JP6421887B2 - セリウム塩の製造方法、酸化セリウム及びセリウム系研磨剤 - Google Patents
セリウム塩の製造方法、酸化セリウム及びセリウム系研磨剤 Download PDFInfo
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- JP6421887B2 JP6421887B2 JP2018018789A JP2018018789A JP6421887B2 JP 6421887 B2 JP6421887 B2 JP 6421887B2 JP 2018018789 A JP2018018789 A JP 2018018789A JP 2018018789 A JP2018018789 A JP 2018018789A JP 6421887 B2 JP6421887 B2 JP 6421887B2
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- cerium
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- cerium oxide
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- 150000000703 Cerium Chemical class 0.000 title claims description 63
- 229910000420 cerium oxide Inorganic materials 0.000 title claims description 57
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 229910052684 Cerium Inorganic materials 0.000 title description 60
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title description 53
- 238000000034 method Methods 0.000 claims description 33
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 30
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 26
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229960001759 cerium oxalate Drugs 0.000 claims description 2
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims description 2
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 239000002245 particle Substances 0.000 description 66
- 229910052761 rare earth metal Inorganic materials 0.000 description 36
- 238000005498 polishing Methods 0.000 description 30
- 150000002910 rare earth metals Chemical class 0.000 description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 20
- -1 bastonite ore Chemical compound 0.000 description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 14
- 239000012266 salt solution Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- 239000012141 concentrate Substances 0.000 description 11
- 239000000543 intermediate Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 238000000926 separation method Methods 0.000 description 9
- 239000002270 dispersing agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000011163 secondary particle Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 235000012431 wafers Nutrition 0.000 description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 5
- 239000001099 ammonium carbonate Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 235000006408 oxalic acid Nutrition 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000403354 Microplus Species 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000001785 cerium compounds Chemical class 0.000 description 2
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 2
- YNFYQHZKLWMOPA-UHFFFAOYSA-H cerium(3+);tricarbonate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O YNFYQHZKLWMOPA-UHFFFAOYSA-H 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052590 monazite Inorganic materials 0.000 description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000004576 sand Substances 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
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- WKBPZYKAUNRMKP-UHFFFAOYSA-N 1-[2-(2,4-dichlorophenyl)pentyl]1,2,4-triazole Chemical compound C=1C=C(Cl)C=C(Cl)C=1C(CCC)CN1C=NC=N1 WKBPZYKAUNRMKP-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000012237 artificial material Substances 0.000 description 1
- WPKYZIPODULRBM-UHFFFAOYSA-N azane;prop-2-enoic acid Chemical compound N.OC(=O)C=C WPKYZIPODULRBM-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 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 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229940065287 selenium compound Drugs 0.000 description 1
- 150000003343 selenium compounds Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000011031 topaz Substances 0.000 description 1
- 229910052853 topaz Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- 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
-
- 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
- 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
- C01F17/247—Carbonates
-
- 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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Description
(1)6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に溶液中に存在する不溶成分の濃度が質量比で5ppm以下であるセリウム塩。
(2)不溶成分が珪素を含む物質である上記(1)記載のセリウム塩。
(3)セリウム化合物から一種または複数種のセリウム含有中間体を得る工程を経て、沈殿剤を加えてセリウム塩の沈殿を得るセリウム塩の製造方法であって、溶液状態のセリウム含有中間体から不溶成分を分離・除去する工程を少なくとも一つ含むセリウム塩の製造方法。
(4)セリウム含有希土塩溶液に沈殿剤を加えてセリウム塩の沈殿を得る工程を含み、該工程では、予め不溶成分を除去した沈殿剤をセリウム含有希土塩溶液に加えて沈殿させる上記(3)記載のセリウム塩の製造方法。
(5)セリウム塩を、6規定硝酸と混合して溶液を得る工程と、該溶液の不溶成分を分離除去する工程と、該除去の後に沈殿剤を加えて精製されたセリウム塩を沈殿させる工程とを含む上記(3)または(4)記載のセリウム塩の製造方法。
(6)沈殿剤が、予め溶媒に溶解して不溶成分を分離除去した溶液状態である上記(3)〜(5)のいずれか記載のセリウム塩の製造方法。
(7)上記(1)または(2)記載のセリウム塩または上記(3)〜(6)のいずれか記載の製造方法で得られたセリウム塩を、250℃以上で高温処理してなる酸化セリウム。
(8)6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に溶液中に存在する不溶成分の濃度が質量比で10ppm以下である上記(7)記載の酸化セリウム。
(9)6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に溶液中に存在する不溶成分の濃度が質量比で10ppm以下である酸化セリウム。
(10)上記(7)〜(9)のいずれか記載の酸化セリウムを含むセリウム系研磨剤。
(11)6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に、溶液中に存在する不溶成分の濃度が質量比で10ppm以下であるセリウム系研磨剤。
市販の炭酸セリウム6水和物240gを、6規定の硝酸150gに溶解し、炭酸セリウム溶解液390gを得た。この溶解液390gを、回転数1,000rpmで120分間遠心分離を行った。分離機を停止した後すみやかに、上澄み液を350g採取した。
次に、得られた炭酸セリウム約6kgをアルミナ製容器に入れ、800℃、空気中で2時間焼成することにより黄白色の粉末を約3kg得た。この粉末をX線回折法で相同定を行ったところ酸化セリウムであることを確認した。焼成粉末粒子径は30〜100μmであった。さらに、得られた酸化セリウム粉末3kgを、ジェットミルを用いて乾式粉砕し、酸化セリウム粒子を得た。
上記作製した酸化セリウム粒子1000gとポリアクリル酸アンモニウム塩水溶液(40質量%)40gと脱イオン水8960gを混合し、撹拌しながら超音波分散を10分間施してセリウム系研磨剤を調製した。得られた研磨剤を孔径1μmのフィルタでろ過した。研磨剤中の粒子をレーザ回折式粒度分布計(マルバーンインストルメンツ社製、マスターサイザ マイクロ・プラス)を用い、屈折率:1.9285、光源:He−Neレーザ、吸収0の条件で、原液(濾過後の研磨剤)について測定した結果、二次粒子径の平均値は200nmであった。
研磨荷重:30kPa
研磨パッド:発泡ポリウレタン樹脂(ロデール社製、型番IC−1000)
回転数:上盤75rpm、研磨パッド75rpm
研磨剤供給速度:200mL/分
研磨対象物:P−TEOS成膜Siウェハ(200mm径)
実施例1と同条件で調製した炭酸セリウム溶解液390gを、孔径が10.0μm、5.0μm、1.0μm、0.1μmのフィルタで段階的に吸引ろ過し、ろ液を390g採取した。
得られた炭酸セリウム約6kgをアルミナ製容器に入れ、800℃、空気中で2時間焼成することにより黄白色の粉末を約3kg得た。この粉末をX線回折法で相同定を行ったところ酸化セリウムであることを確認した。焼成粉末粒子径は30〜100μmであった。さらに、得られた酸化セリウム粉末3kgを、ジェットミルを用いて乾式粉砕し、酸化セリウム粒子を得た。
上記作製した酸化セリウム粒子1000gから、実施例1と同条件で、セリウム系研磨剤を調製し、粒子を測定したところ、二次粒子径の平均値は200nmであった。
(炭酸セリウムの不溶成分)
市販の炭酸セリウム20gを、6規定の硝酸12.5gと濃度30%の過酸化水素12.5gの混合液に加え、常温常圧の条件で170時間放置して完全溶解させ、孔径0.05μmのフィルタで、吸引ろ過を行い、不溶成分を捕集した。このフィルタを走査型電子顕微鏡で観察して、実施例1と同条件で、不溶成分の総質量を導出した。溶解に用いた炭酸セリウムの質量に対し、不溶成分の質量が占める割合を算出したところ、7.8ppmだった。
上記市販の炭酸セリウム6kgをアルミナ製容器に入れ、800℃、空気中で2時間焼成することにより黄白色の粉末を約3kg得た。この粉末をX線回折法で相同定を行ったところ酸化セリウムであることを確認した。焼成粉末粒子径は30〜100μmであった。さらに、得られた酸化セリウム粉末3kgを、ジェットミルを用いて乾式粉砕し、酸化セリウム粒子を得た。
上記作製した酸化セリウム粒子1000gから、実施例1と同条件で、セリウム系研磨剤を調製し、研磨剤粒子を測定した。ただし、レーザ回折式粒度分布計としてマルバーンインストルメンツ社製、商品名マスターサイザー 3000HSを用いた。測定した結果、二次粒子径の平均値は200nmであった。
Claims (3)
- 6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に溶液中に存在する、孔径0.05μmのフィルタで捕集される不溶成分の濃度が質量比で10ppm以下である、酸化セリウム。
- 6規定の硝酸12.5gと30%の過酸化水素水12.5gとの混合液に20g溶解した場合に溶液中に存在する、孔径0.05μmのフィルタで捕集される不溶成分の濃度が質量比で5ppm以下であるセリウム塩を酸化することを含む、酸化セリウムの製造方法。
- 前記セリウム塩は、炭酸セリウム、水酸化セリウム、蓚酸セリウム、及びそれらの水和物からなる群から選ばれるいずれかである、請求項2記載の製造方法。
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