JP5029189B2 - 化学機械的研磨スラリー - Google Patents
化学機械的研磨スラリー Download PDFInfo
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- JP5029189B2 JP5029189B2 JP2007192130A JP2007192130A JP5029189B2 JP 5029189 B2 JP5029189 B2 JP 5029189B2 JP 2007192130 A JP2007192130 A JP 2007192130A JP 2007192130 A JP2007192130 A JP 2007192130A JP 5029189 B2 JP5029189 B2 JP 5029189B2
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- 238000005498 polishing Methods 0.000 title claims description 78
- 239000002002 slurry Substances 0.000 title claims description 50
- 239000000126 substance Substances 0.000 title claims description 5
- 239000002113 nanodiamond Substances 0.000 claims description 60
- 239000012736 aqueous medium Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 description 48
- 239000011737 fluorine Substances 0.000 description 19
- 229910052731 fluorine Inorganic materials 0.000 description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 16
- 229910021642 ultra pure water Inorganic materials 0.000 description 14
- 239000012498 ultrapure water Substances 0.000 description 14
- 239000006185 dispersion Substances 0.000 description 13
- 239000006061 abrasive grain Substances 0.000 description 11
- 238000005119 centrifugation Methods 0.000 description 10
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- 239000004094 surface-active agent Substances 0.000 description 10
- 239000010432 diamond Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910003460 diamond Inorganic materials 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- -1 alumina Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 4
- 239000011164 primary particle Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000003682 fluorination reaction Methods 0.000 description 3
- 125000003709 fluoroalkyl group Chemical group 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 2
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000013341 scale-up Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000000015 trinitrotoluene Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- SSTHBHCRNGPPAI-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro-n,n-bis(2-hydroxyethyl)octane-1-sulfonamide Chemical compound OCCN(CCO)S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SSTHBHCRNGPPAI-UHFFFAOYSA-N 0.000 description 1
- GFABGVSRKCKLKA-ONBPZOJHSA-N 2-[(2s,5r)-5-[(1r)-2-[4-(2-benzamidoethyl)phenoxy]-1-hydroxyethyl]-5-methyloxolan-2-yl]propan-2-yl acetate Chemical compound O1[C@H](C(C)(C)OC(=O)C)CC[C@]1(C)[C@H](O)COC(C=C1)=CC=C1CCNC(=O)C1=CC=CC=C1 GFABGVSRKCKLKA-ONBPZOJHSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 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
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- ZJXZSIYSNXKHEA-UHFFFAOYSA-N ethyl dihydrogen phosphate Chemical compound CCOP(O)(O)=O ZJXZSIYSNXKHEA-UHFFFAOYSA-N 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002221 fluorine Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 229930195712 glutamate Natural products 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- RRRXPPIDPYTNJG-UHFFFAOYSA-N perfluorooctanesulfonamide Chemical compound NS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F RRRXPPIDPYTNJG-UHFFFAOYSA-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
- 239000002244 precipitate Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
Landscapes
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Description
実施例1〜6
あらかじめ、ND(甘粛凌云納米材料有限公司製、ナノダイヤモンド精製粉、粒径:3〜10nm)を圧力1kPaで3時間、400℃に加熱して、NDに含まれる水分を除去した。乾燥処理を行ったNDを20g、ニッケル製の反応管に入れ、これに20℃で、フッ素ガスを流量20ml/min、アルゴンガスを流量380ml/minで流通した。そして、試料を400℃に加熱し、140時間、アルゴンガスとフッ素ガスの流通を継続し、NDとフッ素ガスを反応させ、フッ素化NDを作製した。なお、作製したフッ素化NDのフッ素含有量は元素分析により12重量%であった。
超純水にフッ素系界面活性剤として、ゾニールFSO(デュポン社製)を用い、このフッ素系界面活性剤を、超純水と添加するフッ素系界面活性剤の合計重量に対する含有量が5.5重量%となるように超純水に添加した混合液を100ml作製した。
超純水にフッ素系界面活性剤として、ゾニールFSO(デュポン社製)を用い、このフッ素系界面活性剤を、超純水と添加するフッ素系界面活性剤の合計重量に対する含有量が1.0重量%となるように超純水に添加した混合液を100ml作製した。
超純水に炭化水素系界面活性剤として、アデカノール(ADEKA社製)を用い、この炭化水素系界面活性剤を、超純水と添加する炭化水素系界面活性剤の合計重量に対する含有量が0.8重量%となるように超純水に添加した混合液を100ml作製した。
ND1gを超純水100mlに投入し、上記実施例1〜6と同条件で、超音波照射、遠心分離を行い、遠心分離後の上澄み液を採取して研磨スラリーを作製した。得られた研磨スラリーの粒子濃度は0.8重量%、最大粒子径は280nm、平均粒子径は79nmであった。
市販のダイヤモンド粉末(ニラコ社製、#4000)0.5gを超純水100mlに投入し、上記実施例1〜6と同じ条件で超音波照射を行った。得られた懸濁液は0.1時間以内に殆どの粒子が沈殿し、その上澄み部を研磨スラリーとして採取し粒子濃度を確認したところ0.01重量%以下であり、粒子が分散状態を保持した研磨スラリーは得られなかった。
Si基板上にスパッタ法で銅を堆積させた試料を作製し、あらかじめコロイダルシリカを砥粒とする市販のCMPスラリー(最大粒子径700nm、平均粒子径120nm)で、研磨面の表面粗さ(Ra)が10nmとなるように予備研磨を行ったものを被研磨物とした。この被研磨物に対して、CMP装置により、上記実施例1〜8と比較例2で得られた研磨スラリー、及び上記予備研磨で使用したコロイダルシリカを砥粒とする市販のCMPスラリー(比較例4)を用いて研磨試験を行った。
○:最大研磨速度と最小研磨速度の差が10nm/分以上20nm/分未満
×:最大研磨速度と最小研磨速度の差が20nm/分以上200nm/分未満
また、研磨表面の表面粗さ(Ra)は、AFM及び、光干渉法による表面形状測定器により測定した(測定範囲:2μm×2μm)。また、研磨試験後の被研磨物について、走査型電子顕微鏡(SEM)で任意の10カ所を観察し(1カ所の観察範囲:100μm×100μm)、スクラッチの有無を目視により確認して、以下の基準で評価した。
○:スクラッチ3〜5個
×:スクラッチ多数により、計測不能
結果を表2にまとめて記載する。
Claims (2)
- 化学機械的研磨用の研磨スラリーであって、水性媒質にフッ素化ナノダイヤモンドとフッ素系界面活性剤を含有させることを特徴とする研磨スラリー。
- フッ素系界面活性剤の含有量が、水性媒質とフッ素系界面活性剤の合計重量に対し0.1〜5重量%であり、かつ、フッ素化ナノダイヤモンドの含有量が、研磨スラリーの総重量に対して0.1〜5重量%である、請求項1に記載の研磨スラリー。
Priority Applications (2)
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JP2007192130A JP5029189B2 (ja) | 2006-11-13 | 2007-07-24 | 化学機械的研磨スラリー |
US11/935,595 US20080111102A1 (en) | 2006-11-13 | 2007-11-06 | Chemical Mechanical Polishing Slurry |
Applications Claiming Priority (3)
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JP2006306585 | 2006-11-13 | ||
JP2006306585 | 2006-11-13 | ||
JP2007192130A JP5029189B2 (ja) | 2006-11-13 | 2007-07-24 | 化学機械的研磨スラリー |
Publications (2)
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JP2008147617A JP2008147617A (ja) | 2008-06-26 |
JP5029189B2 true JP5029189B2 (ja) | 2012-09-19 |
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JP2014069308A (ja) * | 2012-09-27 | 2014-04-21 | Tadamasa Fujimura | 研磨材。 |
JP2014118559A (ja) * | 2012-12-17 | 2014-06-30 | Vision Development Co Ltd | 研磨材。 |
JP6329848B2 (ja) * | 2014-08-21 | 2018-05-23 | 株式会社ダイセル | 撥水コート膜及び該撥水コート膜を有する物品、並びに分散液 |
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JP2000001666A (ja) * | 1998-06-16 | 2000-01-07 | Okamoto Machine Tool Works Ltd | 研磨剤スラリ− |
CN101489928B (zh) * | 2006-06-05 | 2012-05-23 | 中央硝子株式会社 | 氟化纳米金刚石分散液的配制方法 |
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