TW201305321A - 研磨用組成物及使用該組成物之研磨方法及半導體裝置之製造方法 - Google Patents
研磨用組成物及使用該組成物之研磨方法及半導體裝置之製造方法 Download PDFInfo
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- TW201305321A TW201305321A TW101110822A TW101110822A TW201305321A TW 201305321 A TW201305321 A TW 201305321A TW 101110822 A TW101110822 A TW 101110822A TW 101110822 A TW101110822 A TW 101110822A TW 201305321 A TW201305321 A TW 201305321A
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- Prior art keywords
- acid
- polishing
- group
- copper
- polishing composition
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- MJZFXVHSXAHDFU-UHFFFAOYSA-N [1-hydroxy-2-(1-methyl-2h-pyridin-3-yl)-1-phosphonoethyl]phosphonic acid Chemical compound CN1CC(CC(O)(P(O)(O)=O)P(O)(O)=O)=CC=C1 MJZFXVHSXAHDFU-UHFFFAOYSA-N 0.000 description 1
- BRTBLZVYDKNGQX-UHFFFAOYSA-N [2-(4-aminophenyl)-1-hydroxy-1-phosphonoethyl]phosphonic acid Chemical compound NC1=CC=C(CC(O)(P(O)(O)=O)P(O)(O)=O)C=C1 BRTBLZVYDKNGQX-UHFFFAOYSA-N 0.000 description 1
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- JHBMGZJQVAIXNT-UHFFFAOYSA-N [4-[4-[bis(2-chloroethyl)amino]phenyl]-1-hydroxy-1-phosphonobutyl]phosphonic acid Chemical compound OP(=O)(O)C(P(O)(O)=O)(O)CCCC1=CC=C(N(CCCl)CCCl)C=C1 JHBMGZJQVAIXNT-UHFFFAOYSA-N 0.000 description 1
- QAAVPHVNSUOBBU-UHFFFAOYSA-N [NH4+].[NH4+].OP(O)=O.[O-]P([O-])=O Chemical compound [NH4+].[NH4+].OP(O)=O.[O-]P([O-])=O QAAVPHVNSUOBBU-UHFFFAOYSA-N 0.000 description 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- SBZOGCANHKAYKV-UHFFFAOYSA-N [[3-[bis(2-chloroethyl)amino]-4-methylphenyl]-hydroxy-phosphonomethyl]phosphonic acid Chemical compound CC1=CC=C(C(O)(P(O)(O)=O)P(O)(O)=O)C=C1N(CCCl)CCCl SBZOGCANHKAYKV-UHFFFAOYSA-N 0.000 description 1
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- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
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- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- WXANAQMHYPHTGY-UHFFFAOYSA-N cerium;ethyne Chemical compound [Ce].[C-]#[C] WXANAQMHYPHTGY-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
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- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- 229940112669 cuprous oxide Drugs 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 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
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 1
- GRKSQRAVWODMGW-UHFFFAOYSA-N ethylphosphonic acid Chemical compound [CH2]CP(O)(O)=O GRKSQRAVWODMGW-UHFFFAOYSA-N 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229940015872 ibandronate Drugs 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229940045996 isethionic acid Drugs 0.000 description 1
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- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- HIQXJRBKNONWAH-UHFFFAOYSA-N methylidenephosphane Chemical compound P=C HIQXJRBKNONWAH-UHFFFAOYSA-N 0.000 description 1
- BEGLCMHJXHIJLR-UHFFFAOYSA-N methylisothiazolinone Chemical compound CN1SC=CC1=O BEGLCMHJXHIJLR-UHFFFAOYSA-N 0.000 description 1
- VMMKGHQPQIEGSQ-UHFFFAOYSA-N minodronic acid Chemical compound C1=CC=CN2C(CC(O)(P(O)(O)=O)P(O)(O)=O)=CN=C21 VMMKGHQPQIEGSQ-UHFFFAOYSA-N 0.000 description 1
- 229950011129 minodronic acid Drugs 0.000 description 1
- PUUSSSIBPPTKTP-UHFFFAOYSA-N neridronic acid Chemical compound NCCCCCC(O)(P(O)(O)=O)P(O)(O)=O PUUSSSIBPPTKTP-UHFFFAOYSA-N 0.000 description 1
- 229950010733 neridronic acid Drugs 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229940046231 pamidronate Drugs 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229940089617 risedronate Drugs 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- JXOHGGNKMLTUBP-HSUXUTPPSA-N shikimic acid Chemical compound O[C@@H]1CC(C(O)=O)=C[C@@H](O)[C@H]1O JXOHGGNKMLTUBP-HSUXUTPPSA-N 0.000 description 1
- JXOHGGNKMLTUBP-JKUQZMGJSA-N shikimic acid Natural products O[C@@H]1CC(C(O)=O)=C[C@H](O)[C@@H]1O JXOHGGNKMLTUBP-JKUQZMGJSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-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
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XRASPMIURGNCCH-UHFFFAOYSA-N zoledronic acid Chemical compound OP(=O)(O)C(P(O)(O)=O)(O)CN1C=CN=C1 XRASPMIURGNCCH-UHFFFAOYSA-N 0.000 description 1
- 229960004276 zoledronic acid Drugs 0.000 description 1
Classifications
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- 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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- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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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
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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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- C09K3/00—Materials not provided for elsewhere
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- C09K3/1409—Abrasive particles per se
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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
- H01L21/302—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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- 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
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- 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
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- H01L21/34—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 not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
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- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
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Abstract
本發明之研磨用組成物係含有氧化劑及下述一般式(1)或(2)所表示之刮痕抑制劑:□式中,X1及X2各自獨立,表示氫原子、羥基、羧基、磷酸基、烷基、芳香基、烷基多胺基、烷基多磷酸基、烷基多羧基、烷基多胺基多磷酸基、或烷基多胺基多羧基。
Description
本發明關於一種研磨用組成物,其係使用在例如用以形成半導體裝置的配線的研磨;及使用該組成物之研磨方法。
在形成半導體裝置之配線的情況,首先,在具有溝槽的絕緣體層上依序形成遮蔽層及導體層。然後,藉由化學機械研磨,至少除去位於溝槽外的導體層的部分(導體層的外側部分)及位於溝槽外的遮蔽層的部分(遮蔽層的外側部分)。此用以至少除去導體層外側部分及遮蔽層外側部分的研磨,通常會分成第1研磨步驟與第2研磨步驟來進行。在第1研磨步驟中,為了使遮蔽層的上面露出,而除去導體層外側部分的一部分。此導體層外側部分的一部分的除去,通常首先以較快的研磨除去速度開始進行,然後抑制研磨除去速度,以使導體層的上面與遮蔽層的上面之間儘量不產生高低差。接下來,在第2研磨步驟中,為了使絕緣體層露出同時得到平坦的表面,而除去至少導體層外側部分的剩餘部分及遮蔽層外側部分(依照情況會包括絕緣體層的一部分)。藉此可得到由殘留在溝槽中的導體層部分所構成之導體配線部。
這種用以形成半導體裝置的配線的研磨,特別是在第2研磨步驟的研磨中,一般而言會使用含有酸等的研磨促
進劑及氧化劑,進一步因應必要含有研磨粒的研磨用組成物。另外還有文獻提出以研磨除去速度的提升與抑制研磨後的研磨對象物的缺陷為目的,而在研磨用組成物中添加有機酸或界面活性劑。例如在專利文獻1中揭示了一種研磨用組成物,其係含有兩種相異粒徑的研磨粒、三唑系化合物及如PBTC般的有機酸以謀求提升遮蔽層的研磨除去速度與抑制表面污垢等的缺陷。在專利文獻2中揭示了一種研磨用組成物,其係含有氧化金屬溶解劑、研磨粒及如HEDP般的不會使研磨粒沉降的界面活性劑,藉由使用不會使研磨粒沉降的界面活性劑以謀求提升研磨對象物的洗淨性與抑制異物附著於研磨對象物。在專利文獻3中揭示了一種研磨用組成物,其係含有氧化劑與如HEDP或NTMP般的特定化合物,藉由使用此特定化合物,主要在銅或銀的研磨對象物上形成金屬保護膜,以謀求抑制研磨對象物上的腐蝕等的缺陷。
然而,在藉由化學機械研磨形成半導體裝置之配線的情況,一般而言會有在導體配線部產生刮痕的情形。專利文獻1~3所揭示的研磨用組成物難以充分抑制這種刮痕。
在導體配線部產生刮痕的原因之一,認為是研磨用組成物中的研磨粒的凝集。因此,用來抑制刮痕的手段向來是採取除去研磨用組成物中粗大的研磨粒或防止研磨粒凝集、添加具有在導體層表面形成保護膜的作用的化學物質等方式。但是,藉由這些手段,刮痕並不會充分受到抑制
。
另外,用來抑制刮痕的其他手段,也會發生使原本不應該除去而位於溝槽中的導體層的部分比絕緣體層還更快地被研磨除去,因此導體配線部的上面與絕緣體層的上面之間的高低差大幅增加這樣的新問題。
[專利文獻1]日本特表2009-514196號公報[專利文獻2]日本特開2005-217360號公報[專利文獻3]日本特開2008-300858號公報
於是,本發明之目的在於提供一種研磨用組成物,其係不太會使導體配線部的上面與絕緣體層的上面之間的高低差增加,可適合使用於得到抑制導體配線部的刮痕之半導體裝置;及使用該組成物之研磨方法及半導體裝置之製造方法。
為了達成上述目的,在本發明之第1形態中提供一種研磨用組成物,其係含有氧化劑及下述一般式(1)或(2)所表示之刮痕抑制劑:
一般式(1)及(2)之中,X1及X2各自獨立,表示氫原子、羥基、羧基、磷酸基、烷基、芳香基、烷基多胺基、烷基多磷酸基、烷基多羧基、烷基多胺基多磷酸基、或烷基多胺基多羧基。
在本發明之第2形態中提供一種研磨方法,其係包含使用上述第1形態所關連之研磨用組成物,對至少一部分具有銅或銅合金的研磨對象物之表面進行研磨。
在本發明之第3形態中提供一種半導體裝置之製造方法,其係包含為了得到半導體裝置而使用上述第1形態所關連之研磨用組成物對至少一部分具有銅或銅合金的研磨對象物之表面進行研磨。
以下對本發明其中一個實施形態作說明。
本實施形態之研磨用組成物係將氧化劑及刮痕抑制劑,宜為與研磨粒及研磨促進劑一起混合至水中而調製。所以,研磨用組成物含有氧化劑及刮痕抑制劑,宜為進一步含有研磨粒及研磨促進劑。
本實施形態之研磨用組成物主要使用於用以形成先前所說明的半導體裝置的配線的研磨,較具體而言為第2研
磨步驟的研磨。絕緣體層之材質並未受到特別限定,而可列舉例如氧化矽、含氟的氧化矽、含硼的氧化矽、含碳的氧化矽、含Si-H的氧化矽、多孔質氧化矽、含甲基的氧化矽、多孔質且含甲基的氧化矽等的氧化矽系絕緣體層、聚醯亞胺系高分子、帕里綸(Parylene)系高分子、鐵氟龍系高分子、其他共聚合系高分子等的高分子系絕緣體層及無定形碳等。其中,氧化矽系絕緣體層為佳,氧化矽、含氟的氧化矽、含硼的氧化矽、含碳的氧化矽為特佳。導體層係由銅或銅合金所構成。遮蔽層的材質並未受到特別限定,而可列舉例如鉭、氮化鉭、其他鉭合金、鈦、氮化鈦、其他鈦合金、鎢、氮化鎢、其他鎢合金。其中,鉭、氮化鉭、鈦、氮化鈦、鎢、氮化鎢為佳,鉭、氮化鉭為特佳。
研磨用組成物中所含有的氧化劑係具有使研磨對象物之表面,特別是遮蔽層及導體層的表面氧化的作用,可提升研磨用組成物所產生的研磨除去速度。
氧化劑可使用例如過氧化物。過氧化物的具體例可列舉例如過氧化氫、過醋酸、過碳酸鹽、過氧化尿素及過氯酸、以及過硫酸鈉、過硫酸鉀、過硫酸銨等的過硫酸鹽。其中,從研磨除去速度的觀點看來,以過氧化氫及過硫酸鹽為佳,從提升水溶液中的安定性及減輕環境負荷的觀點看來,係以過氧化氫為特佳。
研磨用組成物中的氧化劑的含量係以0.1g/L以上為佳,較佳為0.5g/L以上,更佳為1g/L以上。隨著氧化劑的含量變多,研磨用組成物所產生的研磨除去速度會更加提升。
研磨用組成物中的氧化劑的含量另外以200g/L以下為佳,較佳為100g/L以下,更佳為50g/L以下。
隨著氧化劑的含量變少,較能夠抑制研磨用組成物的材料成本,此外還可減輕研磨使用後的研磨用組成物的處理,亦即廢液處理的負荷。另外還可減少氧化劑造成的研磨對象物表面的過度氧化,特別是導體層的過度氧化發生的顧慮。
在導體配線部產生刮痕的原因除了研磨用組成物中的研磨粒之凝集之外,還考慮因為氧化劑由導體層溶出的銅或銅合金會產生氧化銅或氫氧化銅等的不溶性的銅化合物。這些銅化合物與導體配線部的銅或銅合金相比硬度較高,因此會由於衝撞至導體配線部而使導體配線部容易產生刮痕。例如若以莫氏硬度作比較,則氧化亞銅為3.5~4、氧化銅(II)為約4.5、氫氧化銅(II)為3.5~4,相對於此,銅的硬度為2.5~3。
本實施形態之研磨用組成物中所含有的刮痕抑制劑,會使氧化銅或氫氧化銅等的銅化合物溶於研磨用組成物中,結果會有抑制導體配線部的刮痕的作用。另外,刮痕抑
制劑具有選擇性地使氧化銅或氫氧化銅等的銅化合物比導體配線部的銅或銅合金較先溶解的作用,因此不太會使導體配線部的上面與絕緣體層的上面之間的高低差比第1研磨步驟結束時的高低差更增加。另外,氧化銅或氫氧化銅等的銅化合物會有成為研磨粒凝集時的核心的顧慮,而刮痕抑制劑還有抑制這種以研磨粒凝集為原因所產生的刮痕的效果。
所使用的刮痕抑制劑係下述一般式(1)或(2)所表示的化合物:
此處一般式(1)及(2)之中,X1及X2各自獨立,表示氫原子、羥基、羧基、磷酸基、烷基、芳香基、烷基多胺基、烷基多磷酸基、烷基多羧基、烷基多胺基多磷酸基、或烷基多胺基多羧基。
一般式(1)所表示的化合物的具體例可列舉例如羥基膦醯基羧酸、(((2-羥乙基)(2-((膦醯基甲基)胺基)乙基)胺基)甲基)膦酸、乙二胺-N,N’-雙(醋酸)-N,N’-雙(亞甲基膦酸)、(((2-(((雙(羥甲基)膦基)甲基)(膦酸酯甲基)胺基)乙基)醯亞胺基)雙(亞甲基))雙膦酸酯、二乙三胺五(亞甲基膦酸)、二乙三胺三(亞甲基膦酸)、(乙烷-1,2-二基雙(亞胺基
((2-羥苯基)亞甲基)))雙膦酸、二乙三胺五(亞甲基膦酸)、(乙烷-1,2-二基雙((3-(雙(膦醯基甲基)胺基)丙基)醯亞胺基)雙(亞甲基))雙膦酸及[乙烷-1,2-二基雙(醯亞胺基丙烷-2,2-二基)]雙(膦酸)等。
一般式(2)所表示的化合物的具體例可列舉例如乙二胺肆亞甲基膦酸、羥基亞乙基二膦酸、甲烷羥基二膦酸、2-羥基-2-膦醯基丙酸、帕米膦酸、阿侖膦酸、(1,6-二羥基-1,6-己二亞基)肆-膦酸、1-羥基丙烷-1,1-二膦酸、1-羥基丁烷-1,1-二膦酸、4-N,N-二甲基胺基-1-羥基亞丁基-1,1-二膦酸、二環氧丙基-(3-(3,3-雙膦醯基-3-羥基丙基胺基)-2-羥丙基)脲唑、4-(4-(雙(2-氯乙基)胺基)苯基)-1-羥基丁烷-1,1-雙膦酸、(1-羥基-3-(3-吡啶基)亞丙基)雙膦酸、(1-羥基-2-(咪唑并(1,2-A)-吡啶-3-基)亞乙基)雙膦酸、((3-(雙(2-氯乙基)胺基)-4-甲基苯基)羥基亞甲基)雙-膦酸、N-[甲基(4-苯基丙基)]-3-胺基丙基-1-羥基-1,1-雙膦酸膦酸酯、N-(4-苯基丁基)-3-胺基丙基-1-羥基-1,1-雙膦酸、N-[甲基(4-苯基丁基)]-3-胺基丙基-1-羥基-1,1-雙膦酸、[1-羥基-3-[甲基(2-苯氧基乙基)胺基]亞丙基-1,1-雙膦酸、1-羥基-3-胺基丙烷-1,1-二膦酸-gd-dtpa、N-[甲基(4-苯基乙基)]-3-胺基丙基-1-羥基-1,1-雙膦酸、1-羥基-3-[甲基(戊基)胺基]-1-膦醯基丙基膦酸、伊班膦酸鹽、1-(4-羥基苯氧基)乙烷-1,1-雙膦酸四特戊醯氧基甲基、2-(N-甲基-3-吡啶基)-1-羥基亞乙基雙膦酸、(1-羥基-2-(1H-咪唑-1-基)亞乙基)雙-膦酸、2-(4-胺基苯基)-1-羥基-乙烷-1,1-雙膦酸、十八
烷基-1-羥基-1,1-雙膦酸、1-羥基丁烷-1,1-雙膦酸、3-(3-吡啶基)-1-羥基丙烷-1,1-雙膦酸、2-(2-吡啶基)-1-羥基-乙烷-1,1-雙膦酸、2-(4-吡啶基硫代)-1-羥基-乙烷-1,1-雙膦酸、唑來膦酸、利塞膦酸、奈立膦酸、5-胺基戊烷-1-羥基-1,1-雙膦酸、二癸基銨雙膦酸、N-(3-羥基-3,3-二膦醯基丙基)-N,N,N’,N’,N’-五甲基乙烷-1,2-二銨、N-(3-羥基-3,3-二膦醯基丙基)-N,N,N’,N,N’-五甲基己烷-1,2-二銨、N-(8-羥基-8,8-二膦醯基辛基)-N,N,N’,N,N’-五甲基乙烷-1,2-二銨、三乙二醇雙膦酸、四乙二醇雙膦酸、五乙二醇雙膦酸、PEG(350)雙膦酸、(4-乙醯基胺基)-1-羥基亞丁基-1,1-雙膦酸、4-羥基-N,N,N-三甲基-4,4-二膦醯基丁烷-1-銨、8-羥基-N,N,N-三甲基-8,8-二膦醯基辛烷-1-銨、氫化2-(1,2-二氫吡啶-3-基)-1-羥基-1-(羥基次膦酸)乙基膦酸、1-羥基異亞丁基二膦酸及米諾膦酸等。
其中以乙二胺肆亞甲基膦酸、羥基亞乙基二膦酸、甲烷羥基二膦酸、2-羥基-2-膦醯基丙酸、帕米膦酸、阿侖膦酸、(1,6-二羥基-1,6-己二亞基)肆-膦酸、1-羥基丙烷-1,1-二膦酸、羥基膦醯基羧酸、(((2-羥乙基)(2-((膦醯基甲基)胺基)乙基)胺基)甲基)膦酸、乙二胺-N,N’-雙(醋酸)-N,N’-雙(亞甲基膦酸)、(((2-(((雙(羥甲基)膦基)甲基)(膦酸酯甲基)胺基)乙基)醯亞胺基)雙(亞甲基))雙膦酸酯、二乙三胺五(亞甲基膦酸)及二乙三胺三(亞甲基膦酸)為佳,乙二胺肆亞甲基膦酸、羥基亞乙基二膦酸及羥基膦醯基羧酸為特佳。
研磨用組成物中的刮痕抑制劑的含量一般而言,以0.001mmol/L以上為佳,較佳為0.01mmol/L以上,更佳為0.1 mmol/L以上。隨著刮痕抑制劑的含量變多,導體配線部的刮痕會更受抑制。
研磨用組成物中的刮痕抑制劑的含量另外還以10mmol/L以下為佳,較佳為5mmol/L以下,更佳為3mmol/L以下。隨著刮痕抑制劑的含量變少,較能夠抑制研磨用組成物的材料成本,此外還較能夠抑制在導體配線部的上面與絕緣體層的上面之間產生高低差。
研磨用組成物中所任意含有的研磨粒係具有對於研磨對象物實施機械研磨的作用,以提升研磨用組成物所產生的研磨除去速度,特別是提升遮蔽層及絕緣體層的研磨除去速度為目的而使用。
所使用的研磨粒可為無機粒子、有機粒子及有機無機複合粒子之任一者。無機粒子的具體例可列舉例如由二氧化矽、氧化鋁、氧化鈰、二氧化鈦等的金屬氧化物所構成之粒子、以及氮化矽粒子、碳化矽粒子及氮化硼粒子。有機粒子的具體例可列舉例如聚甲基丙烯酸甲酯(PMMA)粒子。其中以二氧化矽為佳,從刮痕抑制與研磨除去速度的觀點看來,特佳為膠狀二氧化矽。
研磨用組成物中的研磨粒的含量係以0.005質量%以上為佳,較佳為0.5質量%以上,更佳為1質量%以上。隨
著研磨粒的含量變多,研磨用組成物所產生的研磨除去速度會更提升。
研磨用組成物中的研磨粒的含量另外還以10質量%以下為佳,較佳為質量8%以下,更佳為5質量%以下。隨著研磨粒的含量變少,較能夠抑制研磨用組成物之材料成本,此外還較能夠抑制在導體配線部的上面與絕緣體層的上面之間產生高低差。
研磨粒的平均初級粒徑係以5nm以上為佳,較佳為7nm以上,更佳為10nm以上。隨著研磨粒的平均初級粒徑變大,研磨用組成物所產生的研磨除去速度會更提升。
研磨粒的平均初級粒徑另外還以100nm以下為佳,較佳為60nm以下,更佳為40nm以下。一般而言,導體層比絕緣體層還容易研磨除去,在導體配線部的上面與絕緣體層的上面之間,會因為滯留在導體層上部的研磨粒而有產生研磨粒的粒徑程度的高低差的顧慮。隨著研磨粒的平均初級粒徑變小,較能夠抑制因為這樣的理由而在導體配線部的上面與絕緣體層的上面之間產生的高低差。此外,研磨粒的平均初級粒徑之值係基於例如BET法所測得的研磨粒之比表面積,由下式:平均初級粒徑[nm]=常數/比表面積[m2/g]來作計算。此外,在研磨粒為膠狀二氧化矽等的二氧化矽的情況,上述常數為2121。
研磨用組成物中所任意含有的研磨促進劑是為了以提
升遮蔽層的研磨除去速度之目的而使用。所使用的研磨促進劑可為無機酸或有機酸之任一者。
無機酸的具體例可列舉例如硫酸、硝酸、硼酸、碳酸、次亞磷酸、亞磷酸及磷酸。
有機酸的具體例可列舉例如蟻酸、醋酸、丙酸、酪酸、纈草酸、2-甲基酪酸、正己酸、3,3-二甲基酪酸、2-乙基酪酸、4-甲基戊酸、正庚酸、2-甲基己酸、正辛酸、2-乙基己酸、安息香酸、羥乙酸、水楊酸、甘油酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、馬來酸、苯二甲酸、蘋果酸、酒石酸、檸檬酸及乳酸等的羧酸、以及甲磺酸、乙磺酸及羥乙磺酸等的有機硫酸。
亦可使用無機酸或有機酸的銨鹽或鹼金屬鹽等的鹽以代替無機酸或有機酸,或與無機酸或有機酸加以組合。在弱酸與強鹼、強酸與弱鹼、或弱酸與弱鹼的組合的情況,可期待有pH的緩衝作用。
其中,從提升遮蔽層的研磨除去速度的效果高這點看來,適合作為研磨促進劑的物質為蘋果酸、酒石酸、檸檬酸、羥乙酸、有機硫酸或該等的銨鹽或鹼金屬鹽,從導體層的蝕刻溶解性低這點看來,以有機硫酸或該等的銨鹽或鹼金屬鹽為更佳,羥乙磺酸或其銨鹽或鹼金屬鹽為最佳。
研磨用組成物中的研磨促進劑的含量係以0.01g/L以上為佳,較佳為0.1g/L以上,更佳為1g/L以上。
隨著研磨促進劑的含量變多,研磨用組成物所產生的研磨除去速度會更提升。
研磨用組成物中的研磨促進劑的含量另外還以50g/L以下為佳,較佳為30g/L以下,更佳為15g/L以下。
隨著研磨促進劑的含量變少,可減少研磨促進劑造成的研磨對象物表面的過度蝕刻發生的顧慮。
在25℃的環境下所測得的研磨用組成物之pH係以7以上為佳,較佳為8以上,更佳為9以上。隨著研磨用組成物之pH值變大,研磨用組成物產生的遮蔽層及絕緣體層的研磨除去速度會更提升。
25℃的環境下所測得的研磨用組成物的pH另外還以12以下為佳,較佳為11以下,更佳為10以下。隨著研磨用組成物之pH值變小,可抑制研磨用組成物中的研磨粒的溶解。另外,隨著研磨用組成物的pH值變小,可抑制原本不該除去而位於溝槽中的導體層的部分受到研磨除去。
為了得到所希望的pH,可使用任意的鹼、酸及緩衝劑。
依據本實施形態可得到以下的優點。
本實施形態之研磨用組成物係含有氧化劑及刮痕抑制劑。
因為氧化劑而由導體層溶出的銅或銅合金所產生的氧化銅或氫氧化銅等的不溶性的銅化合物,會藉由刮痕抑制劑的作用而溶於研磨用組成物中,藉此可抑制導體配線部
的刮痕。通常在使用用以使這種不溶性的銅化合物溶於研磨用組成物中的化合物的情況,原本不該除去而位於溝槽中的導體層的部分會比絕緣體層更快速地研磨除去,因此導體配線部的上面與絕緣體層的上面之間的高低差會大幅增加,而本實施形態的情況,這種高低差的增加不太會發生。這認為是本實施形態所使用的刮痕抑制劑會選擇性地使氧化銅或氫氧化銅等的銅化合物比導體配線部的銅或銅合金較先溶解。另外,刮痕抑制劑還可抑制以氧化銅或氫氧化銅等的銅化合物為核心導致的研磨粒凝集。所以,本實施形態之研磨用組成物不太會使導體配線部的上面與絕緣體層的上面與之間的高低差增加,可適合使用於得到抑制導體配線部的刮痕的半導體裝置。
前述實施形態亦可如下述方式作變更。
前述實施形態之研磨用組成物亦可含有兩種以上的氧化劑。
前述實施形態之研磨用組成物亦可含有兩種以上的刮痕抑制劑。
前述實施形態之研磨用組成物亦可含有兩種以上的研磨粒。
前述實施形態之研磨用組成物亦可含有兩種以上的研磨促進劑。
前述實施形態之研磨用組成物亦可因應必要進一步含有如防腐劑或防黴劑般周知的添加劑。防腐劑及防黴劑的具體例可列舉例如2-甲基-4-異噻唑啉-3-酮、5-氯-2-甲基-
4-異噻唑啉-3-酮等的異噻唑啉系防腐劑、對羥安息香酸酯類及苯氧基乙醇。
前述實施形態之研磨用組成物可為一液型或可為以二液型為首的多液型。
前述實施形態之研磨用組成物亦可藉由使用水等的稀釋液將研磨用組成物的原液稀釋成例如10倍以上而調製。
前述實施形態之研磨用組成物亦可使用在用以形成半導體裝置的配線的研磨以外的用途。
接下來對本發明之實施例及比較例作說明。
將氧化劑、刮痕抑制劑或其替代化合物、研磨粒及研磨促進劑混合至水中,調製出實施例1~3及比較例1~8之研磨用組成物。將實施例1~3之研磨用組成物中的刮痕抑制劑的細節及比較例1~8之研磨用組成物中的刮痕抑制劑的替代的化合物的細節表示於表1之"刮痕抑制劑或其替代化合物"的欄位。此外,雖然未揭示於表1,而實施例1~3及比較例1~8之研磨用組成物任一者皆含有作為氧化劑的過氧化氫3.47g/L、作為研磨粒而平均初級粒徑為30nm的膠狀二氧化矽4質量%,及作為研磨促進劑的羥乙磺酸3.78g/L。另外,任一研磨用組成物皆藉由添加氫氧化鉀將25℃的環境下所測得的pH值調整成10而後使用。
第1研磨步驟係使用Fujimi Incorporated股份有限公司製的研磨用組成物PLANERLITE 7105,對於圖案化銅晶圓(ATDF754遮罩;由銅所構成的導體層的厚度7000Å、溝槽的深度3000Å、由鉭所構成的遮蔽層的厚度100Å,絕緣體層採用二氧化矽)的表面,以表2所記載的第1研磨條件研磨至銅膜厚成為2500Å為止。然後,對相同圖案化銅晶圓的表面使用相同研磨用組成物,以表3所記載之第2研磨條件研磨至遮蔽層的上面露出為止。像這樣研磨之後,在圖案化銅晶圓表面的100μm寬的銅配線部與
100μm寬的絕緣體部交互排列的區域測定銅配線部的上面與絕緣體部的上面之間的高低差的大小,其結果為約450Å。只要可得到前述高低差的大小,則泥漿不限於Fujimi Incorporated股份有限公司製的研磨用組成物PLANERLITE 7105,亦可使用一般的銅研磨用組成物。
接下來,第2研磨步驟係使用實施例1~3及比較例1~8之各研磨用組成物,以表4所記載的第3研磨條件,研磨第1研磨步驟後的圖案化銅晶圓,除去位於溝槽外的導體層的部分及遮蔽層的部分以及絕緣體層的一部分。
對於第2研磨步驟後的圖案化銅晶圓的表面使用暗視野式晶圓缺陷檢查裝置(日立HighTechnologies股份有限公司製的IS-3200)作測定,求得產生表面缺陷的座標值之後,使用缺陷檢視電子顯微鏡(defect review-SEM)(日立HighTechnologies股份有限公司製的RS-4000)觀察表面缺陷。由所觀察到的表面缺陷之中隨機抽出100個,在這些表面缺陷之中統計出被分類成刮痕的缺陷的個數。然後基於此統計值計算每一枚晶圓的刮痕數而求得。將結果揭示於表1之"刮痕個數"的欄位。每一枚晶圓的刮痕個數係以20個以下為佳,較佳為15個以下,更佳為10個以下。
在第2研磨步驟後的圖案化銅晶圓的表面之100μm寬
的銅配線部與100μm寬的絕緣體部交互排列的區域之中,使用廣域AFM(wide area AFM)(日立建機FineTech股份有限公司製的WA-1300)測定銅配線部的上面與絕緣體部的上面之間的高低差的大小,亦即測定銅配線部的上面的水平高度相對於絕緣體部的上面的水平高度低了多少。將結果揭示於表1之"高低差的大小"的欄位。此外,高低差的大小係以500Å以下為佳。
在第2研磨步驟後的圖案化銅晶圓所測得的上述高低差之值加上在第2研磨步驟中研磨掉的絕緣體層的厚度,進一步減去第1研磨步驟後之圖案化銅晶圓所測得的高低差之值(約450Å),將所得到的值除以第2研磨步驟的研磨時間120秒鐘,藉此求得銅研磨速度。將結果揭示於表1之"銅研磨速度"的欄位。此外,在第2研磨步驟中研磨掉的絕緣體層的厚度,係藉由使用膜厚測定器(KLA-Tencor股份有限公司製的A-SET)測定第2研磨步驟後的圖案化銅晶圓的絕緣體層的厚度,將所得到的值由溝槽深度3000Å扣除而求得。
使用實施例1~3及比較例1~8之各研磨用組成物,並以表4所記載的第3研磨條件對鉭空白晶圓的表面研磨60秒鐘時,將使用薄片電阻測定器(日立國際電氣股份有
限公司製的VR-120SD/8)所測得的研磨前後的鉭空白晶圓的厚度的差除以研磨時間(60秒鐘),藉此求得鉭研磨速度。將結果揭示於表1之"鉭研磨速度"的欄位。
在第2研磨步驟中,藉由將研磨掉的絕緣體層的厚度除以絕緣體層研磨時間而求得二氧化矽研磨速度。將結果揭示於表1之"二氧化矽研磨速度"的欄位。此外,在第2研磨步驟中,研磨掉的絕緣體層的厚度係藉由使用膜厚測定器(KLA-Tencor股份有限公司製的A-SET)測定第2研磨步驟後的圖案化銅晶圓的絕緣體層的厚度,將所得到的厚度值由溝槽深度3000Å扣除而求得。絕緣體層研磨時間,係使用由第2研磨步驟的研磨時間120秒鐘減去鉭的清除時間而得的值。鉭的清除時間是指除去絕緣體層上的遮蔽層所必要的時間,且藉由將遮蔽層的厚度100Å除以上述鉭研磨速度而求得。
如表1所示般,在使用實施例1~3之研磨用組成物的情況不太會使高低差增加,可大幅抑制刮痕。相對於此,使用比較例1~8之研磨用組成物的情況,刮痕的數目很多。
另外,在第1研磨步驟後的圖案化銅晶圓中,一般而言,在銅配線部的上面與絕緣體部的上面之間會產生高低差,在第2研磨步驟為了減少此高低差,第2研磨步驟所使用的研磨用組成物宜為使鉭研磨速度及二氧化矽研磨速
度高於銅研磨速度。此情況下,在第2研磨步驟不僅除去位於溝槽外的導體層的部分及遮蔽層的部分,還除去絕緣體層的一部分,因此不太會使銅配線部的上面與絕緣體部的上面之間的高低差增加,而能夠抑制銅配線部的刮痕。
Claims (5)
- 一種研磨用組成物,其係對至少一部分具有銅或銅合金的研磨對象物之表面進行研磨用途所使用的研磨用組成物,並且含有氧化劑及下述一般式(1)或(2)所表示之刮痕抑制劑:
- 如申請專利範圍第1項之研磨用組成物,其中前述刮痕抑制劑係乙二胺肆亞甲基膦酸、羥基亞乙基二膦酸、甲烷羥基二膦酸、2-羥基-2-膦醯基丙酸、帕米膦酸(pamidronic acid)、阿侖膦酸(alendronic acid)、(1,6-二羥基-1,6-己二亞基)肆膦酸、羥基膦醯基羧酸、(((2-羥乙基)(2-((膦醯基甲基)胺基)乙基)胺基)甲基)膦酸、乙二胺-N,N’-雙(醋酸)-N,N’-雙(亞甲基膦酸)、(((2-(((雙(羥甲基)膦基)甲基)(膦酸酯甲基)胺基)乙基)醯亞胺基)雙(亞甲基))雙膦酸酯、二乙三胺五(亞甲基膦酸)、或二乙三胺三(亞甲基膦酸)。
- 如申請專利範圍第1或2項之研磨用組成物,其中 在25℃的環境下所測得的pH值係在7~12的範圍。
- 一種研磨方法,其係包含使用如申請專利範圍第1或2項之研磨用組成物對至少一部分具有銅或銅合金的研磨對象物之表面進行研磨。
- 一種半導體裝置之製造方法,其係包含為了得到半導體裝置而使用如申請專利範圍第1或2項之研磨用組成物,對至少一部分具有銅或銅合金的研磨對象物之表面進行研磨。
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JP4231632B2 (ja) | 2001-04-27 | 2009-03-04 | 花王株式会社 | 研磨液組成物 |
JP2004231748A (ja) * | 2003-01-29 | 2004-08-19 | Fuji Photo Film Co Ltd | 金属用研磨液及び研磨方法 |
JP2005217360A (ja) | 2004-02-02 | 2005-08-11 | Hitachi Chem Co Ltd | 金属用研磨液及び研磨方法 |
JP2005220365A (ja) * | 2004-02-03 | 2005-08-18 | Mitsubishi Gas Chem Co Inc | 銅および銅合金の化学研磨液 |
CN1955249B (zh) | 2005-10-28 | 2012-07-25 | 安集微电子(上海)有限公司 | 用于钽阻挡层的化学机械抛光浆料 |
US20100176335A1 (en) | 2007-06-08 | 2010-07-15 | Techno Semichem Co., Ltd. | CMP Slurry Composition for Copper Damascene Process |
JP2009054796A (ja) * | 2007-08-27 | 2009-03-12 | Fujifilm Corp | 金属用研磨液、及び化学的機械的研磨方法 |
CN101418189B (zh) * | 2007-10-26 | 2013-10-02 | 安集微电子(上海)有限公司 | 一种金属铜的抛光液 |
TWI467055B (zh) * | 2007-12-21 | 2015-01-01 | Wako Pure Chem Ind Ltd | 蝕刻劑及蝕刻方法 |
JP2008300858A (ja) | 2008-07-15 | 2008-12-11 | Fujifilm Corp | 金属用研磨液及び研磨方法 |
-
2012
- 2012-03-28 WO PCT/JP2012/058258 patent/WO2012133591A1/ja active Application Filing
- 2012-03-28 EP EP12764130.6A patent/EP2693460A4/en not_active Withdrawn
- 2012-03-28 JP JP2013507699A patent/JPWO2012133591A1/ja active Pending
- 2012-03-28 US US14/007,272 patent/US9150758B2/en active Active
- 2012-03-28 KR KR1020137028155A patent/KR20140048868A/ko not_active Application Discontinuation
- 2012-03-28 TW TW101110822A patent/TWI567180B/zh active
- 2012-03-28 CN CN201280015514.3A patent/CN103547651A/zh active Pending
Also Published As
Publication number | Publication date |
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EP2693460A4 (en) | 2015-07-15 |
CN103547651A (zh) | 2014-01-29 |
WO2012133591A1 (ja) | 2012-10-04 |
TWI567180B (zh) | 2017-01-21 |
EP2693460A1 (en) | 2014-02-05 |
KR20140048868A (ko) | 2014-04-24 |
JPWO2012133591A1 (ja) | 2014-07-28 |
US9150758B2 (en) | 2015-10-06 |
US20140141612A1 (en) | 2014-05-22 |
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