CN115058199A - High-dispersion ball-like nano cerium oxide polishing solution and application thereof - Google Patents
High-dispersion ball-like nano cerium oxide polishing solution and application thereof Download PDFInfo
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- CN115058199A CN115058199A CN202210989564.7A CN202210989564A CN115058199A CN 115058199 A CN115058199 A CN 115058199A CN 202210989564 A CN202210989564 A CN 202210989564A CN 115058199 A CN115058199 A CN 115058199A
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- Prior art keywords
- cerium oxide
- nano
- polishing solution
- acid
- solution
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Links
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 104
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 238000005498 polishing Methods 0.000 title claims abstract description 87
- 239000006185 dispersion Substances 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 102
- 239000002243 precursor Substances 0.000 claims abstract description 70
- 239000000843 powder Substances 0.000 claims abstract description 51
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 150000000703 Cerium Chemical class 0.000 claims abstract description 28
- 238000001694 spray drying Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 21
- 230000001590 oxidative effect Effects 0.000 claims abstract description 19
- 239000007800 oxidant agent Substances 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 238000010008 shearing Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- 230000007935 neutral effect Effects 0.000 claims abstract description 9
- 238000007670 refining Methods 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 239000012716 precipitator Substances 0.000 claims abstract description 7
- 238000009826 distribution Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 29
- 229910052710 silicon Inorganic materials 0.000 claims description 29
- 239000010703 silicon Substances 0.000 claims description 29
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 26
- 235000002639 sodium chloride Nutrition 0.000 claims description 19
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 229910002651 NO3 Inorganic materials 0.000 claims description 9
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 239000008139 complexing agent Substances 0.000 claims description 7
- 229960001484 edetic acid Drugs 0.000 claims description 7
- -1 polyoxyethylene Polymers 0.000 claims description 7
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004471 Glycine Substances 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 6
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000080 wetting agent Substances 0.000 claims description 6
- 238000004061 bleaching Methods 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 4
- 239000011736 potassium bicarbonate Substances 0.000 claims description 4
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 4
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 3
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 235000011148 calcium chloride Nutrition 0.000 claims description 2
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000011698 potassium fluoride Substances 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 235000019794 sodium silicate Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 claims 1
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 claims 1
- 235000021313 oleic acid Nutrition 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 36
- 238000010438 heat treatment Methods 0.000 description 24
- 235000012431 wafers Nutrition 0.000 description 22
- 239000007788 liquid Substances 0.000 description 19
- 229910021642 ultra pure water Inorganic materials 0.000 description 18
- 239000012498 ultrapure water Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 12
- 238000000926 separation method Methods 0.000 description 10
- 238000003921 particle size analysis Methods 0.000 description 8
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- 238000006243 chemical reaction Methods 0.000 description 7
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- 239000011164 primary particle Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 6
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- 239000011362 coarse particle Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920001030 Polyethylene Glycol 4000 Polymers 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 229910021529 ammonia Inorganic materials 0.000 description 1
- PGJHGXFYDZHMAV-UHFFFAOYSA-K azanium;cerium(3+);disulfate Chemical compound [NH4+].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O PGJHGXFYDZHMAV-UHFFFAOYSA-K 0.000 description 1
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- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a high-dispersion quasi-spherical nano cerium oxide polishing solution and application thereof, wherein the polishing solution comprises quasi-spherical nano cerium oxide powder; the preparation method of the sphere-like nano cerium oxide powder comprises the following steps: (1) mixing tetravalent cerium salt with a polyvinylpyrrolidone solution to prepare a cerium salt solution, adding a precipitator and an oxidant, and shearing at a high speed at 70-90 ℃ until precipitates are generated to prepare precursor slurry; (2) washing the precursor slurry to be neutral, then carrying out spray drying to obtain a cerium oxide precursor, adding auxiliary molten salt into the cerium oxide precursor, refining the material, and carrying out spray drying again; (3) and calcining the obtained material to obtain the nano cerium oxide powder. The obtained product has controllable particle size, uniform appearance, narrow particle size distribution range and extremely high dispersity, can not scratch the surface of a polished part, and can more easily obtain a surface with low roughness.
Description
Technical Field
The invention relates to the technical field of ultra-precision processing of semiconductors, in particular to a high-dispersion spherical nano cerium oxide polishing solution and application thereof.
Background
With the rapid development of integrated circuit technology, the size of semiconductor silicon wafers is continuously enlarged, the diameter of the largest silicon wafer is increased to 300mm at present, and the total number of chips in the edge range occupies a large proportion, so that the processing quality of the edge of the silicon wafer directly affects the total number of chips and the yield of the whole silicon wafer, and the requirement on the edge of a silicon wafer substrate is higher and higher. Chemical Mechanical Polishing (CMP) is the most popular semiconductor material surface planarization technology at present, and is a process combining mechanical friction and chemical corrosion, and combines the advantages of both, so as to obtain a relatively perfect wafer surface.
At present, the mainstream large-size silicon wafer polishing method still adopts three steps of rough polishing, middle polishing and fine polishing. In the rough polishing process, the removal efficiency of the polishing solution is required to be improved as much as possible while the surface quality of the silicon wafer is ensured.
In contrast, cerium oxide has been widely reported as an abrasive for chemical mechanical polishing slurry for semiconductors. Chinese patent CN112908834A discloses that nano cerium oxide with different particle sizes is applied to rapid green environmental protection double-side polishing of silicon wafer substrates, but it can only reduce the distribution of coarse particles by controlling the solid content of slurry, and the solid content is high, and the removal efficiency and surface quality can not be guaranteed. WO2007046420a1 discloses a cerium oxide slurry, a cerium oxide polishing solution, and a method of polishing a substrate using the same, which provide a cerium oxide slurry, a cerium oxide polishing solution, and a method of polishing a substrate using the same, which achieve reduction of polishing damage and increase of polishing speed by reducing the content ratio of coarse particles by maximizing the dispersibility of cerium oxide particles. In the two methods, the content ratio of coarse particles is reduced by improving the dispersibility, so that large particles cannot be fundamentally removed, and the problem of scratches still exists in the using process.
Therefore, it is important to research to improve the polishing effect by synthesizing the sphere-like nano cerium oxide powder with controllable particle size, uniform morphology and excellent dispersibility into the polishing solution.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-dispersion spherical nano cerium oxide polishing solution, which is prepared by preparing spherical nano cerium oxide with controllable particle size, uniform appearance and extremely high dispersibility, and then taking the cerium oxide as a CMP polishing solution of an abrasive, so that the stability of the polishing solution is improved, and a high-precision surface type effect can be obtained in the polishing of silicon-containing solids.
The technical scheme of the invention is as follows:
the preparation of the nanometer cerium oxide powder comprises the following steps:
(1) mixing tetravalent cerium salt with polyvinylpyrrolidone water solution (with concentration of 5-30%) to obtain cerium salt solution, adding precipitant and oxidant with bleaching property, and shearing at high speed at 70-90 deg.C until precipitate is generated to obtain precursor slurry;
(2) washing the precursor slurry to be neutral, then carrying out spray drying to obtain a cerium oxide precursor, adding an auxiliary molten salt into the cerium oxide precursor, refining the material (the particle size D50 is 1um +/-0.2 um) by ball milling and the like, and carrying out spray drying again;
(3) and (3) calcining the material obtained in the step (2) to obtain the nano cerium oxide powder.
Preferably, the molten salt is at least one of ammonium chloride, sodium chloride, potassium chloride, sodium fluoride, ammonium carbonate, sodium carbonate, potassium fluoride, sodium silicate, potassium silicate, sodium sulfate, potassium sulfate and calcium chloride.
Preferably, the tetravalent cerium salt is a carbonate, oxalate, acetate, nitrate or sulfate, as well as mixtures of these salts.
Preferably, the tetravalent cerium salt is one or more of cerium iv nitrate, ammonium cerium sulfate and cerium iv sulfate.
Preferably, the precipitant is at least one of potassium hydroxide, ammonium bicarbonate, potassium bicarbonate, ammonia, ethylenediamine, and hexamethylenediamine.
Preferably, the polyvinylpyrrolidone is: one or more of PVPK15, PVPK30, PVPK60 and PVPK 90.
Preferably, the oxidizing agent is one or more than two of hypochlorous acid, potassium hypochlorite, sodium hypochlorite, calcium hypochlorite and potassium persulfate.
Preferably, the concentration of the cerium salt solution in the step (1) is 0.5-5 mol/L; the molar ratio of the cerium salt to the precipitant and the oxidant is (0.5-5): (0.5-1.5): (0.01 to 0.05); the molar ratio of the fluxing molten salt to the tetravalent cerium salt is 0.01-20: 1.
Preferably, the calcining temperature in the step (3) is 600-850 ℃.
Preferably, the calcination process is: the temperature is raised from room temperature to 400 ℃ at the rate of 0.1 to 50 ℃/min; the temperature rise rate is 0.1-50 ℃/min from 400-850 ℃; roasting for 20-200 min; cooling; the temperature of the spray drying in the step (2) is 230 +/-50 ℃.
Preferably, the particle size of D50 in the particle size distribution of the sphere-like nano cerium oxide powder is 0.08-0.15 um, the particle size of D90 is 0.15-0.25 um, and PDI is less than or equal to 0.1.
Preparing a nano cerium oxide polishing solution: mixing the nanometer cerium oxide powder, an acidic pH regulator, a dispersing agent, a wetting agent, a complexing agent and water, and shearing and dispersing at a high speed to obtain the product.
Preferably, the nano spheroidal cerium oxide powder accounts for 0.01 to 10 percent in weight percentage; 0.01 to 2 percent of dispersant; 0.1 to 20 percent of wetting agent; 0.01 to 2 percent of complexing agent; 0.1 to 2 percent of acidic pH regulator; the balance being water.
Preferably, the nano spheroidal cerium oxide abrasive is 0.2 to 6 percent by weight; 0.1 to 1 percent of dispersant; 0.2 to 10 percent of wetting agent; 0.2 to 1 percent of complexing agent; 0.2 to 1 percent of acidic pH regulator; the balance of water; the pH of the polishing solution is 3.5-5.5.
Preferably, the dispersant is: polyvinyl pyrrolidone (PVPK 30, PVPK 60), polyethylene glycol (PEG 4000 or PEG6000), polyacrylic acid and its salt, and alkylphenol ethoxylate.
Preferably, the acidic pH regulator is one or more of tartaric acid, oxalic acid, acetic acid, glycine, citric acid, succinic acid, salicylic acid, oleic acid, acetic acid or ascorbic acid, and the pH value of the polishing solution is controlled to be 4.0-5.0.
Preferably, the complexing agent is one or more of hydroxyethylidene diphosphonic acid and salts thereof, ethylene diamine tetraacetic acid and salts thereof, oxalic acid, potassium pyrophosphate and potassium thiosulfate.
Preferably, the humectant is at least one of ethanol, propylene glycol, glycerol, ethylene glycol, dimethyl sulfoxide, tween-80 and diethylene glycol.
The sphere-like nano cerium oxide polishing solution is applied to polishing of silicon-containing solids. The silicon-containing solid includes a silicon-containing film, a silicon wafer, precision optical glass, and the like formed on a semiconductor substrate.
The existing domestic nano cerium oxide polishing solution has poor dispersibility, PDI (polymer induced degradation) can not reach below 0.1, and high requirements on polishing precision and polishing surface type can not be met. The invention uses hypochlorous acid and persulfuric acid strong oxidants with bleaching property to control over precursor Ce (OH) 4 Morphology, by flux recombination precursor Ce (OH) 4 The particle size of the nano cerium oxide powder is controlled by roasting, the obtained product has controllable particle size and uniform appearance, and the obtained cerium oxide polishing solution has good dispersibility after high-speed shearing and dispersion liquid preparation. The CMP polishing solution taking the cerium oxide as the abrasive improves the stability of the polishing solution, realizes high cutting amount and high surface quality of the polishing solution, can be applied to polishing of silicon-containing solid, and particularly shows excellent planarization polishing precision in polishing of silicon oxide film silicon wafer slices and precision optical glass.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method is simple, the synthesis reaction time is long, the reaction is easy to control, the single-particle primary particle size of the sphere-like nano cerium oxide is controllable between 15 and 200nm, the sphericity is high, and the distribution is narrow.
(2) The polishing solution prepared by the method for preparing the nano cerium oxide powder has extremely high dispersibility and strong fluidity, and a surface with low roughness can be obtained more easily.
(3) The polishing solution prepared by dispersing the ball-like nano cerium oxide is extremely easy to disperse, can well control large D90 particles, and ensures the stability of the polishing solution, thereby ensuring that the surface of a polished part is not scratched, and more easily obtaining the surface shape effect with high precision.
Drawings
FIG. 1 shows the results of laser particle size analysis of the powder obtained in example 1 after dispersion; where the curve corresponds to the left accumulation (%), the bar corresponds to the right frequency (%), and the same is true below.
FIG. 2 shows the results of X-ray diffraction analysis of the powder obtained in example 1.
FIG. 3 shows the results of SEM analysis of the powder obtained in example 1.
FIG. 4 shows the results of SEM analysis of the powder obtained in example 2.
FIG. 5 shows the results of SEM analysis of the powder obtained in example 3.
FIG. 6 shows the results of SEM analysis of the powder obtained in example 4.
FIG. 7 shows the results of SEM analysis of the powder obtained in example 5.
FIG. 8 shows the results of SEM analysis of the powder obtained in example 6.
Fig. 9 is a roughness measurement chart of the polished blank wafer of example 1.
FIG. 10 shows the results of laser particle size analysis of the powder obtained in example 2 after dispersion.
FIG. 11 shows the results of laser particle size analysis of the powder obtained in example 3 after dispersion.
FIG. 12 shows the results of laser particle size analysis of the powder obtained in example 4 after dispersion.
FIG. 13 shows the results of laser particle size analysis of the powder obtained in example 5 after dispersion.
FIG. 14 shows the results of laser particle size analysis of the powder obtained in example 6 after dispersion.
FIG. 15 shows the results of laser particle size analysis of the powder obtained in comparative example 1 after dispersion.
FIG. 16 shows the results of laser particle size analysis of the powder obtained in comparative example 2 after dispersion.
FIG. 17 is a flow chart of the powder production method of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
Example 1
Preparing nano cerium oxide powder:
(1) preparing raw materials: a10 wt% polyvinylpyrrolidone (PVPK 30) solution diluted by ultrapure water is used as a dispersant solution medium, and a cerium nitrate and ammonium ceric nitrate mixed mother cerium salt solution with the concentration of 2.0mol/L and the concentration of 0.36mmol/L, a potassium hydroxide precipitator solution with the concentration of 0.5mol/L, pH of 12 and a potassium persulfate oxidant solution with the concentration of 0.1mol/L are prepared.
(2) Reaction: adding the cerium salt mixed solution at a flow rate of 1L/min, the potassium hydroxide solution at a flow rate of 1.5L/min and the potassium hypochlorite solution at a flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating the tank to 80 ℃, and generating precipitates under the action of high-speed shearing (the rotating speed is 3000 r/min) to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and separating by high-speed centrifugation (the centrifugation speed is 12000 r/min) to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃ for 90min, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: adding ammonium chloride (the molar ratio of the ammonium chloride to the tetravalent cerium salt is 2.5: 1) according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material (the granularity D501 um) in a sand grinding manner, and performing spray drying in the step (4) again.
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min at the heating rate of 9 ℃/min; the temperature is 400-800 ℃, the time is 100min, and the heating rate is 4 ℃/min; oxidizing and roasting at 800 ℃ for 40 min; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The primary particle size of the nano-cerium oxide powder prepared in this example was 100nm on average.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of polyvinylpyrrolidone K30, 0.3g of ethylenediamine tetraacetic acid and 5g of tween-80 into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of glycine and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the materials are uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Example 2
Preparing nano cerium oxide powder:
(1) preparing raw materials: a10 wt% polyvinylpyrrolidone (PVPK 30) solution diluted by ultrapure water is used as a dispersant solution medium, and a cerium nitrate and ammonium ceric nitrate mixed mother cerium salt solution with the concentration of 2.0mol/L and the concentration of 0.36mmol/L, a potassium hydroxide precipitator solution with the concentration of 0.5mol/L, pH of 12 and a potassium persulfate oxidant solution with the concentration of 0.1mol/L are prepared.
(2) Reaction: adding the cerium salt mixed solution with the flow rate of 1L/min, the potassium hydroxide solution with the flow rate of 1.5L/min and the potassium hypochlorite solution with the flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating at the temperature of 80 ℃, rotating at the speed of 3000r/min, and generating a precipitate under the action of high-speed shearing to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and then carrying out high-speed centrifugal separation to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: and (3) adding sodium chloride according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material in a sand grinding mode, and performing spray drying in the step (4) again.
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min at the heating rate of 9 ℃/min; at the temperature of 400-750 ℃, the time is 100min, and the heating rate is 3.5 ℃/min; oxidizing and roasting at 750 deg.c for 40 min; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The primary particle size of the nano cerium oxide powder prepared in this example was 30nm on average.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of polyethylene glycol PEG4000, 0.3g of ethylene diamine tetraacetic acid and 5g of ethylene glycol into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of tartaric acid and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the materials are uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Example 3
Preparing nano cerium oxide powder:
(1) preparing raw materials: a10 wt% polyvinylpyrrolidone (PVPK 30) solution diluted with ultrapure water was used as a dispersant solution medium to prepare a cerium nitrate solution having a concentration of 2.0mol/L and a cerium ammonium nitrate solution having a concentration of 0.36mmol/L, a potassium hydroxide precipitant solution having a concentration of 0.5mol/L, pH of 12, and a potassium hypochlorite oxidant solution having a concentration of 0.1 mol/L.
(2) Reaction: adding a cerium salt mixed solution with a flow rate of 1L/min, a potassium hydroxide solution with a flow rate of 1.5L/min and a calcium hypochlorite solution with a flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating at a temperature of 80 ℃ and a rotating speed of 3000r/min, and generating a precipitate under the action of high-speed shearing to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and then carrying out high-speed centrifugal separation to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: and (3) adding ammonium chloride according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material in a sand grinding mode, and performing spray drying in the step (4) again.
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min at the heating rate of 9 ℃/min; at the temperature of 400-650 ℃, the time is 80min, and the heating rate is 3.125 ℃/min; oxidizing and roasting for 30min at 650 ℃; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The primary particle size of the nano cerium oxide powder prepared in this example was 20nm on average.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of sodium polyacrylate, 0.3g of hydroxyethylidene diphosphonic acid and 5g of ethylene glycol into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of citric acid and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the slurry is uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Example 4
Preparing nano cerium oxide powder:
(1) preparing raw materials: a10 wt% polyvinylpyrrolidone (PVPK 30) solution diluted by ultrapure water is used as a dispersant solution medium, and a cerium nitrate and ammonium ceric nitrate mixed mother cerium salt solution with the concentration of 2.0mol/L and the concentration of 0.36mmol/L, a potassium bicarbonate precipitator solution with the concentration of 0.5mol/L, pH of 8 and a potassium persulfate oxidant solution with the concentration of 0.1mol/L are prepared.
(2) Reaction: adding a cerium salt mixed solution with a flow rate of 1L/min, a potassium bicarbonate solution with a flow rate of 1.5L/min and a sodium hypochlorite solution with a flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating at a temperature of 80 ℃ and a rotating speed of 3000r/min, and generating a precipitate under the action of high-speed shearing to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and then carrying out high-speed centrifugal separation to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: and (4) adding sodium silicate according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material in a sand grinding mode, and performing spray drying in the step (4).
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min, and the heating rate is 9 ℃/min; at the temperature of 400-850 ℃, the time is 40min, and the heating rate is 11.25 ℃/min; oxidizing and roasting for 30min at 850 ℃; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The nano cerium oxide powder prepared in this example has an average primary particle size of 200 nm.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of polyvinylpyrrolidone K30, 0.3g of ethylenediamine tetraacetic acid and 5g of dimethyl sulfoxide into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of citric acid and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the solution is uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Example 5
Preparing nano cerium oxide powder:
the invention differs from example 1 in that: potassium persulfate is used as an oxidizing agent.
(1) Preparing raw materials: a10 wt% polyvinylpyrrolidone solution diluted by ultrapure water is used as a dispersant solution medium, a cerium nitrate and ammonium ceric nitrate mixed mother cerium salt solution with the concentration of 2.0mol/L and the concentration of 0.36mmol/L, a potassium hydroxide precipitator solution with the concentration of 0.5mol/L, pH of 12 and a potassium persulfate oxidant solution with the concentration of 0.1mol/L are prepared.
(2) Reaction: adding a cerium salt mixed solution with the flow rate of 1L/min, a potassium hydroxide solution with the flow rate of 1.5L/min and a potassium persulfate solution with the flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating at the temperature of 80 ℃ and the rotating speed of 3000r/min, and generating a precipitate under the action of high-speed shearing to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and then carrying out high-speed centrifugal separation to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: and (3) adding ammonium chloride according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material in a sand grinding mode, and performing spray drying in the step (4) again.
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min at the heating rate of 9 ℃/min; the temperature is 400-800 ℃, the time is 100min, and the heating rate is 4 ℃/min; oxidizing and roasting at 800 ℃ for 40 min; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The primary particle size of the nano-cerium oxide powder prepared in this example was 80nm on average.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of polyvinylpyrrolidone K30, 0.3g of ethylenediamine tetraacetic acid and 5g of tween-80 into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of glycine and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the glycine and the nano cerium oxide slurry are uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Example 6
Preparing nano cerium oxide powder:
the invention differs from example 1 in that: sodium chloride is used as auxiliary molten salt.
(1) Preparing raw materials: a10 wt% polyvinylpyrrolidone (PVPK 30) solution diluted by ultrapure water is used as a dispersant solution medium, and a cerium nitrate and ammonium ceric nitrate mixed mother cerium salt solution with the concentration of 2.0mol/L and the concentration of 0.36mmol/L, a potassium hydroxide precipitator solution with the concentration of 0.5mol/L, pH of 12 and a potassium persulfate oxidant solution with the concentration of 0.1mol/L are prepared.
(2) Reaction: adding the cerium salt mixed solution at a flow rate of 1L/min, the potassium hydroxide solution at a flow rate of 1.5L/min and the potassium hypochlorite solution at a flow rate of 0.2L/min into a heating and stirring tank with a polytetrafluoroethylene lining, heating the tank to 80 ℃, and generating precipitates under the action of high-speed shearing (the rotating speed is 3000 r/min) to prepare precursor slurry.
(3) Washing and centrifuging: and washing the precursor slurry to be neutral, and separating by high-speed centrifugation (the centrifugation speed is 12000 r/min) to obtain precursor viscous liquid.
(4) Spray drying: and diluting the precursor viscous liquid, spray-drying the precursor viscous liquid at 230 ℃ for 90min, and performing cyclone separation to obtain a cerium oxide precursor.
(5) And (3) precursor composite drying: and (3) adding sodium chloride according to the mass ratio of 10% of the cerium oxide precursor, mixing and stirring, refining the material in a sand grinding mode, and performing spray drying in the step (4) again.
(6) Roasting: the precursor is heated at the temperature of between room temperature and 400 ℃ for 20min at the heating rate of 9 ℃/min; the temperature is 400-800 ℃, the time is 100min, and the heating rate is 4 ℃/min; oxidizing and roasting at 800 ℃ for 40 min; cooling to room temperature along with the furnace to obtain the nano cerium oxide powder.
The nano cerium oxide powder prepared in this example has an average primary particle size of 60 nm.
Preparing a nano cerium oxide polishing solution:
sequentially adding 3g of polyvinylpyrrolidone K30, 0.3g of ethylenediamine tetraacetic acid and 5g of tween-80 into 491.7g of ultrapure water, stirring at the temperature of 30 ℃ and the stirring speed of 500r/min until the materials are uniformly dissolved to prepare a premixed solution; then adding 5g of glycine and 25g of refined 20wt% nano cerium oxide slurry into 490g of ultrapure water, and stirring until the materials are uniformly dissolved; and finally, slowly pouring the premixed solution under the high-speed stirring of 10000r/min, and continuously stirring for 50min to ensure that the pH value is equal to 4.5, thus obtaining the nano cerium oxide polishing solution.
Comparative example 1
The difference from example 1 is that: the procedure of example 1 was otherwise the same as that of example 1 except that concentrated nitric acid having a concentration of 0.1mol/L was used as the oxidizing agent in place of the strong oxidizing agent having bleaching ability.
The cerous hydroxide precursor of comparative example 1 is subject to agglomeration and nucleation during the formation of precipitates, which results in precursor particles of varying sizes and insufficient sphericity. The strong oxidant with bleaching property can well play a role in inhibiting polymerization at a certain temperature, and simultaneously can ensure that crystal nuclei are more mellow.
And filtering the prepared polishing solution, and then polishing the silicon oxide film silicon wafer slices. The removal rate of silicon was found to be 3524.2A/min, the surface roughness was found to be 0.46nm, and no residue and no scratch were found on the silicon wafer surface.
Comparative example 2
The difference from example 1 is that: the procedure of example 1 was otherwise the same without using flux. And filtering the prepared polishing solution, and then polishing the silicon oxide film silicon wafer slices. The removal rate of silicon was found to be 3968.5A/min, the surface roughness was found to be 1.12nm, and no residue and no scratch were found on the silicon wafer surface.
Comparative example 3
The difference from example 1 is that: using an imported cerium oxide polishing solution: baikalox CP 10S.
And filtering the prepared polishing solution, and then polishing the silicon oxide film silicon wafer slices. The removal rate of silicon was found to be 3866.1A/min, the surface roughness was found to be 0.46nm, and no residue and no scratch were found on the silicon wafer surface.
Comparative example 4
The difference from example 1 is that: the solution preparation was carried out in the same manner as in example 1, except that commercially available nano-cerium oxide powder was used and the nano-cerium oxide was VK-Ce03, a new material, cheng jing rui co.
And filtering the prepared polishing solution, and then polishing the silicon oxide film silicon wafer slices. The removal rate of silicon was found to be 2884.7A/min, the surface roughness was found to be 0.58nm, and no residue or scratch was found on the silicon wafer surface.
The silicon oxide film silicon wafer slices have the same polishing conditions, and the polishing parameters are as follows: a Suzhou Heritl X62D 9B2M-T type polishing machine is used, the material of a polishing disc is damping cloth, the polishing pressure is 20kg, the polishing time is 10min, the rotating speed of the polishing disc is 25rpm, the rotating speed ratio of a central gear is 0.32, and the flow rate of chemical mechanical polishing slurry is 100 mL/min. The wafer slices used for polishing are all available from Shanghai Zhaxi electronics, Inc. The thickness of the silicon oxide film is measured by a spectrum ellipsometer-RC 2 of J.A. Woollam company, the removal rate of the silicon oxide film is obtained by dividing the thickness difference measured before and after polishing by the time consumed for polishing, and the polishing time is 1 minute. The particle size distribution profile was measured by the particle size in nanometers of Malverpa (UK) and by Zeta potential analyzer Zetasizer ultra. The roughness measuring method comprises the following steps: the area of the spot test area is 0.1um x 0.1um measured by ICON atomic force microscope of Bruker, USA. The test results are detailed in table 1 below.
TABLE 1
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A high-dispersion quasi-spherical nano cerium oxide polishing solution is characterized by comprising quasi-spherical nano cerium oxide powder; the preparation method of the sphere-like nano cerium oxide powder comprises the following steps:
(1) mixing tetravalent cerium salt with a polyvinylpyrrolidone solution to prepare a cerium salt solution, adding a precipitator and an oxidant with bleaching property, and shearing at a high speed at 70-90 ℃ until precipitates are generated to prepare precursor slurry;
(2) washing the precursor slurry to be neutral, then carrying out spray drying to obtain a cerium oxide precursor, adding an auxiliary molten salt into the cerium oxide precursor, refining the material, and carrying out spray drying again;
(3) and (3) calcining the material obtained in the step (2) to obtain the nano cerium oxide powder.
2. The polishing solution of claim 1, wherein the fluxing salt is at least one of ammonium chloride, sodium chloride, potassium chloride, sodium fluoride, ammonium carbonate, sodium carbonate, potassium fluoride, sodium silicate, potassium silicate, sodium sulfate, potassium sulfate, and calcium chloride;
the tetravalent cerium salt is one or more than two of carbonate, oxalate, acetate, nitrate and sulfate.
3. The highly dispersed ball-like nano cerium oxide polishing solution according to claim 2, wherein the precipitant is at least one of potassium hydroxide, ammonium bicarbonate, potassium bicarbonate, ammonia water, ethylenediamine and hexamethylenediamine;
the polyvinylpyrrolidone is: one or more of PVPK15, PVPK30, PVPK60 and PVPK 90;
the tetravalent cerium salt is one or more than two of cerium iv nitrate, ammonium ceric sulfate and cerium iv sulfate;
the oxidant is one or more of hypochlorous acid, potassium hypochlorite, sodium hypochlorite, calcium hypochlorite and potassium persulfate.
4. The highly dispersed ball-like nano cerium oxide polishing solution according to claim 3, wherein the concentration of the cerium salt solution in the step (1) is 0.5 to 5 mol/L; the molar ratio of the cerium salt to the precipitant to the oxidant is (0.5-5): (0.5-1.5): (0.01 to 0.05); the molar ratio of the fluxing molten salt to the tetravalent cerium salt is 0.01-20: 1.
5. The highly dispersed sphere-like nano cerium oxide polishing solution according to claim 4, wherein the temperature of the spray drying in the step (2) is 230 ± 50 ℃; the calcining temperature in the step (3) is 600-850 ℃; the calcining process comprises the following steps: the temperature is raised from room temperature to 400 ℃ at the rate of 0.1 to 50 ℃/min; the temperature rise rate is 0.1-50 ℃/min from 400-850 ℃; roasting for 20-200 min.
6. The highly dispersed cerium oxide-like nanoparticle polishing solution of claim 1, wherein the particle size distribution of the cerium oxide-like nanoparticle powder is 0.08-0.15 um in D50 particle size, 0.15-0.25 um in D90 particle size, and 0.1 or less in PDI.
7. The highly dispersed sphere-like nano cerium oxide polishing solution according to any one of claims 1 to 6, wherein the step (3) comprises the following components in percentage by weight:
0.01-10% of nano spheroidal cerium oxide powder; 0.01 to 2 percent of dispersant; 0.1 to 20 percent of wetting agent; 0.01 to 2 percent of complexing agent; 0.1 to 2 percent of acidic pH regulator; the balance being water.
8. The high dispersion sphere-like nano cerium oxide polishing solution according to claim 7, wherein in the step (3), the nano sphere-like cerium oxide abrasive is 0.2-6% by weight; 0.1 to 1 percent of dispersant; 0.2 to 10 percent of wetting agent; 0.2 to 1 percent of complexing agent; 0.2 to 1 percent of acidic pH regulator; the balance of water; the pH of the polishing solution is 3.5-5.5.
9. The highly dispersed sphere-like nano cerium oxide polishing solution according to claim 7, wherein the dispersant in the step (3) is: one or more of polyvinylpyrrolidone, polyethylene glycol, polyacrylic acid and its salts, and alkylphenol polyoxyethylene;
the acidic pH regulator is one or more of tartaric acid, oxalic acid, acetic acid, glycine, citric acid, succinic acid, salicylic acid, oleic acid, acetic acid and ascorbic acid, and the pH value of the polishing solution is controlled to be 4.0-5.0;
the complexing agent is one or more of hydroxyethylidene diphosphonic acid and salts thereof, ethylene diamine tetraacetic acid and salts thereof, oxalic acid, potassium pyrophosphate and potassium thiosulfate;
the wetting agent is at least one of ethanol, propylene glycol, glycerol, ethylene glycol, dimethyl sulfoxide, tween-80 and diethylene glycol.
10. The use of the highly dispersed ball-like nano cerium oxide polishing solution according to any one of claims 1 to 9 in polishing silicon-containing solids.
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