TWI565797B - 電子元件用洗淨液組成物 - Google Patents
電子元件用洗淨液組成物 Download PDFInfo
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- TWI565797B TWI565797B TW101145895A TW101145895A TWI565797B TW I565797 B TWI565797 B TW I565797B TW 101145895 A TW101145895 A TW 101145895A TW 101145895 A TW101145895 A TW 101145895A TW I565797 B TWI565797 B TW I565797B
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- Taiwan
- Prior art keywords
- cleaning liquid
- liquid composition
- cleaning
- composition according
- acid
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims description 81
- 239000000203 mixture Substances 0.000 title claims description 57
- 239000007788 liquid Substances 0.000 title claims description 54
- 239000010949 copper Substances 0.000 claims description 59
- -1 ethylene diamine oxime Chemical class 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 33
- 239000002738 chelating agent Substances 0.000 claims description 32
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 150000007514 bases Chemical class 0.000 claims description 22
- 239000004065 semiconductor Substances 0.000 claims description 21
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
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- 238000005498 polishing Methods 0.000 claims description 9
- 150000003868 ammonium compounds Chemical class 0.000 claims description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 4
- OXHDYFKENBXUEM-UHFFFAOYSA-N glyphosine Chemical compound OC(=O)CN(CP(O)(O)=O)CP(O)(O)=O OXHDYFKENBXUEM-UHFFFAOYSA-N 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 239000005562 Glyphosate Substances 0.000 claims description 2
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 claims description 2
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- 239000012141 concentrate Substances 0.000 claims 2
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- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 7
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- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 5
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- 239000010410 layer Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
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- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 description 3
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- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 description 2
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 2
- FCKYPQBAHLOOJQ-UWVGGRQHSA-N 2-[[(1s,2s)-2-[bis(carboxymethyl)amino]cyclohexyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)[C@H]1CCCC[C@@H]1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UWVGGRQHSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 2
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
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- XFLSMWXCZBIXLV-UHFFFAOYSA-N n,n-dimethyl-2-(4-methylpiperazin-1-yl)ethanamine Chemical compound CN(C)CCN1CCN(C)CC1 XFLSMWXCZBIXLV-UHFFFAOYSA-N 0.000 description 2
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- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
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- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
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- 229920000620 organic polymer Polymers 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
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- 238000003825 pressing Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- VIULODLMHCJIDN-UHFFFAOYSA-N tetraazanium tetraacetate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O VIULODLMHCJIDN-UHFFFAOYSA-N 0.000 description 1
- 150000003536 tetrazoles Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
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- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/79—Phosphine oxides
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/36—Organic compounds containing phosphorus
- C11D3/361—Phosphonates, phosphinates or phosphonites
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/36—Organic compounds containing phosphorus
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/16—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions using inhibitors
- C23G1/18—Organic inhibitors
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
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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
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
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- 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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
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- 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
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
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Description
本發明關於一種使用於電子裝置(electronic device)之洗淨的洗淨液組成物。更詳而言,在半導體元件(semiconductor element)等電子裝置之製造步驟中,使用於洗淨經施加研磨處理、蝕刻處理、化學機械研磨(在下文中,也稱為「CMP」)處理等的金屬材料表面,特別是具有銅配線之半導體基板之洗淨液,以及使用此之該電子裝置之洗淨方法。
伴隨著IC(積體電路)之高積體化,由於微量之雜質對於裝置之性能及產率具有大幅的影響,因此要求嚴格的污染控制。亦即,要求嚴格地控制基板之污染,因此在半導體製造之各步驟中使用各種洗淨液。
一般而言,作為半導體用基板洗淨液,為移除粒子污染係使用屬於鹼性洗淨液之氨-過氧化氫水溶液-水(SC-1),而為移除金屬污染則使用屬於酸性洗淨液之硫酸-過氧化氫水溶液、鹽酸-過氧化氫水溶液-水(SC-2)、稀氫氟酸等,且各洗淨液係因應目的而單獨或組合使用。
在另一方面,伴隨著裝置微細化及多層配線結構化的
進展,在各步驟中係要求基板表面之更精密的平坦化(planarization),並在半導體製造步驟中導入一種CMP(化學機械研磨)技術作為新穎的技術,其係一邊供應研磨粒子(abrasive particle)與化學藥品之混合物漿液(slurry),一邊將晶圓壓著於稱為拋光用軟皮(buff)之研磨布(abrasive cloth)上,並藉由將其旋轉而將化學作用與物理作用併用,以進行將絕緣膜或金屬材料加以研磨及平坦化。而且,在此同時,將加以平坦化的基板表面或構成漿液的物質也已發生變化。經CMP後之基板表面係會由於包含於漿液中之以氧化鋁或二氧化矽、氧化鈰粒子為代表的粒子、或將被研磨的表面之構成物質或包含於漿液中源自藥品之金屬雜質而受到污染。
此等污染物由於會造成圖案缺陷或密著性不良、電特性不良等,因此必須在進入下一個步驟前完全加以移除。為移除此等污染物之一般的CMP後洗淨(post-CMP cleaning),係實施併用洗淨液之化學作用與藉由聚乙烯醇製海綿刷子等的物理作用之刷子洗淨。作為洗淨液,先前對於粒子之移除係使用如氨之鹼。此外,對於金屬污染之移除,在專利文獻1或專利文獻2中提案一種使用有機酸與錯化劑(complexing agent)的技術。
並且,同時移除金屬污染與粒子污染的技術,在專利文獻3提案一種組合有機酸與界面活性劑之洗淨液。然而,伴隨著半導體元件的配線圖案微細化之進行,在CMP後洗淨中的Cu之腐蝕係受到重視,若為酸性洗淨液,則表
面之粗糙度會增大係已成為問題。在另一方面,鹼性洗淨液則會對伴隨著配線微細化所導入的低介電常數(low-dielectric-constant)(low-k)層間絕緣膜材料造成損傷。
在專利文獻4,揭述一種含有膦酸化合物及環氧乙烷化合物及/或環氧丙烷化合物等之發泡性少的洗淨劑組成物;在專利文獻5,揭述一種含有羧酸、含胺化合物及膦酸的CMP後之半導體表面之清淨化溶液;在專利文獻6,揭述一種含有鹼成分與吸附防止劑之半導體晶圓處理液;在專利文獻7至9,揭述一種含有界面活性劑或螯合劑之半導體基板或磁碟等之洗淨用的各種洗淨組成物。但是,任一者並未針對具有銅配線的基板方面加以研討。
作為用於洗淨具有Cu配線的基板之組成物,在專利文獻10,揭述一種具有磺酸系高分子之摻合物;在專利文獻11,揭述一種含有多孔性介電質、腐蝕抑制性溶劑化合物、有機共溶劑、金屬螯合劑及水之洗淨組成物;在專利文獻12,揭述一種含有螯合劑或其鹽、鹼金屬氫氧化物及水之洗淨液。但是,任一種組成物皆未針對low-k材料之損傷加以研討,而且也未針對移除微粒子及金屬雜質兩者加以研討。在專利文獻13,揭述一種含有使得low-k材料的表面成為惰性的去活化劑之洗淨液,但是卻需要移除由於該去活化劑所形成的去活化膜之步驟。
如上所述,一種金屬雜質與顆粒之移除性(removing property)優異、而且並無銅之腐蝕及對於低介電常數層間絕緣膜(interlayer insulating film)的損傷之問題的洗淨液,
直到目前為止仍然不知道。
(專利文獻1)日本特開平第10-072594號公報
(專利文獻2)日本特開平第11-131093號公報
(專利文獻3)日本特開第2001-7071號公報
(專利文獻4)日本特開平第11-116984號公報
(專利文獻5)日本特表第2003-510840號公報
(專利文獻6)日本特開平第06-041773號公報
(專利文獻7)日本特開第2009-084568號公報
(專利文獻8)日本特開第2009-087523號公報
(專利文獻9)日本特開第2010-163608號公報
(專利文獻10)日本特開第2011-040722號公報
(專利文獻11)日本特開第2009-081445號公報
(專利文獻12)國際公開第2004/042811號
(專利文獻13)日本特表第2008-543060號
因此,本發明之目的係在半導體元件等電子裝置之製造步驟中,在經施加研磨處理、蝕刻處理、化學機械研磨(CMP:Chemical Mechanical Polishing)處理等之金屬材料表面,特別是具有銅配線的基板之洗淨方面,提供一種洗淨液組成物,其係對於金屬雜質及微粒子之移除性優異、對於Cu等之金屬材料無腐蝕而可進行洗淨者。
本發明人等為解決上述技術問題而在專心研究時,發見一種包含一種或兩種以上的不含金屬之鹼性化合物、與一種或兩種以上的膦酸系螯合劑(phosphonic acid-based chelating agent),且氫離子濃度(pH值)為8至10之洗淨液組成物,係可使得對於金屬雜質與微粒子之高移除性並存、對於Cu等之金屬材料無腐蝕,且藉由薄氧化膜來保護洗淨後之Cu表面,即可更進一步抑制氧化,並且更進一步推展研究的結果,終於達成本發明。
亦即,本發明係關於下列各項。
(1)一種洗淨液組成物,其係用於洗淨具有銅配線之半導體基板,且包含一種或兩種以上的不含金屬之鹼性化合物、與一種或兩種以上的膦酸系螯合劑,且氫離子濃度(pH值)為8至10。
(2)如上述第(1)項之洗淨液組成物,其中具有銅配線之半導體基板為經化學機械研磨(CMP)後之基板。
(3)如上述第(1)或(2)項之洗淨液組成物,其中不含金屬之鹼性化合物為第四級銨化合物或直鏈脂肪族胺。
(4)如上述第(1)至(3)項中的任一項之洗淨液組成物,其中不含過氧化氫水溶液。
(5)如上述第(1)至(4)項中的任一項之洗淨液組成物,其中不含抗壞血酸(ascorbic acid)。
(6)如上述第(1)至(5)項中的任一項之洗淨液組成物,其中不含羧酸系螯合劑(carboxylic acid-based chelating
agent)。
(7)如上述第(1)至(6)項中的任一項之洗淨液組成物,其中不含金屬之鹼性化合物為氫氧化四甲基銨除外之第四級銨化合物或烷醇胺。
(8)如上述第(1)至(7)項中的任一項之洗淨液組成物,其中膦酸系螯合劑為N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)(EDTPO)、甘胺酸-N,N-雙(亞甲基膦酸)(草二甘膦(glyphosine))、氮基參(亞甲基膦酸)[nitrilotris(methylene phosphonic acid)](NTMP)或此等之鹽。
(9)如上述第(1)至(8)項中的任一項之洗淨液組成物,其中更進一步含有一種或兩種以上的陰離子型或非離子型界面活性劑。
(10)一種濃縮液,其係為稀釋成10倍至1000倍而作成為上述第(1)至(9)項中任一項之洗淨液組成物者。
(11)如上述第(10)項之濃縮液,其係使用含水之稀釋液加以稀釋。
(12)如上述第(10)或(11)項之濃縮液,其pH值為10至12。
(13)一種洗淨具有銅配線之半導體基板之方法,其係使用如上述第(1)至(9)項中任一項之洗淨液組成物。
本發明之洗淨液組成物,係在半導體元件等電子裝置之製造步驟中,在經施加研磨處理、蝕刻處理、化學機械
研磨(CMP)處理等之金屬材料表面之洗淨方面,對於金屬雜質及微粒子之移除性優異、對於Cu等之金屬材料無腐蝕,且藉由薄氧化膜層來保護洗淨後之Cu表面,即可更進一步抑制氧化。
第1圖是表示PSL(聚苯乙烯乳膠)粒子表面、SiO2表面、SiN4表面及裸矽(Bare Si)表面之ζ-電位(zeta-potential)之pH值依存性圖(THE CHEMICAL TIMES 2005,No.4,p6)。
第2圖是表示Cu-水系之波貝克斯圖(Pourbaix diagram:電位與pH值關係曲線)。
第3圖是表示將實施例69之經處理後的塗佈型SiOC系低介電常數(low-k)材料加以成膜的矽晶圓之紅外線吸收(IR)光譜圖。
第4圖是表示將實施例70之經處理後的塗佈型SiOC系低介電常數(low-k)材料加以成膜的矽晶圓之紅外線吸收(IR)光譜圖。
第5圖是表示將比較例31之經處理後的塗佈型SiOC系低介電常數(low-k)材料加以成膜的矽晶圓之紅外線吸收(IR)光譜圖。
在本發明之一模式中,提供一種洗淨液組成物,其係用於洗淨具有銅配線之半導體基板,且包含一種或兩種以上的不含金屬之鹼性化合物、與一種或兩種以上的膦酸系螯合劑,且氫離子濃度(pH值)為8至10。
本發明之洗淨液組成物適用於具有銅配線之半導體基板,特別是適用於經化學機械研磨(CMP)後之基板。經CMP後之基板表面有可能除了基板表面之各種配線及阻障性金屬材料(barrier metal material)(Cu、Ti系化合物、Ta系化合物、Ru等)及絕緣膜材料(SiO2、low-k材料)以外,存在著包含於漿液中之微粒子或金屬雜質。微粒子主要為氧化鋁、二氧化矽及氧化鈰,金屬雜質可列舉:在研磨中溶解於漿液中而再附著的Cu、在漿液中之源自氧化劑的Fe、或包含於漿液中之Cu防蝕劑(anti-corrosive agent)與Cu進行反應的Cu有機金屬錯合物等。
在本發明中,所謂的low-k材料係使用於層間絕緣膜等之具有低介電常數的材料,例如可列舉(但是並不受限於此等):SiOC系材料、多孔質矽、含矽有機高分子、芳香族芳基醚化合物、氟碳化合物等,目前主要是使用多孔質矽及含矽有機高分子。具體而言,可列舉Black Diamond(應用材料公司(Applied Materials,Inc.)製)、Aurora(ASM International公司製)、CERAMATE NCS(日揮觸媒化成公司(JGC Catalysts and Chemicals Co.,Ltd.)製)等。
使用於本發明之鹼性化合物,只要其為可調整成預定的pH值之化合物時,則並無特殊的限制,但是只要是使
用於電子裝置,則較佳為不含金屬之鹼性化合物。若在組成物中含有金屬時,則將發生逆污染(reverse pollution)及對於基板內部之擴散,結果造成由於層間絕緣膜之絕緣不良引起之漏電流(leak current)增大或半導體特性劣化的原因。
鹼性化合物之實例可列舉:第四級銨化合物、胺,但是並不受限於此等。第四級銨化合物可列舉:氫氧化四甲基銨(TMAH)、氫氧化三甲基-2-羥基乙基銨(膽鹼(choline))、氫氧化四乙基銨、氫氧化四丙基銨、氫氧化四丁基銨、氫氧化三甲基苯基銨、氫氧化苯甲基三甲基銨等。此等中,較佳為膽鹼、氫氧化四乙基銨。
胺可列舉:第一級、第二級或第三級脂肪族胺等之有機胺、脂環式胺、芳香族胺及雜環式胺等,但是並不受限於此等。第一級脂肪族胺之實例可列舉(但是並不受限於此等):一乙醇胺、伸乙基二胺、2-(2-胺基乙氧基乙醇)及2-(2-胺基乙基胺基)乙醇。
第二級脂肪族胺之實例可列舉(但是並不受限於此等):二乙醇胺、N-甲基胺基乙醇、二丙基胺及2-乙基胺基乙醇。第三級脂肪族胺之實例可列舉(但是並不受限於此等):三乙醇胺、二甲基胺基乙醇及乙基二乙醇胺。
脂環式胺之實例可列舉(但是並不受限於此等):環戊胺、環己胺。
芳香族胺之實例可列舉(但是並不受限於此等):苯胺。
雜環式胺之實例可列舉(但是並不受限於此等):哌啶、N-甲基哌啶、N-胺基乙基哌啶、哌嗪、N-甲基哌嗪、N,N’-二甲基哌嗪、N-羥基乙基哌嗪、N-甲基-N’-羥基乙基哌嗪、N-胺基乙基哌嗪、N,N’-二甲基胺基乙基甲基哌嗪、嗎啉、N-甲基嗎啉、N-羥基乙基嗎啉、N-胺基乙基嗎啉。
鹼性化合物有可能由於其分子結構而對於low-k材料造成損傷的情況。特別是在使用第一級胺時,經常會對於low-k材料造成損傷,因此鹼性化合物更佳為第二級胺、第三級胺或第四級銨化合物。此外,在胺中,在結構內具有環狀結構之脂環式胺、環狀胺及雜環式胺之一部份的化合物也有會強固地吸附於Cu表面而成為異物的顧慮,因此更佳為烷醇胺等之直鏈脂肪族胺。並且,第一級胺或第二級胺之一部份的化合物,由於與Cu之錯合物穩定度常數(complex stability constant)高、會形成水溶性錯合物,因此有溶解Cu的傾向。因此,胺較佳為第二級脂肪族胺之二乙醇胺、第三級脂肪族胺之三乙醇胺,特佳為三乙醇胺。
並且,鹼性化合物之含量,為調整由於鹼性化合物的種類或其他成分的種類、含量而變動的pH值之作用,並無特殊的限制,在使用時之含量較佳為0.5至50 mmol/L,特佳為0.5至30 mmol/L。若鹼性化合物之含量太低時,則有可能由於微小的組成變動或雜質混入而導致pH值變化,而若鹼性化合物之含量太高時,則有對於low-k材料之
損傷增大的顧慮。
在本發明之一模式中,係不含氫氧化四甲基銨(TMAH)。氫氧化四甲基銨係在第四級銨化合物中毒性高,近年來由於考慮及對於製造步驟上作業員的影響之製造廠商則有對此敬而遠之的傾向,儘可能以不含者為較佳。
在本發明中,洗淨液組成物之pH值較佳為8至10。本發明之洗淨液之顯著的特徵之一,係即使在不使用界面活性劑也可移除微粒子。此係由於在鹼性區域,SiO2或TiO2等之氧化物的表面之帶電會變化(參閱第1圖),利用此點而將基板與微粒子之帶電同時加以控制成負,並以靜電排斥力(electrostatic repulsion force)的作用即可拉開基板與微粒子的緣故。然而,先前的鹼性洗淨液係無法充分地移除基板表面之金屬雜質。此係可認為在鹼性區域,金屬雜質係與氫氧離子(hydroxide ion)(OH-)進行反應、並成為氫氧化物或羥基錯合物而吸附在基板表面而不溶解於液中的緣故。
當使得pH值降低時,雖然可提高金屬雜質之移除性,但是微粒子之移除性卻降低,同時對於施加在基板表面的Cu之損傷則有增大的傾向。此外,相反地,當使得pH值上升時,雖然可提高微粒子之移除性,但是金屬雜質之移除性卻降低,同時對於在鹼性區域是脆弱的SiOC系low-k材料之損傷則有增大的傾向。若根據本發明,藉由將pH值設定為8至10,則可移除微粒子及金屬雜質兩者,且不致於對於Cu及low-k材料兩者造成損傷來進行洗淨
。
此外,若為在此pH值區域時,則在經Cu-CMP後之洗淨中,可在洗淨後之Cu表面形成薄Cu2O層,可抑制放置於大氣中時之急遽的表面氧化。Cu係在水系中,若為在酸性區域之pH值,則呈Cu2+或Cu0的狀態,因此在活性為高的狀態而易於急遽地氧化,但是在鹼性區域,則呈CuO或Cu2O的狀態(參閱第2圖)。因此,在酸性區域之pH值時,在經CMP後之Cu表面係進行不均勻的氧化反應,使得不均勻的氧化膜覆蓋表面、同時增大表面之粗糙度。與此相對,在pH值為8至10時,由於可形成薄Cu2O層,該層則作為保護膜而發揮作用、抑制急劇的氧化、使得平坦性優異的洗淨得以進行。
本發明之洗淨液組成物係包含膦酸系螯合劑。為賦予金屬雜質移除性,雖然螯合劑之添加為有效,但是由於功效係根據溶液之pH值或移除對象的金屬種類而不同,不易選擇適用於用途之螯合劑。一般使用的NTA、EDTA及DPTA等之羧酸系螯合劑、草酸、乳酸等之脂肪族羧酸及其鹽、苯甲酸等之芳香族羧酸及其鹽、羥基羧酸及其鹽、磺酸系螯合劑、及胺基酸等,若為在此pH值區域,則無法充分發揮錯化形成能(complexation ability),因此金屬雜質移除性為低。與此相對,膦酸系螯合劑在pH值8至10之區域,金屬雜質之移除性優異,特別是可對於Fe與Zn兩者可有效地發生作用。
膦酸系螯合劑並無特殊的限制,可列舉:甲基二膦酸
、胺基三(亞甲基膦酸)、1-羥基亞乙基-1,1-二膦酸、氮基參亞甲基膦酸(NTMP)、伸乙基二胺肆(亞甲基膦酸)(EDTPO)、六亞甲基二胺四(亞甲基膦酸)、伸丙基二胺四(亞甲基膦酸)、二伸乙基三胺五(亞甲基膦酸)、三伸乙基四胺六(亞甲基膦酸)、三胺基三乙基胺六(亞甲基膦酸)、反式-1,2-環己烷二胺四(亞甲基膦酸)、乙二醇醚二胺四(亞甲基膦酸)及四伸乙基五胺七(亞甲基膦酸)、甘胺酸-N,N-雙(亞甲基膦酸)(草二甘膦)。此等中,較佳為EDTPO、草二甘膦及NTMP。膦酸系螯合劑係可單獨或相互組合使用。
膦酸系螯合劑之含量並無特殊的限制,使用時之含量較佳為0.1至10 mmol/L,特佳為0.5至5 mmol/L。在膦酸系螯合劑之含量為太低的情況,則金屬雜質移除能力不足,在膦酸系螯合劑之含量為太高的情況,則對於施加在基板表面的金屬材料之損傷增大,且有發生表面變粗糙的顧慮。
本發明之洗淨液組成物係不需要過氧化氫。當過氧化氫共存時,則不僅會造成Cu等之金屬材料的腐蝕,也會產生對於由過氧化氫之分解所造成組成物之穩定性的顧慮。此外,本發明之洗淨液組成物係不需要作為還原劑而作用的抗壞血酸。其理由為本發明之洗淨液組成物由於選擇適當的成分及含量、pH值範圍,在洗淨時,則可抑制Cu之腐蝕,同時可在經處理後的Cu表面形成薄氧化膜。因此,不需要提高洗淨液之還原性。因此,可解決由於抗壞
血酸之共存在而造成金屬雜質移除性降低、或由於抗壞血酸之分解所造成的組成物之不穩定性。
在本發明之洗淨液組成物之一模式,較佳為不含對於Cu表面反應性高、含有N及/或S之雜環式化合物,例如三唑、噻唑、四唑、咪唑等、以及硫醇、氮嗪等。如此的化合物既會強固地吸附在Cu表面、又由於照原狀時則將構成電特性劣化原因,因此更進一步需要移除此等之步驟,特別是苯并三唑係生物分解性低、對於使用微生物分解的廢液處理之負荷大而不適宜。
本發明之洗淨液組成物也可為提高微粒子之移除性而添加界面活性劑。界面活性劑的種類係根據欲移除的微粒子或基板而適當地選擇,但是較佳為水溶性之陰離子型或非離子型。此等中,非離子型由於結構中之環氧乙烷或環氧丙烷之數量或比率,可能會增大對於low-k材料之侵蝕,必須要小心選擇。
本發明之洗淨液組成物由於大部份係以水所構成,當在電子裝置之製造生產線上設置稀釋混合裝置時,則可作為濃縮品來供應,並在即將使用前以含水之稀釋液(此係包括僅以超純水作為稀釋液)加以稀釋而使用,如此則有助於減少輸送成本或在輸送時之二氧化碳氣體、或減少電子裝置製造廠商的製造成本。
本發明之濃縮液的濃縮倍率係可根據所欲構成的組成而適當地決定,大約為10倍以上,較佳為10至1000倍,更佳為50至200倍。
在本發明之洗淨方法之一模式,係一種洗淨具有銅配線之半導體基板之方法,其係使用前述包含一種或兩種以上的不含金屬之鹼性化合物、與一種或兩種以上的膦酸系螯合劑,且氫離子濃度(pH值)為8至10之洗淨液組成物。
其次,就本發明之洗淨液組成物,以實施例及比較例更詳細地說明本發明,但是本發明並不受限於此等實施例者。
將矽晶圓以體積比為氨水(29重量%)-過氧化氫水溶液(30重量%)-水混合液(體積比=1:1:6)加以洗淨後,藉由旋轉塗佈法,以鈣(Ca)、鐵(Fe)、鎳(Ni)、銅(Cu)、鋅(Zn)加以污染成表面濃度為1012 atoms/cm2。將受到污染的晶圓在各洗淨液中,在25℃、無攪拌下浸漬3分鐘後,取出晶圓並以超純水進行3分鐘之流水洗滌處理,加以乾燥後,以全反射螢光X-射線分析裝置(Total-reflection X-ray Fluorescence Spectrometer)測定晶圓表面之金屬濃度、並評估金屬雜質移除性。洗淨液之組成及結果展示於表1。
附註:
EDTPO:N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)
NTMP:氮基參(亞甲基膦酸)
TEA:三乙醇胺
TMAH:氫氧化四甲基銨
NTA:氮基三醋酸
EDTA:伸乙基二胺四醋酸
DPTA:二伸乙基三胺五醋酸
D.L.:偵測極限以下(少於109 atoms/cm2)
如表1所示,若為未添加螯合劑之鹼性化合物水溶液,則移除性低。此外,在添加NTA、EDTA及DPTA等之羧酸系螯合劑、草酸、乳酸等之脂肪族羧酸等、以及還原劑之抗壞血酸的情況,雖然對於某些金屬之移除性有改善,但是無法提高全部五種金屬之移除性。在另一方面,在添加膦酸系螯合劑的情況,則對於全部五種之金屬有功效,且可達成對CMP後洗淨後所要求的清淨度。
將經在表面以電解鍍敷法(electrolytic plating method)成膜Cu的8英寸矽晶圓,使用CMP裝置與CMP漿液(二氧化矽漿液(φ 35 nm)進行研磨30秒鐘。然後,使用洗淨裝置,以各洗淨液在室溫下進行以刷子刷洗潔淨30秒鐘、以超純水洗滌處理30秒鐘,並進行旋轉乾燥。經洗淨後之晶圓,使用表面檢查裝置測定表面之微粒子數,以評估微粒子移除性。洗淨液之組成及結果展示於表2。
附註:
EDTPO:N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)
NTMP:氮基參(亞甲基膦酸)
TEA:三乙醇胺
TMAH:氫氧化四甲基銨
MMP:1-(2-二甲基胺基乙基)-4-甲基哌嗪
CyDTA:反式-1,2-環己烷二胺四醋酸
EDTA.2NH3:伸乙基二胺四醋酸二銨
NIKKOL CMT-30:椰子油脂肪酸甲基牛磺酸、陰離子型界面活性劑
NIKKOL肌胺酸鹽LN:月桂醯基肌胺酸、陰離子系界面活性劑
DKS-NL dash408:非離子型界面活性劑
如表2所示,若為未添加螯合劑之鹼性化合物水溶液,則移除性低,且有許多微粒子殘留於Cu表面上。此外,即使在添加EDTA、CyDTA等之羧酸系螯合劑、草酸等之脂肪族羧酸、以及還原劑之抗壞血酸的情況,微粒子移除性並未獲得改善。在另一方面,在添加膦酸系螯合劑的情況,微粒子移除性係急劇地獲得改善。
將經在表面以濺鍍法成膜Cu的8英寸矽晶圓,切割成1.0×1.5 cm2,並在裝入各洗淨液48毫升的聚乙烯容器中,在30℃、無攪拌下浸漬7分鐘後,以ICP-MS(感應耦合電漿質譜分析儀:Inductively Coupled Plasma-Mass Spectrometer)測定經取出晶圓的洗淨液中之Cu濃度,並由晶圓之Cu表面積與洗淨液中之Cu濃度計算出洗淨液之Cu蝕刻速率(E.R.)。各洗淨液係將調製成預定濃度的螯合劑水溶液之pH值以pH計進行測定,並藉由逐滴加入鹼性化合物,調整成預定的pH值。洗淨液之組成及結果展示於表3。
附註:
EDTPO:N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)
NTMP:氮基參(亞甲基膦酸)
TEA:三乙醇胺
TMAH:氫氧化四甲基銨
MMP:1-(2-二甲基胺基乙基)-4-甲基哌嗪
CyDTA:反式-1,2-環己烷二胺四醋酸
如表3所示,若pH值為低於8時,則Cu之E.R.高,但是若pH值為8至10時,則Cu之E.R.低,且即使為含有螯合劑而金屬雜質移除性為高的洗淨液,對於基板表面之金屬材料的損傷卻為小。
將經在表面以電解鍍敷法成膜Cu的8英寸矽晶圓,在草酸(1 wt%)水溶液中,在25℃、無攪拌下浸漬處理1分鐘、以超純水洗滌、乾燥後,在洗淨液中,在25℃、無攪拌下浸漬處理30分鐘後、以超純水洗滌、乾燥後,使用AFM(原子力顯微鏡:Atomic Force Microscope)測定Cu之表面粗糙度(平均面粗糙度:Ra)。洗淨液之組成及結果展示於表4。
附註:
EDTPO:N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)
NTMP:氮基參(亞甲基膦酸)
TEA:三乙醇胺
如表4所示,與表3之結果相同地,經添加膦酸系螯合劑之鹼性化合物水溶液,即使在長時間浸漬的情況,Cu之表面粗糙度也不會大幅地增大,且與通常作為CMP後洗淨液使用之草酸水溶液相比較,對於Cu之損傷是顯著地低。
將經成膜塗佈型SiOC系低介電常數(low-k)材料(介電常數:2.2)之矽晶圓,在各洗淨液中,在25℃、無攪拌下浸漬處理30分鐘、以超純水洗滌、乾燥後,使用FT-IR(傅立葉變換紅外線分光分析裝置:Fourier Transform Infrared Spectrophotometer)測定紅外線吸收(IR)光譜,並比較1150 cm-1附近之源於Si-O鍵之吸收。
洗淨液之組成及評估結果展示於表5,IR光譜展示於第3至5圖。
附註:
NTMP:氮基參(亞甲基膦酸)
TEA:三乙醇胺
TMAH:氫氧化四甲基銨
如表5、第3至5圖所示,pH值為11之TMAH水溶液係在處理前後low-k材料之源自Si-O鍵之吸收則大幅地
變化、發生low-k材料之結構變化,但是若為pH值為在8至10之範圍內的水溶液,則無如此的變化,因此對於low-k材料之損傷為小。
Claims (12)
- 一種洗淨液組成物,其用於洗淨具有銅配線之半導體基板,且包含0.5至50mmol/L的一種或兩種以上的不含金屬之鹼性化合物、與0.1至10mmol/L的一種或兩種以上的膦酸系螯合劑,且氫離子濃度(pH值)為8至10,並且不含羧酸系螯合劑。
- 如請求項1所述之洗淨液組成物,其中,具有銅配線之半導體基板,是經化學機械研磨(CMP)後之基板。
- 如請求項1或請求項2所述之洗淨液組成物,其中,不含金屬之鹼性化合物,是第四級銨化合物或直鏈脂肪族胺。
- 如請求項1或請求項2所述之洗淨液組成物,其中,不含過氧化氫水溶液。
- 如請求項1或請求項2所述之洗淨液組成物,其中,不含抗壞血酸。
- 如請求項1或請求項2所述之洗淨液組成物,其中,不含金屬之鹼性化合物是除了氫氧化四甲基銨以外之第四級銨化合物或烷醇胺。
- 如請求項1或請求項2所述之洗淨液組成物,其中,膦酸系螯合劑是N,N,N’,N’-伸乙基二胺肆(亞甲基膦酸)(EDTPO)、甘胺酸-N,N-雙(亞甲基膦酸)(草二甘膦)、氮基參(亞甲基膦酸)(NTMP)或此等之鹽。
- 如請求項1或請求項2所述之洗淨液組成物,其中,更進一步含有一種或兩種以上的陰離子型或非離子型界面 活性劑。
- 一種濃縮液,其係為稀釋成10倍至1000倍而作成為如請求項1至8中的任一項所述之洗淨液組成物。
- 如請求項9所述之濃縮液,其係使用含水之稀釋液加以稀釋。
- 如請求項9或請求項10所述之濃縮液,其pH值為10至12。
- 一種洗淨具有銅配線之半導體基板之方法,其使用如請求項1至8中的任一項所述之洗淨液組成物。
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