在于步骤2中,二氧化硅包覆的氮化铝粉末的量增加到150g,烧结完毕后在干燥条件下仍可以保持丸片基体的强度,拉伸强度达到了25Mpa,抗折强度为60Mpa,断裂伸长率为145%,在水中浸泡1小时后,拉伸强度为23Mpa,抗折强度为55Mpa,烘干后,称取重量,重量下降0.5g;2小时后,拉伸强度为22Mpa,抗折强度为53Mpa,强度下降不明显,烘干后,称取重量,重量下降0.4g。The operation is basically the same as in Example 1, the difference is that in step 2, the amount of silica-coated aluminum nitride powder is increased to 150 g, and the strength of the pellet matrix can still be maintained under dry conditions after sintering, and the tensile strength is increased. The strength reached 25Mpa, the flexural strength was 60Mpa, and the elongation at break was 145%. After soaking in water for 1 hour, the tensile strength was 23Mpa, and the flexural strength was 55Mpa. After drying, the weight was weighed, and the weight decreased by 0.5g ; After 2 hours, the tensile strength was 22Mpa, the flexural strength was 53Mpa, and the strength did not decrease significantly. After drying, the weight was weighed, and the weight decreased by 0.4g.
将丸片表面摩擦后,称取丸片原始重量,在水中浸泡1小时,丸片整体拉伸强度为23Mpa,抗折强度为55Mpa,烘干后,称取重量,重量下降1g,说明丸片表面摩擦后,有利于表层氮化铝水解。After rubbing the surface of the pill, weigh the original weight of the pill, soak it in water for 1 hour, the overall tensile strength of the pill is 23Mpa, and the flexural strength is 55Mpa. After the surface is rubbed, it is beneficial to the hydrolysis of the surface aluminum nitride.
实施例4:Example 4:
操作与实施例1基本相同,不同之处在于增加步骤3中混合胶水中10wt%聚乙烯醇胶水的量到200g,由于聚乙烯醇烧结后碳化,能产生大量具有良好吸水能力的毛细微孔,摩擦力增强,去除效率提高,但是磨损率也同时提高。The operation is basically the same as in Example 1, the difference is that the amount of 10wt% polyvinyl alcohol glue in the mixed glue in step 3 is increased to 200g. Due to the carbonization of polyvinyl alcohol after sintering, a large number of capillary pores with good water absorption capacity can be generated, The friction is increased and the removal efficiency is increased, but the wear rate is also increased.
作为对比实验,操作与实施例1基本相同,不同之处在于增加水溶性聚酰亚胺树脂液到500g,固化后,抛光丸片树脂结合剂多,耐磨性提高,可水解填料氮化铝的作用下降,使用5小时后,表面有釉化现象,去除力下降。As a comparative experiment, the operation is basically the same as that of Example 1, the difference is that the water-soluble polyimide resin solution is increased to 500g. After curing, there are more resin binders for polishing pellets, the wear resistance is improved, and the hydrolyzable filler is aluminum nitride. After 5 hours of use, there is glaze on the surface, and the removal power decreases.
实施例5:Example 5:
本实施例对实施例1中凝胶抛光丸片和市售2.5微米金刚石抛光丸片进行了对比实验,抛光工艺与实施例2基本相同,市售丸片采用粉体混料—热压工艺,实验观察了材料去除率随时间的变化,如图5所示,从图中可以看出,初始阶段,热压丸片比凝胶丸片材料去除率高,这是因为凝胶丸片内部树脂网络结构,使其在具有等量树脂结合剂条件下,强度更高,磨料难以脱落,在长时间抛光使用后,凝胶丸片表层氮化铝填料水解,结合力下降,磨料脱落,丸片自修锐,保持了材料去除的稳定性,因此凝胶抛光丸片相比热压丸片具有强度高,材料去除率稳定的特点。In this example, a comparative experiment is carried out on the gel polishing pellets in Example 1 and the commercially available 2.5-micron diamond polishing pellets. The polishing process is basically the same as that in Example 2. The commercially available pellets adopt the powder mixing-hot pressing process. The experiment observed the change of material removal rate with time, as shown in Figure 5. It can be seen from the figure that in the initial stage, the material removal rate of hot-pressed pellets is higher than that of gel pellets, which is because the resin inside the gel pellets The network structure makes it stronger under the condition of the same amount of resin bond, and the abrasive is difficult to fall off. After long-term polishing and use, the aluminum nitride filler on the surface of the gel pellet is hydrolyzed, the bonding force decreases, the abrasive falls off, and the pellet falls off. Self-sharpening maintains the stability of material removal, so gel polishing pellets have the characteristics of higher strength and stable material removal rate than hot pressing pellets.
实施例6:Example 6:
本实施目的是试验出抛光丸片中不同金刚石磨料粒度对研磨抛光的效率影响。The purpose of this implementation is to test the effect of different diamond abrasive particle sizes in the polishing pellet on the efficiency of grinding and polishing.
操作与实施例1基本相同,不同之处在于,金刚石磨料粒径值为W0.5,W1.5,W2.5,W3.5,W5,W7分别制备抛光丸片,在nanopoli100研磨抛光机上对锗平面镜头进行抛光,测量不同金刚石磨料含量条件下凝胶金刚石丸片对锗平面镜头加工后的表面粗糙度和材料去除率,如图6所示,从图中可以看到,随着金刚石磨粒粒径的增大,对工件加工后的表面粗糙度和材料去除率都有所提高,选择不同金刚石粒径可以获得不同的表面粗糙度,金刚石粒径小于2.5微米后,抛光效率下降速度快,表面质量改变不明显。The operation is basically the same as in Example 1, the difference is that the particle size of diamond abrasives is W0.5, W1.5, W2.5, W3.5, W5, W7 to prepare polishing pellets, respectively, on the nanopoli100 grinding and polishing machine. The germanium plane lens was polished, and the surface roughness and material removal rate of the germanium plane lens processed by gel diamond pellets under different diamond abrasive content were measured, as shown in Figure 6. It can be seen from the figure that with the diamond grinding The increase of particle size increases the surface roughness and material removal rate of the workpiece after processing. Different surface roughness can be obtained by selecting different diamond particle sizes. When the diamond particle size is less than 2.5 microns, the polishing efficiency decreases rapidly. , the surface quality does not change significantly.
实施例7:Example 7:
本实施例在实施例2的基础上改变抛光液pH值,观察pH值对丸片磨损率的影响。从图7中可以看出提高抛光液酸碱性都能提高抛光丸片磨损率,这是因为酸碱度提高,氮化铝水解速率提高,有利于抛光丸片自锐,但过高的磨损率不利于丸片面型的保持。In this example, the pH value of the polishing solution was changed on the basis of Example 2, and the effect of the pH value on the wear rate of the pellet was observed. It can be seen from Figure 7 that increasing the acidity and alkalinity of the polishing solution can increase the wear rate of the polishing pellets. This is because the increase of the pH and the hydrolysis rate of aluminum nitride are beneficial to the self-sharpening of the polishing pellets, but the excessive wear rate does not Conducive to the preservation of the shape of the pill.
实施例8:Example 8:
操作与实施例1基本相同,不同之处在于水溶性聚酰亚胺树脂改成水溶性酚醛树脂,步骤3中,烧结温度改为180℃,烧结升温曲线是首先升温到75℃保温1小时,再升温到115℃保温1.5小时,最后升温到180℃保温30min,得到酚醛树脂结合剂抛光丸片,获得的抛光丸片拉伸强度达到了22MPa,硬度达到了56(邵尔硬度),抛光锗平面镜,表面粗糙度可以达到10nm以下。The operation is basically the same as that in Example 1, except that the water-soluble polyimide resin is changed to a water-soluble phenolic resin. In step 3, the sintering temperature is changed to 180°C, and the sintering heating curve is firstly heated to 75°C and kept for 1 hour. Then the temperature was raised to 115°C for 1.5 hours, and finally the temperature was raised to 180°C for 30 minutes to obtain phenolic resin bonded polishing pellets. The tensile strength of the obtained polishing pellets reached 22MPa, and the hardness reached 56 (Shore hardness). Polished germanium For flat mirrors, the surface roughness can reach below 10nm.
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