CN117821017A - Chemical mechanical polishing abrasive particle, preparation method thereof and polishing solution - Google Patents
Chemical mechanical polishing abrasive particle, preparation method thereof and polishing solution Download PDFInfo
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- CN117821017A CN117821017A CN202311844050.3A CN202311844050A CN117821017A CN 117821017 A CN117821017 A CN 117821017A CN 202311844050 A CN202311844050 A CN 202311844050A CN 117821017 A CN117821017 A CN 117821017A
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- chemical mechanical
- mechanical polishing
- polishing abrasive
- polishing
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- 238000005498 polishing Methods 0.000 title claims abstract description 155
- 239000002245 particle Substances 0.000 title claims abstract description 90
- 239000000126 substance Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 229920000642 polymer Polymers 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 88
- 239000000377 silicon dioxide Substances 0.000 claims description 43
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 33
- 230000032683 aging Effects 0.000 claims description 30
- 238000005530 etching Methods 0.000 claims description 30
- 235000012239 silicon dioxide Nutrition 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 239000002105 nanoparticle Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 12
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 12
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 150000002894 organic compounds Chemical class 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 125000003700 epoxy group Chemical group 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 125000003172 aldehyde group Chemical group 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 125000001951 carbamoylamino group Chemical group C(N)(=O)N* 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 claims description 3
- 125000006833 (C1-C5) alkylene group Chemical group 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- BGJOTKHBFYMJST-UHFFFAOYSA-N 2-methylprop-2-enoic acid;n-propan-2-ylprop-2-enamide Chemical compound CC(=C)C(O)=O.CC(C)NC(=O)C=C BGJOTKHBFYMJST-UHFFFAOYSA-N 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 78
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 15
- 239000003575 carbonaceous material Substances 0.000 description 13
- 238000007517 polishing process Methods 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000005416 organic matter Substances 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000006061 abrasive grain Substances 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052809 inorganic oxide Inorganic materials 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- -1 amino, hydroxyl Chemical group 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000006748 scratching Methods 0.000 description 2
- 230000002393 scratching effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2h-oxazine Chemical compound N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- ZSIQJIWKELUFRJ-UHFFFAOYSA-N azepane Chemical compound C1CCCNCC1 ZSIQJIWKELUFRJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 235000019794 sodium silicate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention belongs to the field of polishing, and provides chemical mechanical polishing abrasive particles, a preparation method thereof and polishing solution. The chemical mechanical polishing abrasive particles have a porous structure, and the material of the chemical mechanical polishing abrasive particles comprises a polymer and/or a calcined product of the polymer. The chemical mechanical polishing abrasive particles can reduce scratches of the chemical mechanical polishing abrasive particles on a polishing piece in a chemical mechanical planarization process.
Description
Technical Field
The invention relates to the field of polishing, in particular to chemical mechanical polishing abrasive particles, a preparation method thereof and polishing solution.
Background
Chemical mechanical planarization is an indispensable step in the chip manufacturing process, and its principle is: in the polishing process, the polished part generates relative motion with the polishing pad under a certain pressure, polishing liquid (composed of water, polishing abrasive particles and additives) is applied between the workpiece and the polishing pad, and an ultra-precise polishing surface is obtained under the alternating action of chemistry and machinery. It can be seen that the polishing abrasive particles have a large influence on the polishing rate, the surface flatness of the chip, and the defect level in the chemical mechanical planarization process.
The existing polishing abrasive mainly adopts inorganic oxides (such as alumina, silica, cerium oxide and the like), the hardness of the inorganic oxides is high, scratches of polishing pieces (such as chips) can be caused in the polishing process, and the yield of the polishing pieces is reduced.
Thus, there is a need for improvements in current chemical mechanical polishing abrasive particles.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent.
In a first aspect of the present invention, a chemical mechanical polishing abrasive particle is provided, the chemical mechanical polishing abrasive particle having a porous structure, and a material of the chemical mechanical polishing abrasive particle comprising a polymer and/or a calcined product of the polymer.
The chemical mechanical polishing abrasive particles of the invention have a porous structure, and the material comprises a polymer and/or a baked product of the polymer. Therefore, the chemical mechanical polishing abrasive particles have better elasticity and toughness and lower hardness. In addition, the polymer can realize the regulation and control of different electronic groups such as amino, hydroxyl, carboxyl and the like on the surface of the polymer due to the chemical structure of the polymer, and the abundant regulation and control of the surface groups can further improve the chemical properties (such as hardness reduction and elasticity improvement) of the polishing abrasive particles, so that the scratch of a polishing piece is reduced in the chemical mechanical planarization process. In addition, the baked product of the polymer is a carbon material, the density of the carbon material and the polymer is lower, and the polymer has better suspension property and fluidity, thereby being beneficial to improving the flatness of the polished member in the polishing process.
According to an embodiment of the invention, the polymer comprises at least one of urea formaldehyde resin, phenolic resin, polymethyl methacrylate, poly (N-isopropylacrylamide-methacrylic acid) and epoxy resin. Therefore, the polymer has lower hardness and higher toughness, and the scratch of the polished part can be further reduced in the polishing process.
According to an embodiment of the invention, the roasting is performed under an inert atmosphere, the roasting temperature is 500-800 ℃ and the time is 4-8 h. Thus, the polymer is carbonized to form a carbon material while saving cost.
According to an embodiment of the present invention, the chemical mechanical polishing abrasive particles have a diameter of 10nm to 300nm. Thereby, scratches can be reduced during polishing.
According to an embodiment of the present invention, the chemical mechanical polishing abrasive particles have a specific surface area of 200m 2 /g-400m 2 And/g. Therefore, the elasticity of the chemical mechanical polishing abrasive particles can be improved, the hardness can be reduced, and the polishing rate can be improved.
In a second aspect of the present invention, the present invention provides a method for preparing the chemical mechanical polishing abrasive according to the first aspect of the present invention, comprising the steps of:
(1) Mixing the solution A containing the silicon dioxide nano particles and a silane coupling agent with a first reaction group, and performing first aging to form a solution B containing silicon dioxide modified by the silane coupling agent;
(2) Mixing the solution B with a polymerizable organic compound having a second reactive group, and performing second aging to react the first reactive group with the second reactive group to form a solution C containing first polishing particles of an organic-inorganic doped structure;
(3) Mixing the solution C with an etching solution to etch and remove silicon dioxide in the first polishing particles to form a solution D of second polishing particles comprising a porous polymer;
(4) And (3) carrying out solid-liquid separation, drying and optionally roasting on the solution D to obtain the chemical mechanical polishing abrasive particles with the porous structure.
The method is simple to operate, the silicon dioxide nano particles are used as a hard template agent, the surface of the hard template agent is modified by the silane coupling agent, then the silane coupling agent is reacted with the polymerizable organic matter with the second reactive group to obtain the polymer, the polymer wraps the hard template agent, finally, the hard template agent is removed by etching, and a porous structure is left in the polymer to form the polymer with the porous structure. Optionally, the polymer is carbonized by firing to further form a porous carbon material. Thus, the prepared polishing abrasive particles comprising the porous structure organic matter can improve the flatness of the polishing member during the chemical mechanical polishing process and reduce the scratches of the polishing member.
According to an embodiment of the present invention, step (1) further comprises: mixing an alkaline solvent with an orthosilicic acid solution, and aging for 0.5-4 h at 45-85 ℃ to prepare the solution A; wherein the pH of the alkaline solvent is 9.5-10.5; in the orthosilicic acid solution, the mass concentration of the orthosilicic acid is 2% -7%. Thereby, it is advantageous to obtain silica having a uniform particle size and reduce agglomeration of silica.
According to an embodiment of the present invention, the silane coupling agent has a molecular formula of Y-R 1 -L-Si (OR) 3, wherein R represents a C1-C4 alkyl group, R 1 Represents a single bond, C1-C5 alkylene, L represents a single bond or-OCH 2 -Y represents said first reactive group and comprises an epoxy, vinyl, ureido or mercapto group.
According to an embodiment of the invention, the second reactive group comprises a vinyl group, an epoxy group or an aldehyde group.
According to an embodiment of the present invention, the polymerizable organic comprises at least one of methyl methacrylate, methacrylic acid, isopropyl acrylamide, formaldehyde, ethylene oxide, propylene oxide, and phenol. Thus, on the one hand, these polymerizable monomers are polymerized with the Y groups of the silane coupling agent via the respective second reactive groups to form a polymer, and on the other hand, the formed polymer has a lower hardness, which reduces the risk of scratching the polished part during polishing.
According to an embodiment of the present invention, the etching liquid includes at least one of an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous lithium hydroxide solution, an aqueous magnesium hydroxide solution, an aqueous calcium hydroxide solution, an aqueous ammonia solution, and an aqueous hydrofluoric acid solution.
According to an embodiment of the invention, in step (1), the first ageing is carried out under stirring for a period of time ranging from 1h to 4h and at a temperature ranging from 35 ℃ to 70 ℃. Thereby facilitating the smooth progress of the first aging.
According to an embodiment of the present invention, in the step (1), the mass ratio of the silane coupling agent to the silica nanoparticle is (0.01 to 0.5) to 1. Thereby, self-agglomeration of silica is reduced, and abrasive grains having a moderate surface area and diameter are obtained.
According to an embodiment of the invention, in step (2), the second aging is carried out at room temperature under stirring for a period of time ranging from 0.5h to 3h. Thereby facilitating the second aging.
According to an embodiment of the invention, in step (2), the second aging has a pH of 2-6.
According to an embodiment of the present invention, in the step (2), the molar ratio of the silane coupling agent to the polymerizable organic compound is 1: (0.7-1.3). Thus, the self-agglomeration of the silica is reduced, resulting in a chemical mechanical polishing abrasive grain having a higher toughness and lower hardness.
According to an embodiment of the present invention, in the step (3), the etching reaction time is 4h to 6h. Therefore, the cost is saved, and meanwhile, the silicon dioxide in the organic matters is etched as much as possible, so that the chemical mechanical polishing abrasive particles with moderate specific surface area are obtained, and scratches of polishing pieces are reduced in the polishing process.
According to an embodiment of the present invention, in the step (3), the temperature of the etching reaction is 70 ℃ to 95 ℃. Therefore, the cost is saved, and meanwhile, silicon dioxide in the organic matters is etched and removed as much as possible, so that chemical mechanical polishing abrasive particles with moderate specific surface area are obtained, and scratches of polishing pieces are reduced in the polishing process.
According to the embodiment of the invention, the etching liquid is hydrofluoric acid aqueous solution, and the concentration of HF is 5-15 wt%.
According to the embodiment of the invention, the mass ratio of the silicon dioxide nano particles to the etching liquid is 1:1-5. Therefore, the cost is saved, and meanwhile, the silicon dioxide in the organic matters is etched as much as possible, so that the chemical mechanical polishing abrasive particles with moderate specific surface area are obtained, and scratches of polishing pieces are reduced in the polishing process.
According to an embodiment of the invention, the calcination is performed in an inert atmosphere at a calcination temperature of 500-800 ℃ for a calcination time of 4-8 hours. Thereby, the organic matter is carbonized, and meanwhile, the production cost is reduced.
In a third aspect of the present invention, there is provided a polishing slurry comprising the chemical mechanical polishing abrasive particles of the first aspect of the present invention. Thus, the polishing liquid is particularly suitable for the chemical mechanical planarization process of polishing pieces, and can reduce scratches of the polishing pieces.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 illustrates a schematic view of some embodiments of a process for making chemical mechanical polishing abrasive particles.
Detailed Description
Embodiments of the present invention are described in detail below. The embodiments described below are exemplary only for explaining the present invention and are not to be construed as limiting the present invention.
In a first aspect, the present invention provides a chemical mechanical polishing abrasive particle having a porous structure, and the material of the chemical mechanical polishing abrasive particle comprises a polymer and/or a calcined product of the polymer. Therefore, the chemical mechanical polishing abrasive particles with the porous structure have better elasticity and toughness and lower hardness, the surface of the chemical mechanical polishing abrasive particles can also realize the regulation and control of different electronic groups such as amino groups, hydroxyl groups, carboxyl groups and the like, and the abundant surface group regulation and control can further improve the chemical properties (such as hardness reduction and elasticity improvement) of the chemical mechanical polishing abrasive particles, so that the chemical mechanical polishing abrasive particles can reduce the scratch of a polished part in the chemical mechanical planarization process. In addition, the baked product (carbon material) of the polymer still maintains a porous structure, which can improve the flatness of the polishing member during chemical mechanical polishing and reduce scratches of the polishing member. Specifically, in the chemical mechanical planarization process, the polymer or the baked product thereof rubs on the polished member, and because the hardness of the particles is relatively low, the toughness is good, the risk of breakage in the polishing process is low, so that scratches of the polished member can be reduced, in addition, the density of the polymer or the baked product thereof is low, better suspension property and fluidity are shown, and further, the flatness of the polished member is improved in the polishing process.
According to the invention, the polymers are selected on the basis of: the hardness and density of the obtained chemical mechanical polishing abrasive particles are smaller than those of inorganic oxide.
In some embodiments, the polymer comprises at least one of urea formaldehyde resin, phenolic resin, polymethyl methacrylate, poly (N-isopropylacrylamide-methacrylic acid), epoxy resin. Thus, the polymer can be used as a chemical mechanical polishing material.
Optionally, the polymer is urea formaldehyde resin.
In some embodiments, the firing is performed under an inert atmosphere at a firing temperature of 500 ℃ to 800 ℃, e.g., 500 ℃, 600 ℃, 700 ℃, 800 ℃, and the like. Thus, the degree of carbonization can be controlled, and a carbon material having a certain mechanical strength can be obtained.
Alternatively, the calcination time is 4h-8h, e.g. 4h, 5h, 6h, 7h, 8h.
In some embodiments, the chemical mechanical polishing abrasive particles have a diameter of 10nm to 300nm.
Further, the chemical mechanical polishing abrasive particles are polymers, and the average diameter of the polymers is 20nm-300nm.
Further, the chemical mechanical polishing abrasive particles are calcined products of a polymer, the calcined products of the polymer are carbon materials, and the average diameter of the carbon materials is 10nm-100nm.
In some embodiments, the chemical mechanical polishing abrasive particles have a specific surface area of 200m 2 /g-400m 2 /g, e.g. 200m 2 /g、232m 2 /g、290m 2 /g、400m 2 /g, etc. Therefore, the elasticity of the chemical mechanical polishing abrasive particles can be improved, the hardness can be reduced, and the polishing rate can be improved.
In a second aspect, the present invention provides a method of preparing a chemical mechanical polishing abrasive comprising the steps of:
(1) Mixing the solution A containing the silicon dioxide nano particles and a silane coupling agent with a first reaction group, and performing first aging to form a solution B containing silicon dioxide modified by the silane coupling agent;
(2) Mixing the solution B with a polymerizable organic compound having a second reactive group, and performing second aging to react the first reactive group with the second reactive group to form a solution C containing first polishing particles of an organic-inorganic doped structure;
(3) Mixing the solution C with an etching solution to etch silicon dioxide in the first polishing particles to form a solution D of second polishing particles comprising a porous polymer;
(4) And (3) carrying out solid-liquid separation, drying and optionally roasting on the solution D to obtain the chemical mechanical polishing abrasive particles with the porous structure.
The method is simple to operate, the silicon dioxide nano particles are used as a hard template agent, the surface of the hard template agent is modified by the silane coupling agent, then the silane coupling agent is reacted with the polymerizable organic matter with the second reactive group to obtain the polymer, the polymer wraps the hard template agent, finally, the hard template agent is removed by etching, and a porous structure is left in the polymer to form the polymer with the porous structure. Optionally, the polymer is carbonized by firing to further form a porous carbon material. Thus, the prepared polishing abrasive particles comprising the porous structure organic matter can improve the flatness of the polishing member during the chemical mechanical polishing process and reduce the scratches of the polishing member.
According to the present invention, in step (1), a solution a containing silica nanoparticles and a silane coupling agent having a first reactive group are mixed and subjected to a first aging to form a solution B containing silane coupling agent-modified silica.
In some embodiments, the first aging is performed under stirring conditions to modify the silica with a silane coupling agent having a first reactive group.
Further, the temperature of the first aging is 35 ℃ to 70 ℃. Therefore, the first aging is facilitated to be smoothly carried out, the agglomeration of the silicon dioxide nano particles is reduced, and the silicon dioxide modified by the silane coupling agent is formed.
Further, the time for the first aging is 1h to 4h, for example, 1h, 2h, 3h, 4h, etc.
In some embodiments, step (1) further comprises: mixing alkaline solvent with the orthosilicic acid solution, and aging for 0.5h-4h at 45-85 ℃ to prepare solution A.
Alternatively, the alkaline solvent has a pH of 9.5-10.5.
Alternatively, the alkaline solvent is an aqueous solution of a base. The base includes at least one of sodium hydroxide, potassium hydroxide, lithium hydroxide, magnesium hydroxide, calcium hydroxide, ammonia, oxazine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, ethanolamine, triethylenediamine, diethylenetriamine hexamethylenetetramine, hexamethyleneimine, triethylenediamine, cycloethyleneimine, morpholine, piperazine, and cyclohexylamine.
Optionally, the mass concentration of the orthosilicic acid in the orthosilicic acid solution is 2% -7%.
As some specific examples, the preparation of an orthosilicic acid solution using a silicone source, comprising: the organosilicon source is added into an acidic aqueous solution with the pH value of 2-4 for aging for 0.5-2 h. Wherein the organosilicon source comprises at least one of tetramethoxysilane, tetraethoxysilane, and tetrapropoxysilane.
As other specific examples, the preparation of an orthosilicic acid solution using an inorganic silicon source includes: the aqueous solution of inorganic silicon source is passed through strong ion exchange resin to obtain orthosilicic acid solution. Wherein the inorganic silicon source comprises at least one of potassium silicate, sodium silicate, and sodium metasilicate.
In some embodiments, the silane coupling agent having a first reactive group has the formula Y-R 1 -L-Si(OR) 3 Wherein R represents a C1-C4 alkyl group, R 1 Represents a single bond, C1-C5 alkylene (e.g. -CH 2 -、-CH 2 CH 2 、-CH 2 CH 2 CH 2 -、-CH 2 CH 2 CH 2 CH 2 (-), L represents a single bond or-OCH 2 -Y represents said first reactive group and comprises an epoxy, vinyl, ureido or mercapto group.
As some examples, the silane coupling agent having a first reactive group includes at least one of 3-ureidopropyltriethoxysilane, vinyltriethoxysilane, and gamma- (2, 3-glycidoxy) propyltrimethoxysilane.
In the step (1), the amount of the silane coupling agent may be selected according to the amount of the hard template agent. Generally, the mass ratio of the silane coupling agent to the silica nanoparticles is (0.01-0.5) to 1.
According to the present invention, in the step (2), the B solution is mixed with a polymerizable organic substance having a second reactive group, and a second aging is performed to react the first reactive group with the second reactive group, thereby forming a C solution of the first polishing particles having an organic-inorganic doping structure.
In some embodiments, the polymerizable organic having a second reactive group includes at least one of methyl methacrylate, methacrylic acid, isopropyl acrylamide, formaldehyde, ethylene oxide, propylene oxide, and phenol. Thus, on the one hand, these polymerizable monomers are polymerized with the Y groups of the silane coupling agent via the respective second reactive groups to form a polymer, and on the other hand, the formed polymer has a lower hardness, which reduces the risk of scratching the polished part during polishing.
It will be appreciated that the second reactive group and its corresponding polymerisable organic species (monomer) may be selected in dependence on the type of first reactive group.
As some examples, the first reactive group is an ureido group and the second reactive group is an aldehyde group. The silane coupling agent with urea groups and the polymerizable organic matter with aldehyde groups are polymerized for 0.5h-3h at room temperature under the condition that the pH value is 2-6, so as to form urea-formaldehyde resin.
In the step (2), the amount of the polymerizable organic compound may be selected according to the amount of the silane coupling agent. Generally, the molar ratio of silane coupling agent to polymerizable organic is 1: (0.7-1.3). Therefore, the chemical mechanical polishing abrasive with moderate specific surface area can be obtained, and the agglomeration of the abrasive is reduced.
According to the present invention, in step (3), the C solution is mixed with an etching solution to remove silica in the first polishing particles by etching, forming a D solution of second polishing particles including a porous polymer.
In the step (3), optionally, the etching reaction time is 4-6 h. Therefore, the silicon dioxide is completely removed, and the waste of etching liquid materials is avoided as much as possible.
It will be appreciated that the end of the etching reaction is based on complete dissolution of the silicon oxide.
Alternatively, the temperature of the etching reaction is 70 ℃ to 95 ℃. Therefore, the template agent is etched away, and the aim of adjusting the hardness of the chemical mechanical polishing abrasive particles is fulfilled, so that scratches in the polishing process are reduced, the etching rate is improved, and in addition, the decomposition of organic matters in the etching reaction process is reduced in the temperature range.
In the step (3), the etching liquid can be selected according to the type of the material of the first polishing particles, and only the silicon dioxide in the first polishing particles is etched and removed, and the etching liquid does not react with the polymer. In some embodiments, the etching solution includes at least one of an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous lithium hydroxide solution, an aqueous magnesium hydroxide solution, an aqueous calcium hydroxide solution, an aqueous ammonia solution, and an aqueous hydrofluoric acid solution.
Optionally, the etching solution is an aqueous solution of hydrofluoric acid, and the concentration of HF is 5wt% to 15wt%.
In the step (3), the amount of the etching solution may be selected according to the amount of the hard template. Generally, the mass ratio of the silicon dioxide nano particles to the etching solution is 1:1-5.
According to the present invention, in step (4), the D solution is filtered, washed, dried, and optionally calcined to obtain chemical mechanical polishing abrasive grains having a porous structure.
Typically, the solid-liquid separation includes centrifugation and filtration.
Further, the method also comprises the step of washing the product after solid-liquid separation, wherein the washing is to wash the separated product by adopting ethanol solution.
Generally, the temperature of the drying may be 60℃to 100℃such as 60℃80℃100 ℃.
In step (4), baking may or may not be included after baking. The porous polymer may be further carbonized by the firing to form a porous carbon material.
The conditions of the calcination may be selected according to the type of polymer, so long as the polymer is carbonized to form a carbon material.
In some embodiments, the temperature of calcination is 500 ℃ to 800 ℃, e.g., 500 ℃, 600 ℃, 700 ℃, 800 ℃, etc. Thereby, the organic matter is carbonized to form the carbon material while saving the cost.
Alternatively, the calcination time is 4h-8h, e.g., 4h, 6h, 7h, 8h, etc.
Optionally, the inert atmosphere is nitrogen.
As a specific example, referring to fig. 1, a method of preparing the composite polishing abrasive particle includes:
s1: mixing an alkaline solvent with the pH value of 9.5-10.5 with an orthosilicic acid solution, and aging for 1.5-4h at 45-85 ℃ to prepare an A solution containing silica nanoparticles;
s2: mixing the solution A containing the silicon dioxide nano particles and a silane coupling agent with a first reaction group, and performing first aging to form a solution B containing silicon dioxide modified by the silane coupling agent;
s3: mixing the solution B with a polymerizable organic compound having a second reactive group, and performing second aging to react the first reactive group with the second reactive group to form a solution C containing first polishing particles of an organic-inorganic doped structure;
s4: mixing the solution C with an etching solution to etch silicon dioxide in the first polishing particles to form a solution D of second polishing particles comprising a porous polymer;
s5: and (3) carrying out solid-liquid separation, washing, drying and optionally roasting on the solution D to obtain the chemical mechanical polishing abrasive particles with the porous structure.
In the method of the present invention, the porous chemical mechanical polishing abrasive particles comprise polymers and/or calcined products of the polymers, and scratches on the polishing article can be reduced during chemical mechanical polishing due to the porous and elastic properties of the polymers and/or calcined products of the polymers. Therefore, the organic substance having a porous structure has a great advantage in reducing scratches of the polishing member.
In a third aspect of the present invention, there is provided a polishing slurry comprising the chemical mechanical polishing abrasive particles of the first aspect of the present invention. The polishing solution is particularly suitable for the chemical mechanical planarization process of polishing pieces and can reduce scratches of the polishing pieces.
In some embodiments, the polishing solution may be obtained by formulating the chemical mechanical polishing abrasive particles as an aqueous solution having a mass concentration of 1% -5% and adjusting the pH to 4-10.5.
The following description of the present invention is made by way of specific examples, which are given for illustration of the present invention and should not be construed as limiting the scope of the invention.
The following examples illustrate the chemical mechanical polishing abrasive particles and methods of making the same.
Example 1
Mixing 100g of sodium hydroxide aqueous solution with the pH of 10.5 with 300g of orthosilicic acid solution with the mass fraction of 4.5 percent (calculated as silicon dioxide), and aging for 2 hours at the temperature of 75 ℃ to obtain solution A containing silicon dioxide nano particles;
heating the solution A to 45 ℃, adding 13.56g of 3-urea propyl triethoxysilane under the condition of strong stirring, and then stirring and aging for 2 hours, and marking as a solution B;
cooling the solution B to room temperature, then adopting a 4wt% hydrochloric acid solution, adjusting the pH of the solution B to 2.5, adding 6.14g of formaldehyde aqueous solution (the mass concentration of formaldehyde is 37%), and then stirring and aging for 1h to form a solution C of first polishing particles containing an organic-inorganic doping structure;
adding 20g of HF solution with the mass fraction of 10% into the solution C, and etching for 5 hours at the temperature of 85 ℃ to obtain solution D of second polishing particles comprising porous urea resin;
filtering, washing and drying the solution D (the temperature is 60 ℃) to obtain the urea-formaldehyde resin with the porous structure.
Examples 2 to 3
A porous urea-formaldehyde resin was prepared in the same manner as in example 1 except that the addition amounts of 3-ureidopropyltriethoxysilane were adjusted to 17.19g and 25.12g, respectively, as shown in Table 1.
Examples 4 to 6
A porous urea-formaldehyde resin was prepared in the same manner as in example 1 except that the addition amounts of the aqueous formaldehyde solutions were adjusted to 1.5g, 4.3g and 15g, respectively, as shown in Table 1.
Examples 7 to 10
A porous urea-formaldehyde resin was prepared in the same manner as in example 1 except that 100g of the porous urea-formaldehyde resin was calcined in a nitrogen atmosphere for 4 hours at 300℃at 500℃at 800℃at 950℃to give a calcined product of the urea-formaldehyde resin as a carbon material, as shown in Table 1.
Comparative example 1
The preparation method of the spherical silicon dioxide (43 nm) polishing abrasive particles mainly comprises the steps of dropwise adding 500g of sodium silicate solution with the mass fraction of 10%, mixing with NaOH aqueous solution with the pH of 10.5, controlling the dropwise adding rate to be 1mL/min, and aging at 90 ℃ to obtain the particles with the average particle diameter of 43 nm.
TABLE 1
Note that: the amounts of the "polymerizable organic" columns in Table 1 are the aqueous nail aldehyde solutions.
Test case
(1) Characterization of specific surface area and diameter of chemical mechanical polishing abrasive particles
Specific surface area: n (N) 2 The adsorption and desorption method was used for the test.
Diameter: the incident angle of the light source was 173 deg. at normal temperature by dynamic light scattering test.
(2) Polishing effect test
1) Preparation of polishing liquid
Polishing solution 1: and preparing a polishing solution with the mass fraction of 2% of the chemical mechanical polishing abrasive particles by using deionized water, and adjusting the pH value of the polishing solution to 8.5 by using a KOH aqueous solution.
2) Silicon wafer scratch detection
Polishing test is carried out on a 4-inch silicon wafer by using a G & P polishing machine poly500, the polishing pressure is 3.5psi, the polishing pad is IC1000, the rotation speeds of a polishing head and the polishing pad are respectively 60/65rpm, and the flow rate of polishing feeding is 50mL/min; polishing time was 2min, and scratches of the polished silicon wafer were detected.
The test results are shown in Table 2.
TABLE 2
As can be seen from the above table, the porous organic material provided by the present invention can reduce scratches of the polishing member.
Compared with examples 1-3, it can be seen that if the amount of the silane coupling agent is large, the specific surface area of the chemical mechanical polishing abrasive particles is reduced, and the diameter is increased, because the silane coupling agent has high bond and proportion on the surface of silicon dioxide, so that the silicon dioxide nano particles are unstable, agglomeration occurs, the formation of organic matters is further reduced, and scratches on the surface of a polished part in the polishing process are increased. If the amount of the silane coupling agent is small, the amount of bonded silica is reduced, and the excessive silica increases the hardness of the product, thereby increasing scratches on the surface of the polishing member during polishing.
Examples 4-6 are compared to example 1, and it can be seen that the use of a relatively low amount of formaldehyde results in a relatively low polymer content in the cmp abrasive particles, resulting in a reduction in the specific surface area of the particles, which increases the scratches on the surface of the polished part during polishing. When the formaldehyde content is too high, the chemical mechanical polishing abrasive grains have a relatively high specific surface area but are severely agglomerated, thereby increasing scratches on the surface of the polishing member during polishing.
Examples 7-9 compared to example 1, it can be seen that when the firing temperature is below 500 ℃, the specific surface area of the particles decreases, and this is mainly because some of the polymer therein is not carbonized, resulting in particles whose specific surface area is relatively low, whereas as the firing temperature increases, the specific surface area of the product increases.
Comparative example 1 it can be seen that the chemical mechanical polishing abrasive grains of the present invention have a larger specific surface and can reduce scratches of a polishing article as compared with example 1.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. All patents and publications referred to herein are incorporated by reference in their entirety. The terms "comprising" or "including" are used in an open-ended fashion, i.e., including the teachings described herein, but not excluding additional aspects.
In the description of the present specification, reference to the term "one embodiment," "another embodiment," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment is included in at least one embodiment of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction. In addition, it should be noted that, in this specification, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (17)
1. A chemical mechanical polishing abrasive particle, characterized in that the chemical mechanical polishing abrasive particle has a porous structure, and the material of the chemical mechanical polishing abrasive particle comprises a polymer and/or a calcined product of the polymer.
2. The chemical mechanical polishing abrasive particle of claim 1, wherein the polymer comprises at least one of urea formaldehyde resin, phenolic resin, polymethyl methacrylate, poly (N-isopropylacrylamide-methacrylic acid), epoxy resin.
3. The chemical mechanical polishing abrasive particle according to claim 1, wherein the firing is performed in an inert atmosphere at a firing temperature of 500 ℃ to 800 ℃ for a time of 4 hours to 8 hours.
4. The chemical mechanical polishing abrasive particle according to claim 1, wherein the chemical mechanical polishing abrasive particle has a diameter of 10nm to 300nm.
5. The chemical mechanical polishing abrasive particle according to claim 1, wherein the chemical mechanical polishing abrasive particle has a specific surface area of 200m 2 /g-400m 2 /g。
6. A method of preparing the chemical mechanical polishing abrasive according to any one of claims 1 to 5, comprising the steps of:
(1) Mixing the solution A containing the silicon dioxide nano particles and a silane coupling agent with a first reaction group, and performing first aging to form a solution B containing silicon dioxide modified by the silane coupling agent;
(2) Mixing the solution B with a polymerizable organic compound having a second reactive group, and performing second aging to react the first reactive group with the second reactive group to form a solution C containing first polishing particles of an organic-inorganic doped structure;
(3) Mixing the solution C with an etching solution to etch silicon dioxide in the first polishing particles to form a solution D of second polishing particles comprising a porous polymer;
(4) And (3) carrying out solid-liquid separation, drying and optionally roasting on the solution D to obtain the chemical mechanical polishing abrasive particles with the porous structure.
7. The method of claim 6, wherein step (1) further comprises: mixing an alkaline solvent with an orthosilicic acid solution, aging for 0.5h-4h at 45-85 ℃ to prepare the solution A, wherein,
the pH of the alkaline solvent is 9.5-10.5;
in the orthosilicic acid solution, the mass concentration of the orthosilicic acid is 2% -7%.
8. The method of claim 6, wherein the silane coupling agent has a formula of Y-R 1 -L-Si (OR) 3, wherein R represents a C1-C4 alkyl group, R 1 Represents a single bond, C1-C5 alkylene, L represents a single bond or-OCH 2 -Y represents said first reactive group and comprises an epoxy, vinyl, ureido or mercapto group;
the second reactive group includes a vinyl group, an epoxy group, or an aldehyde group.
9. The method of claim 6, wherein the polymerizable organic comprises at least one of methyl methacrylate, methacrylic acid, isopropyl acrylamide, formaldehyde, ethylene oxide, propylene oxide, and phenol;
the etching liquid comprises at least one of an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous lithium hydroxide solution, an aqueous magnesium hydroxide solution, an aqueous calcium hydroxide solution, an aqueous ammonia solution and an aqueous hydrofluoric acid solution.
10. The process according to any one of claims 6 to 9, wherein in step (1), the first aging is carried out under stirring for a period of time ranging from 1h to 4h and at a temperature ranging from 35 ℃ to 70 ℃.
11. The method according to any one of claims 6 to 9, wherein in step (1), the mass ratio of the silane coupling agent to the silica nanoparticles is (0.01 to 0.5) to 1.
12. The process according to any one of claims 6 to 9, wherein in step (2), the second ageing is carried out at room temperature under stirring for a period of time ranging from 0.5h to 3h;
the second aging has a pH of 2-6.
13. The method according to any one of claims 6 to 9, wherein in step (2), the molar ratio of the silane coupling agent to the polymerizable organic is 1: (0.7 to 1.3).
14. The method according to any one of claims 6 to 9, wherein in step (3), the etching reaction is carried out at a temperature of 70 ℃ to 95 ℃ for a time of 4 hours to 6 hours.
15. The method according to any one of claims 6 to 9, wherein in the step (3), the etching liquid is an aqueous hydrofluoric acid solution, and the concentration of hydrofluoric acid is 5wt% to 15wt%;
the mass ratio of the silicon dioxide nano particles to the etching solution is 1:1-5.
16. The method according to any one of claims 6 to 9, wherein the calcination is carried out in an inert atmosphere at a calcination temperature of 500 ℃ to 800 ℃ for a calcination time of 4h to 8h.
17. A polishing slurry comprising the chemical mechanical polishing abrasive particles according to any one of claims 1 to 5.
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