JP5012026B2 - CeO2微粒子の製造方法 - Google Patents
CeO2微粒子の製造方法 Download PDFInfo
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- JP5012026B2 JP5012026B2 JP2006542417A JP2006542417A JP5012026B2 JP 5012026 B2 JP5012026 B2 JP 5012026B2 JP 2006542417 A JP2006542417 A JP 2006542417A JP 2006542417 A JP2006542417 A JP 2006542417A JP 5012026 B2 JP5012026 B2 JP 5012026B2
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- 239000010419 fine particle Substances 0.000 title claims description 60
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title 1
- 239000013078 crystal Substances 0.000 claims description 26
- 239000000155 melt Substances 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 8
- 239000011164 primary particle Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 238000005498 polishing Methods 0.000 description 56
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- 238000000034 method Methods 0.000 description 22
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- 238000002425 crystallisation Methods 0.000 description 17
- 230000008025 crystallization Effects 0.000 description 16
- 229910004298 SiO 2 Inorganic materials 0.000 description 14
- 239000010410 layer Substances 0.000 description 13
- 238000002844 melting Methods 0.000 description 12
- 230000008018 melting Effects 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000011521 glass Substances 0.000 description 9
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- 238000010298 pulverizing process Methods 0.000 description 7
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 239000003002 pH adjusting agent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 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 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
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- 229910021344 molybdenum silicide Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
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- 239000006179 pH buffering agent Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-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
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal borates Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 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 description 1
- QCCDYNYSHILRDG-UHFFFAOYSA-K cerium(3+);trifluoride Chemical compound [F-].[F-].[F-].[Ce+3] QCCDYNYSHILRDG-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
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- QBEGYEWDTSUVHH-UHFFFAOYSA-P diazanium;cerium(3+);pentanitrate Chemical compound [NH4+].[NH4+].[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBEGYEWDTSUVHH-UHFFFAOYSA-P 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
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- 239000002244 precipitate Substances 0.000 description 1
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
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- 238000010792 warming Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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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
- C09K3/1427—Abrasive particles per se obtained by division of a mass agglomerated by melting, at least partially, e.g. with a binder
-
- 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
- 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
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- 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
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- 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
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- 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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- 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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- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Description
また、トランジスタ等の素子間を電気的に分離するために、シャロートレンチによる素子分離法(Shallow Trench Isolation、以下STIという。)が用いられている。これは、素子領域をSiNx膜でマスクしてシリコン基板にトレンチ溝を形成した後、トレンチ溝を埋め込むようにSiO2膜を堆積させ、SiNx膜上の余分なSiO2膜をCMPによって除去し、素子領域を電気的に分離する方法である。CMPの際、SiNx膜の研磨速度とSiO2膜の研磨速度に選択比を持たせ、SiNx膜が露出した時点で研磨が終了するように、SiNx膜をストッパーとして使用するのが一般的である。
[例1〜17]
酸化セリウム(CeO2)、RCO3(R=Ba及び/又はSr)及び酸化ホウ素(B2O3)を、それぞれCeO2、RO及びB2O3基準のモル%表示で表1に示す割合となるように秤量し、少量のエタノールを添加して自動乳鉢で混合・粉砕した。その後、乾燥させて原料粉末を得た。
原料混合物の化学組成をそれぞれ表2に示す割合に変更し、かつ、表2に示す結晶化温度でフレークを8時間加熱した以外は例1と同様にして、CeO2微粒子を得た。得られたCeO2微粒子の鉱物相を例1と同じ方法で同定したところ、いずれもCeO2単相からなる結晶性の高い粒子であった。また、得られた微粒子の結晶子径を例1と同じ方法で測定したところ、表2に示すように、いずれも非常に細かい粒子径を有していた。さらに、結晶化温度の上昇に伴い、結晶子径が増加することが確認された。
例5と同様にして混合・粉砕操作、溶融操作を行って得られた溶融物を、電気炉内で300℃/hの速度で室温まで冷却したところ、不透明な固形物が生成し、非晶質物質は得られなかった。
酸化セリウム(CeO2)、炭酸バリウム(BaCO3)及び酸化ホウ素(B2O3)を、それぞれCeO2、BaO及びB2O3基準のモル%表示で表3に示す割合となるように秤量し、例5と同様にして混合・粉砕操作、溶融操作を行ったところ、不透明な固形物が生成し、非晶質物質は得られなかった。
酸化セリウム(CeO2)、炭酸バリウム(BaCO3)及び酸化ホウ素(B2O3)を、それぞれCeO2、BaO及びB2O3基準のモル%表示で表3に示す割合となるように秤量し、例1と同様にして混合・粉砕操作、溶融操作及び急速冷却操作を行ったところ、透明なフレークが得られた。しかし、例1と同様にして結晶化操作、溶脱操作を行った結果、結晶性のCeO2微粒子はほとんど得られなかった。
上記例19で得られたCeO2微粒子100gを約800mLの蒸留水に添加し、撹拌しつつ、0.1mol/Lの硝酸を徐々に加えてpH4.0に調整したものに対し、さらに全体積が1Lとなるまで蒸留水を添加して、10質量%のCeO2を含むスラリー原液Aを調製した。また、上記例24で得られたCeO2微粒子100gを約800mLの蒸留水に添加し、撹拌しつつ、0.1mol/Lの硝酸を徐々に加えてpH4.0に調整したものに対し、さらに全体積が1Lとなるまで蒸留水を添加して、10質量%のCeO2を含むスラリー原液Bを調製した。さらに、市販のCeO2微粒子(シーアイ化成社製、商品名:NanoTek、平均一次粒子径:14nm)を蒸留水に添加して10質量%のスラリー原液Cとした。
研磨は、以下の装置及び条件で行った。
研磨機:全自動CMP装置MIRRA(Applied Materials社製、商品名:Compass)、
研磨圧:20kPa、
回転数:プラテン(定盤)105rpm、
ヘッド(基盤保持部):98rpm、
研磨用スラリー供給速度:200mL/分、
研磨パッド:IC1000(ロデール社製)。
被研磨物としては、以下の(a)及び(b)を用いた(いずれもSematech社製)。
(a)SiO2(絶縁層)研磨速度評価用ウェハ:Si基板上に厚さ800nmのSiO2層をプラズマCVDで成膜した8インチウェハ。
(b)SiNx(ストッパー層)研磨速度評価用ウェハ:Si基板上に厚さ100nmのSiNxを熱CVDで成膜した8インチウェハ。
研磨速度は、研磨前後の膜厚から算出した。膜厚の測定には、光干渉式全自動膜厚測定装置UV1280SE(KLAテンコール社製)を用いた。絶縁層、ストッパー層のそれぞれの研磨速度の評価として、上記(a)及び(b)を使用し、この評価には、上記例30〜35の組成の研磨用スラリーを使用した。
なお、2004年11月8日に出願された日本特許出願2004−323854号の明細書、特許請求の範囲、図面及び要約書の全内容をここに引用し、本発明の明細書の開示として、取り入れるものである。
Claims (7)
- 酸化物基準のモル%表示で、CeO2を5〜50%、RO(RはMg、Ca、Sr及びBaからなる群より選ばれる1種以上)を10〜50%、B2O3を30〜75%含む溶融物を得る工程と、前記溶融物を急速冷却して非晶質物質とする工程と、前記非晶質物質からCeO2結晶を析出させる工程と、得られた結晶化物から前記CeO2結晶を分離する工程と、をこの順に含むことを特徴とするCeO2微粒子の製造方法。
- 前記溶融物中に、前記CeO2、前記RO及び前記B2O3をCeO2:(RO+B2O3)=5:95〜50:50のモル比で含む請求項1に記載のCeO2微粒子の製造方法。
- 前記溶融物中に、前記RO及び前記B2O3をRO:B2O3=20:80〜50:50のモル比で含む請求項1又は2に記載のCeO2微粒子の製造方法。
- 前記溶融物を急速冷却してフレーク状又はファイバー状の非晶質物質を得る請求項1〜3のいずれか1項に記載のCeO2微粒子の製造方法。
- 前記非晶質物質からCeO2結晶を析出させる工程を600〜900℃で行う請求項1〜4のいずれか1項に記載のCeO2微粒子の製造方法。
- 前記CeO2結晶を分離する工程を酸を用いて行う請求項1〜5のいずれか1項に記載のCeO2微粒子の製造方法。
- 前記CeO2微粒子の平均一次粒子径が5〜200nmである請求項1〜6のいずれか1項に記載のCeO 2 微粒子の製造方法。
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PCT/JP2005/020188 WO2006049197A1 (ja) | 2004-11-08 | 2005-11-02 | CeO2微粒子の製造方法及び該微粒子を含む研磨用スラリー |
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JP4945982B2 (ja) * | 2005-06-01 | 2012-06-06 | 旭硝子株式会社 | 希土類元素ドープCeO2微粒子の製造方法 |
SG170807A1 (en) * | 2006-04-27 | 2011-05-30 | Asahi Glass Co Ltd | Fine particles of oxide crystal and slurry for polishing which contains the fine particles |
SG136886A1 (en) | 2006-04-28 | 2007-11-29 | Asahi Glass Co Ltd | Method for producing glass substrate for magnetic disk, and magnetic disk |
JP4929855B2 (ja) * | 2006-06-07 | 2012-05-09 | 旭硝子株式会社 | セリア−ジルコニア固溶体微粒子の製造方法 |
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WO2008093801A1 (ja) * | 2007-02-02 | 2008-08-07 | Asahi Glass Company, Limited | 固溶体微粒子の製造方法 |
KR20100062998A (ko) * | 2007-09-07 | 2010-06-10 | 아사히 가라스 가부시키가이샤 | 산화물 결정 미립자의 제조 방법 |
EP2221276A4 (en) * | 2007-12-10 | 2011-03-09 | Asahi Glass Co Ltd | FINE CRYSTALLINE GRAINS SOLID SOLUTION OF CERI-ZIRCONE OXIDE AND METHOD FOR THE PRODUCTION THEREOF |
EP2471756A4 (en) * | 2009-08-28 | 2015-05-27 | Asahi Glass Co Ltd | METHOD FOR PRODUCING FLAKES AND METHOD FOR PRODUCING GLASS PRODUCT |
CN104010770B (zh) * | 2011-12-22 | 2017-07-21 | 柯尼卡美能达株式会社 | 研磨材料再生方法及再生研磨材料 |
MY176270A (en) * | 2011-12-27 | 2020-07-25 | Konica Minolta Inc | Method for separating polishing material and regenerated polishing material |
FR2999560B1 (fr) | 2012-12-18 | 2015-01-23 | Saint Gobain Ct Recherches | Poudre de cristallites |
JP2016056215A (ja) * | 2013-02-05 | 2016-04-21 | コニカミノルタ株式会社 | 研磨材の製造方法 |
JP6237650B2 (ja) * | 2013-02-05 | 2017-11-29 | コニカミノルタ株式会社 | コア・シェル型無機粒子 |
JP2016055352A (ja) * | 2013-02-05 | 2016-04-21 | コニカミノルタ株式会社 | 研磨材スラリー |
JP2016055351A (ja) * | 2013-02-05 | 2016-04-21 | コニカミノルタ株式会社 | 研磨材スラリー |
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