CN1296454C - 一种用于化学－机械抛光浆中颗粒的制备方法以及该方法制备的颗粒 - Google Patents
一种用于化学－机械抛光浆中颗粒的制备方法以及该方法制备的颗粒 Download PDFInfo
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- CN1296454C CN1296454C CNB02822664XA CN02822664A CN1296454C CN 1296454 C CN1296454 C CN 1296454C CN B02822664X A CNB02822664X A CN B02822664XA CN 02822664 A CN02822664 A CN 02822664A CN 1296454 C CN1296454 C CN 1296454C
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- 239000002245 particle Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000002002 slurry Substances 0.000 title claims abstract description 37
- 238000005498 polishing Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000243 solution Substances 0.000 claims abstract description 23
- 150000000703 Cerium Chemical class 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 13
- 238000009156 water cure Methods 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 claims description 4
- 150000003609 titanium compounds Chemical class 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical group [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
- 229910052706 scandium Inorganic materials 0.000 claims description 2
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- 230000001934 delay Effects 0.000 claims 2
- 239000003082 abrasive agent Substances 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 18
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 18
- 239000006061 abrasive grain Substances 0.000 description 12
- 238000001354 calcination Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XQMTUIZTZJXUFM-UHFFFAOYSA-N tetraethoxy silicate Chemical compound CCOO[Si](OOCC)(OOCC)OOCC XQMTUIZTZJXUFM-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910000667 (NH4)2Ce(NO3)6 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- -1 cerium ion Chemical class 0.000 description 1
- ZEDZJUDTPVFRNB-UHFFFAOYSA-K cerium(3+);triiodide Chemical compound I[Ce](I)I ZEDZJUDTPVFRNB-UHFFFAOYSA-K 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 1
- MOOUSOJAOQPDEH-UHFFFAOYSA-K cerium(iii) bromide Chemical compound [Br-].[Br-].[Br-].[Ce+3] MOOUSOJAOQPDEH-UHFFFAOYSA-K 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003325 scandium Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001890 transfection Methods 0.000 description 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/60—Compounds characterised by their crystallite size
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
本发明提供一种在化学-机械抛光浆中作为研磨剂颗粒的生产方法。本发明方法包括将晶体助长剂例如Ti[OCH(CH3)2]]4添加到铈盐水溶液中，用一种或更多碱将溶液的pH值调到大于7.0，然后溶液进行热水处理温度从90℃到大约500℃从而生成颗粒。
Description
技术领域
本发明涉及一种在化学-机械抛光浆中作为研磨剂的颗粒生产方法，以及用此方法生产的颗粒。
背景技术
化学-机械抛光(CMP)浆在例如生产半导体芯片及其类似物制备过程中可用来磨平其表面。CMP浆典型地包括化学腐蚀剂和分散在液态载体中的研磨颗粒。当研磨颗粒用抛光板压在被抛光表面时，其起到研磨的作用。
众所周知，CMP浆中使用的研磨颗粒的大小、组成和形态在抛光速率上起着很重要的作用。多年来，CMP浆由以下这些物质组成的研磨颗粒构成：例如，氧化铝(Al2O3)，氧化铈(CeO2)，氧化铁(Fe2O3)，硅石(SiO2)，金刚砂(SiC)，氮化硅(Si3N4)，氧化锡(SnO2)，氧化钛(TiO2)，碳化钡(TiC)，三氧化钨(WO3)，氧化钇(Y2O3)，氧化锆(ZrO2)及其氧化物。在这些氧化物当中，由于二氧化铈(CeO2)的高抛光性能，它是CMP浆磨平半导体氧化硅绝缘层最有效的研磨剂。
到目前为止，煅烧是生产CMP浆研磨颗粒最常用的办法。在煅烧过程中，前体如碳酸盐、草酸盐、硝酸盐和磷酸盐转化为相应的氧化物。煅烧结束后，生成的氧化物被研磨到足够小防止刮擦的颗粒尺寸和分布。
尽管广泛使用煅烧工艺，但存在一定的缺陷。比如，耗能大，因而相当昂贵。而且在煅烧中会生成有毒的和/或带腐蚀性的气态副产物。另外，很难避免在煅烧和其后研磨过程中污染物的进入。最后，很难获得适合尺寸研磨颗粒的狭窄分布。
众所周知，含有污染物和/或过大研磨颗粒的CMP浆会导致在抛光过程中形成不必要的表面划痕。这对粗糙的抛光工艺不是一个关键因素，但对生产精细的光学表面、半导体晶片、集成电路以及无缺陷物体表面来说是必要的。这只有在研磨颗粒直径小于1.0μm并且CMP浆不含污染物的情况下才能获得。利用传统的煅烧方法和研磨技术来获得符合这些要求的研磨颗粒是极其困难和不划算的。
另一个用于CMP浆研磨颗粒的生产方法是热水合成，其也被称作热水处理。在该方法中，将金属盐的碱性水溶液在不同时段内保持在高温和高压下，以产生悬浮在溶液当中固体氧化物的小颗粒。用热水处理法生成二氧化铈(CeO2)颗粒的方法已经被公开，如，王，美国专利No.5,389,352。
经热水处理法生产的研磨颗粒比煅烧/研磨方法更具优势。但是，传统的热水处理法不易达到所需的高抛光速率。
发明内容
本发明提供一种在化学-机械抛光浆中作为研磨剂颗粒的生产方法。本方法包括将晶体助长剂如异丙醇钛(IV)加入到铈盐水溶液，用一个或更多碱将pH值调到大于7.0，然后溶液从大约90℃加热到大约500℃温度进行热水处理液从而生成颗粒。虽然还不了解确切的原理，但是，在热水处理过程中溶液中的晶体助长剂的存在导致形成的颗粒具有大于预期晶体的尺寸。用这种方法形成的颗粒相对于用传统的热水处理法形成的颗粒，可以高得多的速率抛光表面。
本发明前述以及其它技术特征将在下文中更加详细描述并尤其在权利要求中指出，下面描述中还详细阐明本发明具体实施方式的示例，这些是示例，但也只是阐述了应用本发明原理的几种不同方式。
具体实施方式
本发明提供一种不需煅烧和/或研磨在化学-机械抛光浆中作为研磨剂颗粒的生产方法。本方法包括将一种晶体助长剂加入到一种铈盐水溶液中，用一种或更多碱将pH值调节到大于7.0，然后溶液从大约90℃加热到大约500℃温度进行热水处理液从而生成颗粒。
用于本发明方法的优选铈盐是(NH4)2Ce(NO3)6(硝酸铈(IV)铵)。但是，也可选用其它的水溶铈盐。虽然铈盐溶液中的铈的化合价本质上不是关键的，但四价铈盐(IV)比三价铈盐(III)好。本发明中适合的铈盐包括例如，硝酸铈、氯化铈、硫酸铈、溴化铈和碘化铈。
本溶液还必须包括一个或更多晶体助长剂。目前最优选的晶体助长剂是一种钛化合物，称为Ti[OCH(CH3)2]4(异丙醇钛(IV))。也可使用其它的钛化合物，比如，氯化钛、硫酸钛、溴化钛和氯氧化钛。要获得具有较大微晶尺寸的颗粒，使用晶体助长剂是必要的。
使用除了钛之外其它金属的化合物作为本发明的晶体助长剂也是可行的，比如，镧、钪、和/或铝的盐。尤其是钪盐，可依照本方法生产具有较大晶体尺寸的氧化铈颗粒。但是，鉴于目前未知的原因，使用钪化合物作为晶体助长剂而生成的颗粒不如使用钛化合物作为晶体助长剂而生成的颗粒在CMP抛光应用中作为研磨剂更有效。
必须加入一个或更多碱提高溶液的pH值大于7.0，并有助于具有胶状均一性溶液的形成。适用的碱包括例如，氢氧化铵、有机胺如乙胺和乙醇胺，和/或聚有机胺如聚乙烯亚胺。也可以加入其它化合物如尿素助于晶体的增长。胶状溶液在快速搅拌下会分解成小颗粒。
胶状液然后进行热水处理。该过程这样完成，将溶液移入一个不锈钢容器里，密封容器，然后放在一个烘箱里加热，温度从大约90℃到大约500℃，持续大约10分种到数小时。反应完成后，不锈钢容器在冷水中淬火，或在一定时间内逐渐冷却。在进行热水处理时，可以搅拌溶液，但不是必须。该反应也可以在连续搅拌下放在高压锅内进行。
测试显示，通过改变初始铈盐浓度可控制颗粒的平均大小(直径)：初始铈离子浓度越高，生成的颗粒越大。使用添加剂如尿素易于生成较小的颗粒。反应时间、温度和pH值对颗粒大小具有很小或没有影响。通过该方法可获得从大约5nm到大约1000nm的颗粒，但是最优选平均直径在大约50nm到大约250nm范围的颗粒。
虽然目前还不清楚其中的原理，由于某种原因，为了生产具有大晶体尺寸的研磨颗粒，其可用众所周知的X-射线衍射法来确定，晶体助长剂如Ti[OCH(CH3)2]4(异丙醇钛(IV))的存在是很关键的。例如，在相同的热水条件下(如温度，时间，pH值等)，含有(异丙醇钛(IV))晶体助长剂的溶液可产生具有210平均晶体尺寸的颗粒，然而不含(异丙醇钛(IV))晶体助长剂的溶液可产生只有42平均晶体尺寸的颗粒。基于某些原因，在热水处理过程中，溶液中晶体助长剂的存在加快了微晶的晶体生长。这是必需的，因为由较大晶体尺寸颗粒形成的CMP浆抛光表面例如四乙氧基原硅酸盐(TEOS)二氧化硅膜时，比由较小晶体颗粒形成的CMP浆具有高得多的抛光速率。因此，优选具有大于大约60的平均微晶尺寸的颗粒，更优选的是具有大于大约200的平均微晶尺寸的颗粒。
要注意的是，用于本发明晶体助长剂的化合物易于在水介质中迅速地分解，降低它们促进具有较大晶体尺寸颗粒形成的效率。相应地，最好在晶体助长剂中加入一种或更多稳定化合物，如乙酰丙酮，以阻止或延缓这种化合物水解。以这种方式稳定时，晶体助长剂就有充分的时间在通过加入一种或更多碱形成胶状溶液之前，在分子水平与铈盐均匀地混合。申请人发现，晶体助长剂以这种方式达到稳定时，在热水处理过程中形成的颗粒容易具有较大晶体尺寸。
本发明方法形成的颗粒尤其适于在CMP浆中使用。通过本方法或通过加水、酸和/或碱调整研磨剂浓度和pH值到所需的水平而产生颗粒从而得到CMP浆。物体表面，包括但不限于TEOS二氧化硅、玻璃丝、有机硅、氮化硅、氧氮化硅、硅，金刚砂、计算机存储器硬盘基质、含硅的低电容绝缘体以及含硅陶瓷，都可以使用含有用本发明颗粒的CMP浆进行抛光。
以下实施例只是用来阐明本发明而不是用来对权利要求的限定。
实施例1
在1000ml的塑料瓶中，将41.6克的(NH4)2Ce(NO3)6(硝酸铈(IV)铵)溶于500ml去离子蒸馏水(Dl-水)和1.2克CH3COCH2OCCH3(乙酰丙酮)中形成溶液。在36克的C2H5NH2(乙胺)搅拌加入后，再向溶液中加入2.4克的Ti[OCH(CH3)2]4(异丙醇钛(IV))。然后加入足量的Dl-水使最终溶积达到800ml。将此溶液搅拌5分钟并移入一个1000ml干净的不锈钢容器中。密封不锈钢容器并摇晃5分种，然后放入一个烘箱，在300℃下加热6小时。之后从烘箱内取出不锈钢容器在室温下冷却。将容器内的反应产物移到一个1000ml干净的塑料瓶中。如图1所示，反应产物为具有狭窄分布(D50＝87nm；D90＝101nm；D10＝68nm)的CeO2(氧化铈)分散系。氧化铈颗粒具有平均微晶尺寸为210。
实施例2
(对比实施例)
除了没有使用Ti[OCH(CH3)2]4(异丙醇钛(IV))外，使用实施例1中相同材料和方法形成一个氧化铈颗粒分散系。这样形成的氧化铈颗粒有一个狭窄的分布(D50＝89nm；D90＝99nm；D10＝72nm)，与实施例1中形成的氧化铈颗粒相似，但平均微晶尺寸仅为42。
实施例3
除了没有使用CH3COCH2OCCH3(乙酰丙酮)外，使用实施例1中相同的材料和方法形成一个氧化铈颗粒分散系。这样形成的氧化铈颗粒有一个狭窄的分布(D50＝80nm；D90＝97nm；D10＝60nm)，与实施例1中形成的氧化铈颗粒相似，但平均微晶尺寸仅为90。
实施例4
用氧化铈颗粒形成四种化学-机械抛光浆。浆A由100重量份实施例1中形成的氧化铈纳米颗粒分散系构成。浆B与浆A相同，除了使用在实施例2中形成的氧化铈纳米颗粒分散系而不是在实施例1中形成的氧化铈纳米颗粒分散系。浆C与浆A相同，除了使用在实施例3中形成的氧化铈纳米颗粒分散系而不是在实施例1中形成的氧化铈纳米颗粒分散系。浆D与浆A相同，除了氧化铈纳米颗粒分散系包括传统煅烧的氧化铈(Ferro电子材料SRS-616A)，其平均颗粒大小为D50＝141nm，分散于pH值为10.0的水中。相同的TEOS SiO2(二氧化硅)晶片分别用浆A、浆B、浆C和浆D抛光。使用Strasbaugh 6EC抛光剂，一个在3.2磅每平方英寸(psi)下行压力带有Suba IV背板的Rodel IC1000板，一个旋转速度达到60rpm的转盘以及浆的流速为150ml/min，进行抛光。用浆A抛光的晶片去除SiO2的速度为3500/min，并生成一个均方根平均粗糙度0.8的表面。用浆B抛光的晶片去除SiO2的速度为85/min，并生成一个均方根平均粗糙度1.0的表面。用浆C抛光的晶片去除SiO2的速度为1875/min，并生成一个均方根平均粗糙度2.0的表面。用浆D抛光的晶片去除SiO2的速度为4200/min，并生成一个均方根平均粗糙度3.0的表面。
对那些本领域的技术人员来说，很容易想到其它的优点及变化。因而，本发明从更广泛的角度来说，不受在此显示和描述的具体说明和实施例的限制。相应地，可以不离开附加的权利要求以及等同物所限定的总的发明概念范围或精神，进行各种变化。
Claims (9)
1.一种在化学-机械抛光浆中用作研磨剂颗粒的生产方法，包括在铈盐水溶液中加入晶体助长剂，加入一种或更多碱将溶液pH值调到大于7.0，以及溶液进行热水处理在从90℃加热到500℃温度来生产所述颗粒，其中晶体助长剂是选自异丙醇钛(IV)，氯化钛、硫酸钛、溴化钛、氯氧化钛，以及选自镧、钪、铝的金属盐，以及上述组合。
2.如权利要求1所述的方法，其中所述颗粒具有平均颗粒尺寸在5nm到1000nm范围之内。
3.如权利要求1所述的方法，其中所述颗粒具有大于60的平均微晶尺寸。
4.如权利要求1所述的方法，其中所述颗粒具有大于200的平均微晶尺寸。
5.如权利要求1所述的方法，其中所述铈盐是硝酸铈(IV)铵。
6.如权利要求1所述的方法，其中所述钛化合物为异丙醇钛(IV)。
7.如权利要求1所述的方法，其中所述碱选自氢氧化铵、乙胺、乙醇胺以及聚乙烯亚胺。
8.如权利要求1所述的方法，其中所述溶液进一步包括延缓晶体助长剂水解的化合物。
9.如权利要求8所述的方法，其中所述延缓晶体助长剂水解的化合物包括乙酰丙酮。
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| FR2545830B1 (fr) * | 1983-05-13 | 1986-01-03 | Rhone Poulenc Spec Chim | Nouvelle composition de polissage a base de cerium et son procede de fabrication |
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-
2001
- 2001-11-16 US US09/992,485 patent/US6596042B1/en not_active Expired - Lifetime
-
2002
- 2002-09-25 US US10/255,136 patent/US6818030B2/en not_active Expired - Lifetime
- 2002-11-04 JP JP2003545749A patent/JP4202257B2/ja not_active Expired - Fee Related
- 2002-11-04 WO PCT/US2002/035373 patent/WO2003044122A1/en active IP Right Grant
- 2002-11-04 CA CA2467030A patent/CA2467030C/en not_active Expired - Fee Related
- 2002-11-04 KR KR1020047007234A patent/KR20050043789A/ko not_active Application Discontinuation
- 2002-11-04 EP EP02792227A patent/EP1444309A4/en not_active Withdrawn
- 2002-11-04 CN CNB02822664XA patent/CN1296454C/zh not_active Expired - Fee Related
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| US4529410A (en) * | 1979-12-27 | 1985-07-16 | Rhone-Poulenc Industries | Rare earth polishing compositions |
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| US5026421A (en) * | 1987-12-09 | 1991-06-25 | Rhone-Poulenc Chimie | Polishing compositions based on cerium and process for the preparation thereof |
| US5389352A (en) * | 1993-07-21 | 1995-02-14 | Rodel, Inc. | Oxide particles and method for producing them |
Also Published As
| Publication number | Publication date |
|---|---|
| US20030093957A1 (en) | 2003-05-22 |
| US6818030B2 (en) | 2004-11-16 |
| AU2002357690A1 (en) | 2003-06-10 |
| WO2003044122A1 (en) | 2003-05-30 |
| EP1444309A1 (en) | 2004-08-11 |
| EP1444309A4 (en) | 2007-07-18 |
| CA2467030C (en) | 2010-10-12 |
| US6596042B1 (en) | 2003-07-22 |
| JP4202257B2 (ja) | 2008-12-24 |
| JP2005509725A (ja) | 2005-04-14 |
| KR20050043789A (ko) | 2005-05-11 |
| CN1585811A (zh) | 2005-02-23 |
| CA2467030A1 (en) | 2003-05-30 |
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