JP7044704B2 - 研磨用組成物、研磨用組成物の製造方法および研磨方法 - Google Patents
研磨用組成物、研磨用組成物の製造方法および研磨方法 Download PDFInfo
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- JP7044704B2 JP7044704B2 JP2018527457A JP2018527457A JP7044704B2 JP 7044704 B2 JP7044704 B2 JP 7044704B2 JP 2018527457 A JP2018527457 A JP 2018527457A JP 2018527457 A JP2018527457 A JP 2018527457A JP 7044704 B2 JP7044704 B2 JP 7044704B2
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- 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 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- DHNRXBZYEKSXIM-UHFFFAOYSA-N chloromethylisothiazolinone Chemical compound CN1SC(Cl)=CC1=O DHNRXBZYEKSXIM-UHFFFAOYSA-N 0.000 description 1
- 125000000259 cinnolinyl group Chemical class N1=NC(=CC2=CC=CC=C12)* 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 238000007865 diluting Methods 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
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- 238000002296 dynamic light scattering Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- QFWPJPIVLCBXFJ-UHFFFAOYSA-N glymidine Chemical compound N1=CC(OCCOC)=CN=C1NS(=O)(=O)C1=CC=CC=C1 QFWPJPIVLCBXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 125000003453 indazolyl group Chemical class N1N=C(C2=C1C=CC=C2)* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- SRPSOCQMBCNWFR-UHFFFAOYSA-N iodous acid Chemical compound OI=O SRPSOCQMBCNWFR-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229940045996 isethionic acid Drugs 0.000 description 1
- 125000000904 isoindolyl group Chemical class C=1(NC=C2C=CC=CC12)* 0.000 description 1
- 125000002183 isoquinolinyl group Chemical class C1(=NC=CC2=CC=CC=C12)* 0.000 description 1
- 150000003854 isothiazoles Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000011068 loading method Methods 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
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 125000005385 peroxodisulfate group Chemical group 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- LFSXCDWNBUNEEM-UHFFFAOYSA-N phthalazine Chemical class C1=NN=CC2=CC=CC=C21 LFSXCDWNBUNEEM-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
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- 229940068041 phytic acid Drugs 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 125000001042 pteridinyl group Chemical class N1=C(N=CC2=NC=CN=C12)* 0.000 description 1
- 125000000561 purinyl group Chemical class N1=C(N=C2N=CNC2=C1)* 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 125000002294 quinazolinyl group Chemical class N1=C(N=CC2=CC=CC=C12)* 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 125000002943 quinolinyl group Chemical class N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 125000001567 quinoxalinyl group Chemical class N1=C(C=NC2=CC=CC=C12)* 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 150000003557 thiazoles Chemical class 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
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Images
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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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
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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
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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
- C09K3/1454—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
- H01L21/302—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
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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
- H01L21/302—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
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- H—ELECTRICITY
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- 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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- 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
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- Condensed Matter Physics & Semiconductors (AREA)
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- Mechanical Treatment Of Semiconductor (AREA)
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Description
本発明の一側面に係る研磨用組成物は、熱重量測定により得られる重量変化率分布曲線の25℃以上250℃以下の範囲における最大ピーク温度が30℃以上53℃以下であるシリカを含み、25℃でのpHが6.0未満である。
研磨用組成物に添加し得る酸化剤は、研磨対象物の表面を酸化する作用を有し、研磨用組成物による研磨対象物の研磨速度を向上させる。
研磨用組成物中に金属防食剤を加えることにより、研磨用組成物を用いた研磨で配線の脇に凹みが生じるのをより抑えることができる。また、研磨用組成物を用いて研磨した後の研磨対象物の表面にディッシングが生じるのをより抑えることができる。
本発明で用いられる防腐剤および防カビ剤としては、例えば、2-メチル-4-イソチアゾリン-3-オンや5-クロロ-2-メチル-4-イソチアゾリン-3-オン等のイソチアゾリン系防腐剤、パラオキシ安息香酸エステル類、およびフェノキシエタノール等が挙げられる。これら防腐剤および防カビ剤は、単独でもまたは2種以上混合して用いてもよい。
本発明の研磨用組成物の製造方法は、特に制限されず、例えば、砥粒、および必要に応じて他の成分を、例えば分散媒中で、攪拌混合することにより得ることができる。すなわち、本発明の一側面では、研磨対象物を研磨するために用いられる研磨用組成物の製造方法であって、熱重量測定により得られる重量変化率分布曲線の25℃以上250℃以下の範囲における最大ピーク温度が30℃以上53℃以下であるシリカを準備すること、当該シリカと水とを混合すること、および混合物の25℃でのpHを6.0未満に調整することを含む、製造方法が提供される。
本発明において、研磨対象物は特に制限されず、金属、酸素原子及びケイ素原子を有する研磨対象物、ケイ素-ケイ素結合を有する研磨対象物、窒素原子及びケイ素原子を有する研磨対象物などが挙げられる。
上述のように、本発明の一側面に係る研磨用組成物や、上記製造方法により製造される研磨用組成物は、酸素原子と、ケイ素原子と、を含む研磨対象物の研磨に特に好適に用いられる。よって、本発明の一側面によれば、酸素原子およびケイ素原子を含む研磨対象物を、上記の研磨用組成物を用いて、または上記の製造方法により研磨用組成物を得、当該研磨用組成物を用いて研磨対象物を研磨することを有する、研磨方法が提供される。また、本発明の好ましい形態によると、オルトケイ酸テトラエチル(TEOS)を含む研磨対象物を、本発明の研磨用組成物を用いて、または上記の製造方法により研磨用組成物を得、当該研磨用組成物を用いて研磨することを有する、研磨方法が提供される。
シリカ(砥粒)の平均一次粒子径(nm)は、約0.2gのシリカサンプルについて、BET法で3~5回連続で測定した値から算出したシリカ粒子の比表面積(SA)の平均値を基に、シリカ粒子の形状が真球であると仮定して算出する。なお、これらの値から、会合度(平均二次粒子径/平均一次粒子径)の値についても算出できる。
シリカ(砥粒)の真密度(g/cm3)は、下記方法によって測定される。詳細には、まず、るつぼにシリカ水溶液を固形分(シリカ)で約15gとなるように入れ、市販のホットプレートを使用して、約200℃で水分を蒸発させる。さらに、シリカの空隙に残留した水分も除去するために、電気炉(アドバンテック株式会社製、焼成炉)にて300℃で1時間の熱処理を行い、処理後の乾燥シリカを乳鉢で擂り潰す。次に、あらかじめ精密天秤(株式会社エー・アンド・デイ製、GH-202)にて重量を測定した100ml比重瓶(Wa(g))に、上記にて作製した乾燥シリカを10g入れて重量を測定した(Wb(g))後、エタノールを20ml加えて、減圧したデシケータ内で30分間脱気する。その後、比重瓶内をエタノールで満たし、栓をして重量を測定する(Wc(g))。シリカの重量測定を終えた比重瓶は内容物を廃棄し、洗浄後にエタノールで満たし重量を測定する(Wd(g))。これらの重量と測定時のエタノールの温度(t(℃))から、式1および式2で真密度を算出する。
シリカ(砥粒)の比表面積(m2/g)は、BET法を用いて測定する。詳細には、試料(シリカ)を105℃で12時間以上加温して水分を除去する。乾燥したシリカを乳鉢で擂り潰し、あらかじめ重量を測定したセル(Wa’(g))にシリカを約0.2g入れて重量を測定した(Wb’(g))後、5分以上、比表面積計(株式会社島津製作所製、flowsorb II 2300)の加温部で180℃に保温する。その後、測定部に装着し、脱気時の吸着面積(A[m2])を計測する。当該A値を用いて、下記式3により、比表面積SA[m2/g]を求める。
TGは、測定サンプルの温度をある一定のプログラムに従って変化させたときのサンプルの重量変化を検出する解析手法であり、温度の関数としてプロットされたデータを得る。まず、測定試料であるシリカを105℃で24時間乾燥させ、遊離水分を除去する。乾燥させた試料をめのう乳鉢で磨り潰した後、アルミナパンに約30mg量り入れ、TG測定機(Thermo plus Evo(リガク社製))を用いて測定を行う。標準試料としてはα-アルミナを用いる。測定の際は、先ず、2℃/分で測定部の温度を150℃まで上昇させ、余剰水分を蒸発させる。これにより、乾燥後の静置時間の違いによる吸湿量の差の影響を排除する。その後、相対湿度70%RH、25℃の雰囲気中で40分間静置させることで試料に水分を吸湿させる。測定部が25℃に低下したら直ちに、1℃/分で測定部の温度を250℃まで上昇させ、経時的な熱重量変化を0.5分ごとに観測する。測定で求めた重量変化から単位面積当たりの重量変化率(重量変化率)を算出する。重量変化率を縦軸に、測定温度を横軸にとってプロットし、ガウシアンフィッティングを行って重量変化率分布曲線を得て、最大ピークのボトム温度(TGピーク温度)を求める。なお、測定点n-1(試料重量Wn-1、測定温度Tn-1)と次の測定点n(試料重量Wn、測定温度Tn)との間における重量変化率(ΔW)は以下の式4により算出される値である。
砥粒として砥粒1を準備した。砥粒1は、平均一次粒子径が35nm、平均二次粒子径が67nm、会合度が1.9、BET比表面積が78m2/g、真密度が1.80g/cm3、TGピーク温度が55.0℃の、ゾルーゲル法により作製したコロイダルシリカである。熱重量測定により得られた砥粒1(比較例1)についての重量変化率分布曲線を図2に示す。
上記砥粒1を以下の条件にて水熱処理して得た砥粒2を用いた以外は、比較例1と同様の手法により、研磨用組成物2を調製した。すなわち、1kgの砥粒1をバンドヒーター式オートクレーブ(耐圧硝子工業社製 TAS-1型)に投入した(シリカ濃度19.5質量%、pH7.3)。当装置は容器に密着したバンドヒーターにより温度を制御し、内部は攪拌しながら均一に試料に熱を加える仕組みになっている。水熱処理は、室温(25℃)を始点として、昇温速度が1.75℃/分、最高温度が160℃、最高温度(160℃)を維持する時間が1時間45分、最高温度(160℃)における圧力が0.63MPaになるよう設定し、プログラム運転で行った。水熱処理が完了した砥粒は、加熱時間が過剰に延びない様、直ちに室温環境下に戻した。上記手法により、砥粒2を得た。
砥粒として砥粒3を準備した。砥粒3は、平均一次粒子径が32nm、平均二次粒子径が61nm、会合度が1.9、BET比表面積が90m2/g、真密度が2.10g/cm3、TGピーク温度が44.5℃の、ゾルーゲル法により作製したコロイダルシリカである。
比較例2において、研磨用組成物のpHが4.0となるように、pH調整剤として乳酸を加えることにより研磨用組成物を調製した。上記以外は比較例2と同様にして、研磨用組成物4を作製した。熱重量測定により得られた砥粒3(実施例2)についての重量変化率分布曲線を図2に示す。
上記で得られた各研磨用組成物を用いて、研磨対象物(TEOS基板)を以下の研磨条件で研磨した際の研磨速度(TEOS RR)を測定した。
研磨機:小型卓上研磨機(日本エンギス株式会社製、EJ380IN)
研磨パッド:硬質ポリウレタン製パッド(ニッタ・ハース株式会社製、IC1000)
プラテン(定盤)回転速度:60[rpm]
ヘッド(キャリア)回転速度:60[rpm]
研磨圧力:3.0[psi]
研磨用組成物(スラリー)の流量:100[ml/min]
研磨時間:1[min]
研磨速度(研磨レート)は、研磨対象物の研磨前後の膜厚を光干渉式膜厚測定装置(株式会社SCREENホールディングス製、ラムダエースVM2030)によって求めて、その差を研磨時間で除することにより評価した(下記式参照)。
上記で得られた各研磨用組成物を用いて、下記方法に従って、欠陥(スクラッチ数)を評価した。詳細には、研磨対象物表面のスクラッチの個数は、ケーエルエー・テンコール(KLA-TENCOR)株式会社製の欠陥検出装置(ウエハ検査装置)“Surfscan(登録商標) SP2”を用いて、ウエハ全面(ただし外周2mmは除く)上の0.13μm以上の欠陥を検出した。検出した欠陥を、Review-SEM(RS-6000、株式会社日立ハイテクノロジーズ製)で全数観察することで、欠陥(スクラッチ)数を集計した。得られた欠陥(スクラッチ)数を下記の判断基準に従って評価した。
◎:0.13μm以上の欠陥が20個以下
○:0.13μm以上の欠陥が21個以上30個以下
△:0.13μm以上の欠陥が31個以上50個以下
×:0.13μm以上の欠陥が51個以上
Claims (8)
- 熱重量測定により得られる重量変化率分布曲線の25℃以上250℃以下の範囲における最大ピーク温度が30℃以上53℃以下であり、真密度が1.80g/cm3以上2.10g/cm3以下であり、会合度が1.5以上5.0以下である、ゾル-ゲル法により製造されたコロイダルシリカを含み、25℃でのpHが6.0未満である、研磨用組成物。
- さらに水を含有する、請求項1に記載の研磨用組成物。
- さらに酸を含む、請求項2に記載の研磨用組成物。
- 前記コロイダルシリカの含有量が、組成物全体に対して0質量%を超えて8質量%以下である、請求項1~3のいずれか1項に記載の研磨用組成物。
- 前記コロイダルシリカの真密度が1.90g/cm3以上2.10g/cm3以下である、請求項1~4のいずれか1項に記載の研磨用組成物。
- 酸素原子およびケイ素原子を含む研磨対象物を研磨するために用いられる、請求項1~5のいずれか1項に記載の研磨用組成物。
- 研磨対象物を研磨するために用いられる研磨用組成物の製造方法であって、
熱重量測定により得られる重量変化率分布曲線の25℃以上250℃以下の範囲における最大ピーク温度が30℃以上53℃以下であり、真密度が1.80g/cm3以上2.10g/cm3以下であり、会合度が1.5以上5.0以下であるシリカを準備すること、
当該シリカと、水とを混合すること、および
混合物の25℃でのpHを6.0未満に調整することを含み、
前記シリカを準備することは、ゾル-ゲル法によりコロイダルシリカを製造する段階を含む、製造方法。 - 酸素原子およびケイ素原子を含む研磨対象物を、請求項1~6のいずれか1項に記載の研磨用組成物を用いて、または
請求項7に記載の製造方法により研磨用組成物を得、当該研磨用組成物を用いて研磨対象物を研磨することを有する、研磨方法。
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