JP2015110513A - 結晶性酸化セリウム及びその製造方法 - Google Patents
結晶性酸化セリウム及びその製造方法 Download PDFInfo
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- JP2015110513A JP2015110513A JP2014242195A JP2014242195A JP2015110513A JP 2015110513 A JP2015110513 A JP 2015110513A JP 2014242195 A JP2014242195 A JP 2014242195A JP 2014242195 A JP2014242195 A JP 2014242195A JP 2015110513 A JP2015110513 A JP 2015110513A
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- cerium oxide
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 214
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 90
- 239000013078 crystal Substances 0.000 claims abstract description 69
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 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 abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 9
- -1 cerium carbonate compound Chemical class 0.000 claims description 70
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 238000010298 pulverizing process Methods 0.000 claims description 34
- WMOHXRDWCVHXGS-UHFFFAOYSA-N [La].[Ce] Chemical compound [La].[Ce] WMOHXRDWCVHXGS-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 18
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003021 water soluble solvent Substances 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 3
- 238000000034 method Methods 0.000 abstract description 47
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 abstract description 46
- 238000005498 polishing Methods 0.000 abstract description 35
- 230000008569 process Effects 0.000 abstract description 26
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000635 electron micrograph Methods 0.000 description 17
- 238000003756 stirring Methods 0.000 description 17
- 150000000703 Cerium Chemical class 0.000 description 14
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 description 13
- 239000012153 distilled water Substances 0.000 description 13
- 238000009826 distribution Methods 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 12
- 239000011324 bead Substances 0.000 description 12
- 239000004202 carbamide Substances 0.000 description 12
- 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
- 239000000843 powder Substances 0.000 description 11
- 239000002243 precursor Substances 0.000 description 11
- 230000035484 reaction time Effects 0.000 description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 229920006318 anionic polymer Polymers 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 238000000790 scattering method Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 102100035472 DNA polymerase iota Human genes 0.000 description 1
- 101001094672 Homo sapiens DNA polymerase iota Proteins 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CLSZAABBVGFUJA-UHFFFAOYSA-N O.C1(OOO1)=O.[Ce] Chemical compound O.C1(OOO1)=O.[Ce] CLSZAABBVGFUJA-UHFFFAOYSA-N 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- NAFHKBCKZMZCTP-UHFFFAOYSA-K [Ce+3].OOC([O-])=O.OOC([O-])=O.OOC([O-])=O Chemical compound [Ce+3].OOC([O-])=O.OOC([O-])=O.OOC([O-])=O NAFHKBCKZMZCTP-UHFFFAOYSA-K 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000000223 laser vaporisation method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
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- 239000005304 optical glass Substances 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
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- 238000007086 side reaction Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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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
- C01F17/20—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
- 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
-
- 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
-
- 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
- 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
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/39—Particle morphology extending in three dimensions parallelepiped-like
-
- C—CHEMISTRY; METALLURGY
- 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
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse 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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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Abstract
Description
前記ランタナイトセリウムの反応を約50〜130℃の温度下で進めて、斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)を含む炭酸セリウム系化合物を形成することができ、このような温度範囲内で反応温度または反応時間などの諸般条件を調節して、前記斜方晶系セリウムオキシカーボネートハイドレート(Ce2O(CO3)2・H2O)の生成程度を調節することができる。
[実施例1:炭酸セリウム系化合物及び結晶性酸化セリウムの製造]
常圧(1atm)、常温(RT)下で、ランタナイトセリウム23kgを蒸溜水140kgに分散して形成した水溶液を、180℃に昇温した反応器で2時間反応させた。この後、反応結果物をスプレードライヤーで乾燥して、炭酸セリウム系化合物を得た。
ランタナイトセリウム70kgを使用する点を除いては、実施例1と同様な方法で炭酸セリウム系化合物と酸化セリウムを得た。
ランタナイトセリウム70kgを蒸溜水140kgに分散して形成した水溶液を、80℃に昇温した反応器で3時間維持し、130℃に昇温した反応器で1時間維持する点を除いて、実施例1と同様な方法で炭酸セリウム系化合物と酸化セリウムを得た。
ランタナイトセリウム70kgを蒸溜水140kgに分散して形成した水溶液を80℃に昇温した反応器で24時間維持する点を除いて、実施例1と同様な方法で炭酸セリウム系化合物と酸化セリウムを得た。
セリウム硝酸塩69kgを常温で蒸溜水32kgに溶解した第1水溶液と、沈澱剤であるウレア35kgを常温で蒸溜水32kgに溶解した第2水溶液とを反応器に投入して、混合させた後、反応器を180℃に昇温して、2時間反応させた。
常圧(1atm)、常温(RT)下で、セリウム硝酸塩43.4kgとウレア18kgを混合し、これを140℃まで昇温した反応器で16時間反応させた。この後、結果物をゆっくり冷却させ、水で希釈して、反応を終結した後、80℃の真空状態下で24時間乾燥させ、炭酸セリウム系化合物を製造した。
ランタナイトセリウムを回転式連続加熱炉であるRotary kilinで900度で熱処理して、酸化セリウムを得た。
まず、XRDデータから、実施例で製造された酸化セリウムの結晶性を確認した。図7は、実施例1乃至4で製造された結晶性酸化セリウムのX線回折分析結果(XRDパターン)を示すものであって、これを通じて結晶性酸化セリウムの形成を確認した。
A.上記実施例1乃至4及び比較例1乃至3で製造された炭酸セリウム系化合物の電子顕微鏡写真(SEM写真)は、図1乃至6に示された通りである。
上記実施例1乃至4及び比較例1乃至3で製造されたCMP用スラリー(酸化セリウム、分散剤及び蒸溜水の混合物)に対してPOLI 500 Polisherで研磨評価を行い、結果を表2に示した。研磨後、研磨対象膜上のスクラッチ数は、KLA PENCO社のCS10装備で確認し、長さ300nm以上のdefectをスクラッチとし、スクラッチ数を算出した。
Claims (13)
- 70乃至120nmの体積平均粒径及び8乃至12.5nmの粒径の標準偏差を有することを特徴とするサブミクロン結晶性酸化セリウム。
- 前記平均粒径及び標準偏差は、垂直型ミル(mill)及び水平型ミル(mill)を用いて粉砕された後の値であることを特徴とする請求項1に記載の結晶性酸化セリウム。
- 前記粉砕前に、0.5乃至3μmの体積平均粒径を有し、
複数の酸化セリウム粒子を含み、
それぞれの酸化セリウム粒子上には、複数の結晶粒(crystal grain)を定義する境界(boundary)が形成されており、
それぞれの結晶粒は、一つ以上の酸化セリウム結晶を含むことを特徴とする請求項2に記載の結晶性酸化セリウム。 - 前記粉砕前に、前記結晶粒は、20乃至300nmの大きさを有し、前記酸化セリウム結晶は、10乃至200nmの結晶サイズを有することを特徴とする請求項3に記載の結晶性酸化セリウム。
- 請求項1乃至4のいずれか一項の結晶性酸化セリウムを研磨剤として含むことを特徴とする酸化セリウムスラリー。
- 分散剤、及び、pH調節剤をさらに含むことを特徴とする請求項5に記載の酸化セリウムスラリー。
- ランタナイト(Lanthanite)セリウムを50℃以上で反応させて、炭酸セリウム系化合物を形成するステップと、
前記炭酸セリウム系化合物を熱処理して、酸化セリウムを形成するステップと、
前記酸化セリウムを粉砕するステップと、
を含むことを特徴とする請求項1の結晶性酸化セリウムの製造方法。 - 前記ランタナイト(Lanthanite)セリウムの反応は、液状媒質内で行われることを特徴とする請求項7に記載の結晶性酸化セリウムの製造方法。
- 前記液状媒質は、水、及び、アルコール、DMSOまたはDMFを含む水溶性溶媒を含むことを特徴とする請求項8に記載の結晶性酸化セリウムの製造方法。
- 前記ランタナイトセリウムの反応は、ランタナイトセリウム:液状媒質の重量比が1:0.5乃至1:20になる量の液状媒質内で行われることを特徴とする請求項8に記載の結晶性酸化セリウムの製造方法。
- 前記ランタナイトセリウムの反応は、常圧乃至100barの圧力下で開始されることを特徴とする請求項7に記載の結晶性酸化セリウムの製造方法。
- 前記熱処理ステップは、300乃至1500℃で行われることを特徴とする請求項7に記載の結晶性酸化セリウムの製造方法。
- 前記粉砕は、垂直型ミル(mill)と水平型ミル(mill)を用いて行われることを特徴とする請求項7に記載の結晶性酸化セリウムの製造方法。
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006273994A (ja) * | 2005-03-29 | 2006-10-12 | Mitsui Mining & Smelting Co Ltd | セリウム系研摩材及びその中間体並びにこれらの製造方法 |
US20070104629A1 (en) * | 2003-01-31 | 2007-05-10 | Nanoproducts Corporation | Nanoparticles of rare earth oxides |
JP2008013689A (ja) * | 2006-07-06 | 2008-01-24 | Mitsui Mining & Smelting Co Ltd | セリウム系研摩材用原料およびセリウム系研摩材の製造方法並びにセリウム系研摩材 |
JP2010505735A (ja) * | 2006-10-09 | 2010-02-25 | ロデイア・オペラシヨン | 酸化セリウム粒子の液体懸濁物及び粉末、その製造方法並びに研磨におけるその使用 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11181403A (ja) | 1997-12-18 | 1999-07-06 | Hitachi Chem Co Ltd | 酸化セリウム研磨剤及び基板の研磨法 |
KR100477939B1 (ko) * | 2002-04-15 | 2005-03-18 | 주식회사 엘지화학 | 단결정 산화세륨 분말의 제조방법 |
AU2003275697A1 (en) | 2002-10-28 | 2004-05-13 | Nissan Chemical Industries, Ltd. | Cerium oxide particles and process for the production thereof |
JP4273921B2 (ja) | 2002-10-28 | 2009-06-03 | 日産化学工業株式会社 | 酸化セリウム粒子及び加湿焼成による製造方法 |
JP4273920B2 (ja) | 2002-10-28 | 2009-06-03 | 日産化学工業株式会社 | 酸化セリウム粒子及び多段階焼成による製造方法 |
CN100337926C (zh) * | 2002-10-28 | 2007-09-19 | 日产化学工业株式会社 | 氧化铈粒子及其制造方法 |
US8388710B2 (en) * | 2005-01-26 | 2013-03-05 | Lg Chem, Ltd. | Cerium oxide powder, method for preparing the same, and CMP slurry comprising the same |
DE102005038136A1 (de) * | 2005-08-12 | 2007-02-15 | Degussa Ag | Ceroxid-Pulver und Ceroxid-Dispersion |
WO2007088868A1 (ja) * | 2006-01-31 | 2007-08-09 | Hitachi Chemical Co., Ltd. | 絶縁膜研磨用cmp研磨剤、研磨方法、該研磨方法で研磨された半導体電子部品 |
US7976810B2 (en) * | 2007-03-16 | 2011-07-12 | Lg Chem, Ltd. | Method for preparing cerium carbonate powder |
JP5019323B2 (ja) * | 2007-03-20 | 2012-09-05 | 独立行政法人物質・材料研究機構 | 希土類元素をドープしたセリア焼結体とその製造方法 |
CN101652324B (zh) | 2007-05-03 | 2012-05-30 | 株式会社Lg化学 | 用作磨料的氧化铈粉末和含有该粉末的cmp浆料 |
EP2007102B1 (en) | 2007-06-21 | 2017-11-22 | Alcatel Lucent | Content-on-demand method and network therefor |
KR20100004181A (ko) | 2008-07-03 | 2010-01-13 | 삼성전자주식회사 | 화학 기계적 연마용 슬러리 조성물, 이의 제조 방법 및화학 기계적 연마방법 |
KR20110020559A (ko) | 2009-08-24 | 2011-03-03 | 노틸러스효성 주식회사 | 금융 자동화기기의 임베디드 메인보드 |
KR101050789B1 (ko) * | 2009-09-21 | 2011-07-20 | 주식회사 엘지화학 | 탄산세륨계 화합물의 제조 방법, 산화세륨의 제조 방법 및 결정성 산화세륨 |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070104629A1 (en) * | 2003-01-31 | 2007-05-10 | Nanoproducts Corporation | Nanoparticles of rare earth oxides |
JP2006273994A (ja) * | 2005-03-29 | 2006-10-12 | Mitsui Mining & Smelting Co Ltd | セリウム系研摩材及びその中間体並びにこれらの製造方法 |
JP2008013689A (ja) * | 2006-07-06 | 2008-01-24 | Mitsui Mining & Smelting Co Ltd | セリウム系研摩材用原料およびセリウム系研摩材の製造方法並びにセリウム系研摩材 |
JP2010505735A (ja) * | 2006-10-09 | 2010-02-25 | ロデイア・オペラシヨン | 酸化セリウム粒子の液体懸濁物及び粉末、その製造方法並びに研磨におけるその使用 |
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