JP5509114B2 - Cmp研磨剤及び基板の研磨方法 - Google Patents
Cmp研磨剤及び基板の研磨方法 Download PDFInfo
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- JP5509114B2 JP5509114B2 JP2011031168A JP2011031168A JP5509114B2 JP 5509114 B2 JP5509114 B2 JP 5509114B2 JP 2011031168 A JP2011031168 A JP 2011031168A JP 2011031168 A JP2011031168 A JP 2011031168A JP 5509114 B2 JP5509114 B2 JP 5509114B2
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- JP
- Japan
- Prior art keywords
- polishing
- water
- azobis
- cerium oxide
- propane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005498 polishing Methods 0.000 title claims description 132
- 238000000034 method Methods 0.000 title claims description 42
- 239000000758 substrate Substances 0.000 title claims description 37
- 239000003795 chemical substances by application Substances 0.000 title claims description 19
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 61
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 61
- 239000002245 particle Substances 0.000 claims description 56
- 229920003169 water-soluble polymer Polymers 0.000 claims description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- -1 cationic azo compound Chemical class 0.000 claims description 27
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- 238000002955 isolation Methods 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 15
- 150000003839 salts Chemical class 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 12
- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 claims description 12
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- WYFGBFHRZGNGAU-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;hydrochloride Chemical compound Cl.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 WYFGBFHRZGNGAU-UHFFFAOYSA-N 0.000 claims description 3
- CZSHOUBXIGQRDI-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;sulfuric acid;hydrate Chemical compound O.OS(O)(=O)=O.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 CZSHOUBXIGQRDI-UHFFFAOYSA-N 0.000 claims description 3
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 1
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- JKRBKUNNPGKVLF-UHFFFAOYSA-N bis[2-(4,5-dihydro-1h-imidazol-2-yl)propan-2-yl]diazene;sulfo hydrogen sulfate;dihydrate Chemical compound O.O.OS(=O)(=O)OS(O)(=O)=O.N=1CCNC=1C(C)(C)N=NC(C)(C)C1=NCCN1 JKRBKUNNPGKVLF-UHFFFAOYSA-N 0.000 description 1
- PVEOYINWKBTPIZ-UHFFFAOYSA-N but-3-enoic acid Chemical compound OC(=O)CC=C PVEOYINWKBTPIZ-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 150000001734 carboxylic acid salts Chemical class 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- KHSBAWXKALEJFR-UHFFFAOYSA-H cerium(3+);tricarbonate;hydrate Chemical compound O.[Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O KHSBAWXKALEJFR-UHFFFAOYSA-H 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 235000019316 curdlan Nutrition 0.000 description 1
- 229940078035 curdlan Drugs 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- JZKFHQMONDVVNF-UHFFFAOYSA-N dodecyl sulfate;tris(2-hydroxyethyl)azanium Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCOS(O)(=O)=O JZKFHQMONDVVNF-UHFFFAOYSA-N 0.000 description 1
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229940100608 glycol distearate Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 125000004283 imidazolin-2-yl group Chemical group [H]N1C(*)=NC([H])([H])C1([H])[H] 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229940094506 lauryl betaine Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- HNEGQIOMVPPMNR-NSCUHMNNSA-N mesaconic acid Chemical compound OC(=O)C(/C)=C/C(O)=O HNEGQIOMVPPMNR-NSCUHMNNSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- HNEGQIOMVPPMNR-UHFFFAOYSA-N methylfumaric acid Natural products OC(=O)C(C)=CC(O)=O HNEGQIOMVPPMNR-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- JHRDEHLFNLLCQS-UHFFFAOYSA-N n'-hydroxy-2-methylpropanimidamide Chemical compound CC(C)C(N)=NO JHRDEHLFNLLCQS-UHFFFAOYSA-N 0.000 description 1
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 description 1
- GSGDTSDELPUTKU-UHFFFAOYSA-N nonoxybenzene Chemical compound CCCCCCCCCOC1=CC=CC=C1 GSGDTSDELPUTKU-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- UPHWVVKYDQHTCF-UHFFFAOYSA-N octadecylazanium;acetate Chemical compound CC(O)=O.CCCCCCCCCCCCCCCCCCN UPHWVVKYDQHTCF-UHFFFAOYSA-N 0.000 description 1
- 229920002114 octoxynol-9 Polymers 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- LCLHHZYHLXDRQG-ZNKJPWOQSA-N pectic acid Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)O[C@H](C(O)=O)[C@@H]1OC1[C@H](O)[C@@H](O)[C@@H](OC2[C@@H]([C@@H](O)[C@@H](O)[C@H](O2)C(O)=O)O)[C@@H](C(O)=O)O1 LCLHHZYHLXDRQG-ZNKJPWOQSA-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
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 108010064470 polyaspartate Proteins 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000010318 polygalacturonic acid Substances 0.000 description 1
- 229920002643 polyglutamic acid Polymers 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 description 1
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010988 polyoxyethylene sorbitan tristearate Nutrition 0.000 description 1
- 239000001816 polyoxyethylene sorbitan tristearate Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 150000004804 polysaccharides Chemical class 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical group Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XJAJNAQBHCNNBM-UHFFFAOYSA-N sulfo hydrogen sulfate dihydrate Chemical compound O.O.OS(=O)(=O)OS(O)(=O)=O XJAJNAQBHCNNBM-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- UIERETOOQGIECD-ONEGZZNKSA-N tiglic acid Chemical compound C\C=C(/C)C(O)=O UIERETOOQGIECD-ONEGZZNKSA-N 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- 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
- 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
- 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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Description
(水溶性高分子の合成)
脱イオン水960gを3リットルの合成用フラスコに投入し、窒素ガス雰囲気下で撹拌しながら90℃に昇温後、アクリル酸497gと2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕53gとをメタノール500gに溶解させたものを2時間かけてフラスコ中に注入した。その後90℃で3時間保温後、冷却して取り出し水溶性高分子溶液を得た。その不揮発分を測定したところ、25重量%であった。さらに、示差屈折計(株式会社日立製作所製型番L−3300)を備えたHPLCポンプ(株式会社日立製作所製 型番L−7100)にGPCカラム (日立化成工業株式会社製型番W550)を接続し、0.3M NaClを移動相として用い、上記で得られたポリアクリル酸の分子量測定を行ったところ、その重量平均分子量は5,000(ポリエチレングリコール換算値)であった。
炭酸セリウム水和物40kgをアルミナ製容器に入れ、830℃で2時間空気中で焼成することにより黄白色の粉末を約20kg得た。この粉末をX線回折法で相同定を行なったところ酸化セリウムであること確認した。焼成粉末粒子径は30〜100μmであった。酸化セリウム粒子粉末15kgをジェットミルを用いて乾式粉砕を行なった。乾式粉砕後の多結晶体の比表面積をBET法により測定した結果、9m2/gであった。
浅素子分離(STI)絶縁膜CMP評価用試験ウエハとして、SEMATECH製864ウエハ(φ200mm)を用いた(SiN膜厚150nm、SiO2膜厚凸部610nm、凹部610nm)。研磨装置(Applied Materials社製商品名 Mirra)の、保持する基板取り付け用の吸着パッドを貼り付けたホルダーに上記試験ウエハをセットし、一方、φ480mmの研磨定盤にロデール社製多孔質ウレタン樹脂製の研磨パッド型番IC−1000(K溝)を貼り付けた。該パッド上に絶縁膜面を下にして前記ホルダーを載せ、さらに加工荷重としてメンブレン、リテーナリング、インナチューブ圧力をそれぞれ3.0psi、3.5psi、3.0psi(20.6Pa、24.0Pa、20.6Pa)に設定した。定盤上に上記で調製したCMP研磨剤を200ミリリットル/分の速度で滴下しながら、定盤とウエハとをそれぞれ98rpm、78rpmで作動させてSTI絶縁膜CMP評価用試験ウエハを研磨した。研磨定盤トルク電流値をモニタすることで、研磨の終点検出を行った。研磨後のウエハを純水で良く洗浄後、乾燥した。その後、光干渉式膜厚装置(ナノメトリクス社製商品名、Nanospec AFT−5100)を用いて、凹部の絶縁膜の残膜厚、凸部の絶縁膜の残膜厚、あるいはSiN膜の残膜厚を測定した。さらにVeeco社製段差計Dektak 型番V200−Siを用いて、研磨後の凸部と凹部の残段差を測定した。表1に得られた各測定結果を示す。
(水溶性高分子の合成)
脱イオン水960gを3リットルの合成用フラスコに投入し、窒素ガス雰囲気下で撹拌しながら90℃に昇温後、アクリル酸497gと2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕二硫酸塩二水和物103gとを脱イオン水500gに溶解させたものを2時間かけてフラスコ中に注入した。その後90℃で3時間保温後、冷却して取り出し水溶性高分子溶液を得た。不揮発分を測定したところ、25重量%であった。実施例1と同様に、得られた水溶性高分子の分子量測定を行ったところ、その重量平均分子量は3,200(ポリエチレングリコール換算値)であった。
上記で得られたポリアクリル酸水溶液(25重量%)48gと脱イオン水2352gを混合し、アンモニア水(25重量%)にてpH5.3に調整した。さらに上記の酸化セリウムスラリ(固形分:5重量%)600gを添加し、酸化セリウム系CMP研磨剤(固形分:1.0重量%)を作製した。研磨剤pHは5.5、また、研磨剤中の粒子をレーザ回折式粒度分布計で測定するために、適当な濃度に希釈して測定した結果、粒径の平均値が170nmであった。
上記で作製した研磨剤を用いた以外は実施例1と同様に浅素子分離(STI)絶縁膜CMP評価用試験ウエハの研磨を行い、表1に示す結果を得た。
(水溶性高分子の合成)
脱イオン水960gを3リットルの合成用フラスコに投入し、窒素ガス雰囲気下で撹拌しながら90℃に昇温後、メタクリル酸256g、アクリル酸255g及び2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕46gを、メタノール500gに溶解させたものを2時間かけてフラスコ中に注入した。その後90℃で3時間保温後、冷却して取り出し水溶性高分子溶液を得た。その不揮発分を測定したところ、25重量%であった。実施例1と同様に、得られた水溶性高分子の分子量測定を行ったところ、その重量平均分子量は4,200(ポリエチレングリコール換算値)であった。
上記で得られたポリアクリル酸−メタクリル酸共重合体水溶液(25重量%)36gと脱イオン水2364gを混合し、アンモニア水(25重量%)にてpH4.9に調整した。さらに上記の酸化セリウムスラリ(固形分:5重量%)600gを添加し、酸化セリウム系CMP研磨剤(固形分:1.0重量%)を作製した。研磨剤pHは5.1、また、研磨剤中の粒子をレーザ回折式粒度分布計で測定するために、適当な濃度に希釈して測定した結果、粒径の平均値が170nmであった。
上記で作製した研磨剤を用いた以外は実施例1と同様に浅素子分離(STI)絶縁膜CMP評価用試験ウエハの研磨を行い、表1に示す結果を得た。
(水溶性高分子の合成)
脱イオン水960gを3リットルの合成用フラスコに投入し、窒素ガス雰囲気下で撹拌しながら90℃に昇温後、メタクリル酸256g、アクリル酸255g及び2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕二硫酸塩二水和物89gを、脱イオン水500gに溶解させたものを2時間かけてフラスコ中に注入した。その後90℃で3時間保温後、冷却して取り出し水溶性高分子溶液を得た。その不揮発分を測定したところ、25重量%であった。実施例1と同様に、得られた水溶性高分子の分子量測定を行ったところ、その重量平均分子量は7,500(ポリエチレングリコール換算値)であった。
上記で得られたポリアクリル酸−メタクリル酸共重合体水溶液(25重量%)30gと脱イオン水2370gを混合し、アンモニア水(25重量%)にてpH4.6に調整した。さらに上記の酸化セリウムスラリ(固形分:5重量%)600gを添加し、酸化セリウム系CMP研磨剤(固形分:1.0重量%)を作製した。研磨剤pHは4.8、また、研磨剤中の粒子をレーザ回折式粒度分布計で測定するために、適当な濃度に希釈して測定した結果、粒径の平均値が170nmであった。
上記で作製した研磨剤を用いた以外は実施例1と同様に浅素子分離(STI)絶縁膜CMP評価用試験ウエハの研磨を行い、表1に示す結果を得た。
(水溶性高分子の合成)
イソプロパノール480g、脱イオン水480gを3リットルの合成用フラスコに投入し、窒素ガス雰囲気下で撹拌しながら75℃に昇温後、アクリル酸560gと、2,2´−アゾビスイソブチロニトリル40gとをイソプロパノール500gに溶解させたものを2時間かけてフラスコ中に注入した。その後75℃で3時間保温後、冷却して取り出し水溶性高分子溶液を得た。その不揮発分を測定したところ、25重量%であった。実施例1と同様に、得られた水溶性高分子の分子量測定を行ったところ、その重量平均分子量は25,000(ポリエチレングリコール換算値)であった。
上記ポリアクリル酸水溶液(25重量%)30gと脱イオン水2370gを混合し、アンモニア水(25重量%)にてpH6.9に調整した。さらに上記の酸化セリウムスラリ(固形分:5重量%)600gを添加し、酸化セリウム研磨剤(固形分:1.0重量%)を作製した。研磨剤pHは7.0、また、研磨剤中の粒子をレーザ回折式粒度分布計で測定するために、適当な濃度に希釈して測定した結果、粒径の平均値が170nmであった。
Claims (12)
- 凹凸を有する無機絶縁膜の凸部を選択的に研磨する平坦化工程、又は、シャロートレンチ分離の形成工程において、余分の無機絶縁膜を除去するために用いられるCMP研磨剤であって、
酸化セリウム粒子、分散剤、水溶性高分子および水を含有し、前記水溶性高分子が、カチオン性アゾ化合物およびその塩の少なくとも一方を重合開始剤として、不飽和二重結合を有するカルボン酸およびその塩の少なくとも一方を含む単量体が重合してなる重合体であり、
前記カチオン性アゾ化合物およびその塩は、2,2´−アゾビス〔2−(5−メチル−2−イミダゾリン−2−イル)プロパン〕塩酸塩、2,2´−アゾビス〔2−(2−イミダゾリン−2−イル) プロパン〕、2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕塩酸塩、2,2 ´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕硫酸塩水和物、2,2´−アゾビス〔2−(3,4,5,6−テトラヒドロピリミジン−2−イル)プロパン塩酸塩、2,2´−アゾビス{2−〔1−(2−ヒドロキシエチル)−2−イミダゾリン−2−イル〕プロパン}塩酸塩、2,2´−アゾビス〔2−アミノジプロパン〕塩酸塩、及び2,2´−アゾビス(2−メチルプロピオンアミドオキシム)からなる群から選択される少なくとも一種であり、
酸化セリウム粒子、分散剤および水を含む酸化セリウムスラリと、水溶性高分子および水を含む添加液とを分けた二液式CMP研磨剤として保存されるCMP研磨剤。 - 前記水溶性高分子の配合量が、CMP研磨剤100重量部に対して0.01重量部以上5重量部以下である請求項1記載のCMP研磨剤。
- 前記水溶性高分子の重量平均分子量が200以上50,000以下である請求項1又は2記載のCMP研磨剤。
- 前記酸化セリウム粒子の平均粒径が1nm以上400nm以下である請求項1〜3のいずれか1項に記載のCMP研磨剤。
- 前記酸化セリウム粒子の配合量が、CMP研磨剤100重量部に対して0.1重量部以上5重量部以下である請求項1〜4のいずれか1項に記載のCMP研磨剤。
- pHが4.5以上6.0以下である請求項1〜5のいずれか1項に記載のCMP研磨剤。
- 前記無機絶縁膜が酸化珪素を含む、請求項1〜6のいずれか1項に記載のCMP研磨剤。
- 被研磨膜を形成した基板を研磨定盤の研磨布に押しあて加圧し、請求項1〜7のいずれか1項に記載のCMP研磨剤を被研磨膜と研磨布との間に供給しながら、基板と研磨定盤とを相対的に動かして、余分の被研磨膜を除去する基板の研磨方法。
- 酸化セリウム粒子、分散剤および水を含む酸化セリウムスラリと混合してCMP研磨剤を得るために使用される添加液であって、
該CMP研磨剤は、凹凸を有する無機絶縁膜の凸部を選択的に研磨する平坦化工程、又は、シャロートレンチ分離の形成工程において、余分の無機絶縁膜を除去するために用いられるものであり、
水溶性高分子および水を含有し、前記水溶性高分子が、カチオン性アゾ化合物およびその塩の少なくとも一方を重合開始剤として、不飽和二重結合を有するカルボン酸およびその塩の少なくとも一方を含む単量体が重合してなる重合体であり、
前記カチオン性アゾ化合物およびその塩は、2,2´−アゾビス〔2−(5−メチル−2−イミダゾリン−2−イル)プロパン〕塩酸塩、2,2´−アゾビス〔2−(2−イミダゾリン−2−イル) プロパン〕、2,2´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕塩酸塩、2,2 ´−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕硫酸塩水和物、2,2´−アゾビス〔2−(3,4,5,6−テトラヒドロピリミジン−2−イル)プロパン塩酸塩、2,2´−アゾビス{2−〔1−(2−ヒドロキシエチル)−2−イミダゾリン−2−イル〕プロパン}塩酸塩、2,2´−アゾビス〔2−アミノジプロパン〕塩酸塩、及び2,2´−アゾビス(2−メチルプロピオンアミドオキシム)からなる群から選択される少なくとも一種である、CMP研磨剤用添加液。 - 前記水溶性高分子の重量平均分子量が200以上50,000以下である請求項9記載のCMP研磨剤用添加液。
- 前記無機絶縁膜が酸化珪素を含む、請求項9又は10記載のCMP研磨剤用添加液。
- 被研磨膜を形成した基板を研磨定盤の研磨布に押しあて加圧し、請求項9〜11のいずれか1項に記載のCMP研磨剤用添加液と、酸化セリウム粒子、分散剤、および水を含む酸化セリウムスラリとを、被研磨膜と研磨布との間に供給しながら、基板と研磨定盤とを相対的に動かして、余分の被研磨膜を除去する基板の研磨方法。
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JP2011103498A (ja) | 2011-05-26 |
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