CN1225529C - 电子材料用基板洗净液 - Google Patents
电子材料用基板洗净液 Download PDFInfo
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- CN1225529C CN1225529C CNB001060465A CN00106046A CN1225529C CN 1225529 C CN1225529 C CN 1225529C CN B001060465 A CNB001060465 A CN B001060465A CN 00106046 A CN00106046 A CN 00106046A CN 1225529 C CN1225529 C CN 1225529C
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- 239000012776 electronic material Substances 0.000 title claims abstract description 13
- 238000004140 cleaning Methods 0.000 title abstract description 16
- 239000007788 liquid Substances 0.000 title description 3
- 239000000758 substrate Substances 0.000 claims abstract description 34
- -1 organic acid compound Chemical class 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 239000004094 surface-active agent Substances 0.000 claims abstract description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 60
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 235000006408 oxalic acid Nutrition 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000013543 active substance Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 150000003863 ammonium salts Chemical class 0.000 claims description 7
- 239000003352 sequestering agent Substances 0.000 claims description 7
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- HCPOCMMGKBZWSJ-UHFFFAOYSA-N ethyl 3-hydrazinyl-3-oxopropanoate Chemical compound CCOC(=O)CC(=O)NN HCPOCMMGKBZWSJ-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 231100000719 pollutant Toxicity 0.000 claims description 3
- 229940095064 tartrate Drugs 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 125000002270 phosphoric acid ester group Chemical group 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 24
- 239000007769 metal material Substances 0.000 abstract description 6
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 5
- XMRUJYGYYCLRGJ-UHFFFAOYSA-N azanium;2-[2-[2-[2-(4-nonylphenoxy)ethoxy]ethoxy]ethoxy]ethyl sulfate Chemical compound [NH4+].CCCCCCCCCC1=CC=C(OCCOCCOCCOCCOS([O-])(=O)=O)C=C1 XMRUJYGYYCLRGJ-UHFFFAOYSA-N 0.000 description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006061 abrasive grain Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 102200115452 rs137852659 Human genes 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 241000282320 Panthera leo Species 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 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 1
- FOGYNLXERPKEGN-UHFFFAOYSA-N 3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfopropyl)phenoxy]propane-1-sulfonic acid Chemical compound COC1=CC=CC(CC(CS(O)(=O)=O)OC=2C(=CC(CCCS(O)(=O)=O)=CC=2)OC)=C1O FOGYNLXERPKEGN-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 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
- 229910021529 ammonia Inorganic materials 0.000 description 1
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- FQTCUKQMGGJRCU-UHFFFAOYSA-N n,n-diacetylacetamide Chemical compound CC(=O)N(C(C)=O)C(C)=O FQTCUKQMGGJRCU-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000012797 qualification Methods 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
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- 238000009736 wetting Methods 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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/26—Cleaning or polishing of the conductive pattern
-
- 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
-
- 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
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02063—Cleaning during device manufacture during, before or after processing of insulating layers the processing being the formation of vias or contact holes
-
- 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
- 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
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/07—Electric details
- H05K2201/0753—Insulation
- H05K2201/0761—Insulation resistance, e.g. of the surface of the PCB between the conductors
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/12—Using specific substances
- H05K2203/122—Organic non-polymeric compounds, e.g. oil, wax, thiol
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Emergency Medicine (AREA)
- Health & Medical Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Detergent Compositions (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
本发明提供不腐蚀金属、能够高效率地同时去除基板表面的金属杂质和颗粒的洗净液。该洗净电子材料用基板的洗净液含有分散剂和表面活性剂中的至少一种及有机酸化合物,且该洗净液不含有碱;所述有机酸化合物是从草酸、丙二酸、苹果酸、酒石酸、柠檬酸及它们的铵盐组成的组中选择的1种或2种以上,且所述有机酸化合物的量是所述洗净液的总量的0.01~30重量%;所述表面活性剂是阴离子型或者非离子型表面活性剂;所述分散剂是磷酸酯,且所述分散剂和表面活性剂的量是所述洗净液的总量的0.0001~10重量%。
Description
技术领域
本发明涉及洗净电子材料用基板的洗净液,特别是涉及在半导体制造过程中,用于去除吸附在具有金属配线的基板上的金属杂质和颗粒污染物的洗净液。
背景技术
伴随集成电路(IC)的高集成化,微量的杂质对器件的性能、合格率造成大的影响,因此要求严格地控制污染物。即,要求严格地控制基板的金属杂质浓度或颗粒,为此在半导体制造的各过程中使用各种洗净液。
一般情况下,作为洗净半导体用基板等电子材料用基板的洗净液,有硫酸一过氧化氢水、氨-过氧化氢水-水(SC-1)、盐酸-过氧化氢水-水(SC-2)、稀氢氟酸,根据目的可单独使用或者组合使用各洗净液。
最近,绝缘膜的平坦化、连接孔的形成、波形花纹(ダマシン)配线等中的化学机械研磨(以下称为“CMP”)技术已引入半导体制造过程中。CMP的技术是一边供给研磨剂颗粒和化学药品的混合物浆液,一边将基片压接在称为磨光轮的研磨布上,通过旋转并利用化学作用和物理作用来研磨绝缘膜或金属材料,由此进行平坦化。
在金属材料(W或Cu)的CMP中使用的浆液,是组合使用研磨颗粒(氧化铝、二氧化硅、二氧化锰、氧化铈、氧化锆等)和氧化剂(硝酸铁、过氧化氢等)。因此,CMP工程后的基板表面被来自浆液的金属杂质或研磨颗粒、进而被研磨屑污染。特别是在氧化剂中使用硝酸铁的情况下,被高浓度的Fe污染,不仅使基板本身的电特性劣化,而且也有污染生产线的2次污染的危险。
因此,在后续的工程之前必须迅速地去除CMP过程中吸附的金属杂质和颗粒。
在层间绝缘膜的CMP中,使用稀氢氟酸去除金属杂质,并使用氨水去除颗粒。
但是,稀氢氟酸腐蚀金属材料,因此在W或Cu的CMP后的洗净中不能使用。
作为不腐蚀金属材料的洗净液,已报道了柠檬酸水溶液(月刊七ミコンダクタ-ヮ-ルド,第92页,No.3,1997)。另外,还有人提出通过组合柠檬酸等有机酸和配位剂来提高金属杂质的洗净能力(特开平10-72594)。但是,这些有机酸洗净液的金属杂质去除能力不充分,并且也没有对颗粒的洗净力。
另一方面,在颗粒的去除中使用的氨水也腐蚀Cu,因此不能作为Cu-CMP后的洗净液使用。进而,在洗净中使用2种洗净液,在使过程复杂的同时,还具有药液的使用量增大的问题。因而,从成本或环境问题方面考虑,也需要不腐蚀金属材料、能够去除金属杂质和颗粒的新洗净技术。
从以上的事实看,强烈期望在洗净电子材料用基板时不经过复杂的工序、能够简便且高效率地进行洗净的洗净剂。
发明内容
即,本发明的目的在于提供不腐蚀金属、能够高效率地同时去除基板表面的金属杂质、颗粒的电子材料用基板洗净液。
在本发明中,所谓电子材料用基板是指半导体用基片、色滤光片、薄膜应用电子器件用基板(液晶、等离子体、EL等平板显示,光·磁盘、CCD等)。
本发明人为解决上述问题反复进行了深入的研究,结果惊奇地发现,在草酸等有机酸的水溶液中添加分散剂或表面活性剂,能不腐蚀金属,而且能够同时且极高效率地洗净吸附的金属杂质和颗粒,从而实现了本发明。
即,本发明涉及洗净电子材料用基板的洗净液,该洗净液含有分散剂和表面活性剂中的至少一种及有机酸化合物,且该洗净液不含有碱;所述有机酸化合物是从草酸、丙二酸、苹果酸、酒石酸、柠檬酸及它们的铵盐组成的组中选择的1种或2种以上,且所述有机酸化合物的量是所述洗净液的总量的0.01~30重量%;所述表面活性剂是阴离子型或者非离子型表面活性剂;所述分散剂是磷酸酯,且所述分散剂和表面活性剂的量是所述洗净液的总量的0.0001~10重量%。
另外,本发明涉及进而含有螯合剂的上述洗净液。
本发明还涉及进而含有水溶性醇的上述洗净液。
本发明也涉及能够同时去除吸附在基板上的金属杂质和颗粒污染物的上述洗净液。
本发明进而涉及电子材料用基板是施加金属配线后的基板的上述洗净液。
进而本发明涉及在化学机械研磨后使用的上述洗净液。
虽然尚未清楚按照本发明的洗净液的洗净机制,但可如下进行推测。通常情况下,在水溶液中颗粒保持称为ζ电位的电荷,同样半导体基板也保持。如果半导体基板和颗粒的电荷是不同符号的,则在基板和颗粒间产生引力作用,颗粒吸附在基板上。如果是相同符号的,则产生斥力作用,颗粒不吸附在基板上。也就是说,控制ζ电位,由此可抑制颗粒的吸附,或者能够去除吸附的颗粒。pH是重要的控制ζ电位的因素。在pH 8以上的碱性时,大部分的物质保持负电荷,因此抑制颗粒的吸附,容易进行脱离。以往,在颗粒的去除中使用像氨那样的碱,正是根据这样的理由。
另外,可考虑通过添加表面活性剂或分散剂来控制ζ电位。在本发明中利用分散剂或表面活性剂的方法,不大幅度地改变液性,因此作为解决问题的手段是最好的方法。
具体实施方式
在本发明中使用的有机酸化合物是甲酸、乙酸、丙酸等脂肪族一元羧酸或草酸、丙二酸、琥珀酸等二元羧酸类,酒石酸、苹果酸、柠檬酸等羟基多元羧酸类,及其铵盐。特别是多元羧酸类,其金属杂质的去除能力高,作为在本发明中使用的有机酸化合物是最合适的。
洗净液中的有机酸化合物的浓度是0.01~30重量%,最好是0.03~10重量%。在有机酸化合物的浓度过低时,不能充分地发挥洗净效果,而即使达到过高的浓度,也不能期待与浓度相称的效果。并且在不析出结晶的范围,还要考虑有机酸的溶解度而适当确定该浓度。
只要是能够达到本发明期望的目的,可以使用任何的分散剂、表面活性剂作为本发明中的分散剂、表面活性剂。作为分散剂,典型的有偏磷酸、焦磷酸等缩合磷酸或肌醇六磷酸、二(聚氧乙烯)烷基醚磷酸、三(聚氧乙烯)烷基醚磷酸等磷酸酯类,例如作为二(聚氧乙烯)烷基醚磷酸,以NIKKOL DDP-8、NIKKOL DDP-10(日光化学品株式会社)等商品名市售,作为三(聚氧乙烯)烷基醚磷酸,以NIKKOL TDP-8、NIKKOL TDP-10(日光化学品株式会社)等商品名市售。对于表面活性剂,典型的是使用阴离子型表面活性剂或者非离子型表面活性剂,特别是带有作为强亲水性基团的磺酸基或羧酸基的阴离子型表面活性剂,或者环氧乙烷链长而且亲水性高的非离子型表面活性剂,这可达到良好的效果。具体地可举出聚氧乙烯壬苯基醚型或脱水山梨糖醇型的非离子表面活性剂(例如以ェマルグンMS-110、レォド-ルス-バ-TW-0120(花王株式会社)等商品名市售者),磺酸或者磺酸盐类型的阴离子型表面活性剂(例如商品名Newcol 210、Newcol 560SF、Newcol707SF(日本乳化剂株式会社)),或高分子型阴离子表面活性剂。作为高分子型阴离子表面活性剂,例如可举出:(1)萘磺酸和甲醛的缩合物及其盐,(2)丙烯酸或甲基丙烯酸等羧酸聚合物及其盐,(3)木质素磺酸及其盐。
作为(1),有以デモ-ルN、デモ-ルAS(以上,花王株式会社)、ボリス夕-NP-100(日本油脂株式会社)、ルノックス1000、1000C、1500A(以上,东邦化学工业株式会社)、ィォネットD-2、三洋レベロンPHL(以上,三洋化成株式会社)、ロ-マPWA-40(サンノグコ株式会社)等商品名市售者,以铵盐或者游离酸形式且不含金属杂质的デモ-ルAS或ロ-マPWA-40等是特别合适的。作为(2),有以デモ-ルEP、ボィズ520、ボィズ521、ボィズ523A(以上,花王株式会社)、ボリスタ-A-1060、ボリスタ-OM、ボリスタ-OMA(以上,日本油脂株式会社)、ボリティ530、ボリティ540、ボリティ550(以上,狮王株式会社)、キヤリボンB、キヤリボンL-400、ェレミノルMBN-1、サンスバ-ルPS-2、サンスバ-ルPS-8、サンスバ-ルPDN-173、サンスバ-ルPS-30、トキサノンGR-31A、トキサノンGR-30、トキサノンNSA-400(以上,三洋化成株式会社)、Disrol H14N(日本乳化剂株式会社)等商品名市售者,铵盐或者游离酸类型的ボィズ523A、ボリスタ-OMA是特别合适的。作为(3),可例示出以ソルボ-ル9047K(以上,东邦化学工业株式会社)商品名市售者。钠盐等金属盐以离子交换树脂进行处理,如果使Na等金属转变成H或NH4,就能够使用。
分散剂、表面活性剂的浓度是0.0001~10重量%,优选是0.001~1.0重量%,特别优选的是0.001~0.1重量%。在分散剂浓度低的情况下,颗粒的去除效果不充分,并且即使过高,也不能期待与其相称的效果。
本发明品为了提高和基板的亲和性,或为了抑制表面活性剂的发泡性,也可以加入水溶性醇类。
作为水溶性醇类,可以使用甲醇、乙醇、1-丙醇、2-丙醇、2-甲基-1-丙醇、2-甲氧基乙醇等。水溶性醇的浓度是0.01~30重量%,特别优选的是1~10重量%。
本发明品为了进一步提高金属杂质的去除性,也可以添加螯合剂。
作为螯合剂,优选的是多氨基羧酸类及其铵盐,具体的是乙二胺四乙酸、三乙酸胺、反式1,2-环己二胺四乙酸及其铵盐。螯合剂的浓度是0.0001~0.1重量%,特别优选的是0.0001~0.01重量%。
下面,同时示出本发明的实施例和比较例,详细地说明本发明,但本发明并不受这些实施例的限制。
实施例
以表1所示的组成分别配制成按照本发明的洗净液和比较用的洗净液。
表1
洗净液 | 有机酸化合物 | 分散剂、表面活性剂、螯合剂、水溶性醇 |
实施例1 | 草酸0.34重量% | Disrol H14N 0.01重量% |
实施例2 | 草酸0.34重量% | ボリティ550 0.01重量% |
实施例3 | 草酸0.34重量% | ソルボル9047K 0.01重量% |
实施例4 | 草酸0.34重量% | Newcol 707SF 0.01重量% |
实施例5 | 草酸0.34重量% | レォド-ルス-バ-TW-01200.01重量% |
实施例6 | 草酸0.34重量% | 焦磷酸 0.01重量% |
实施例7 | 草酸0.34重量% | デモ-ルAS 0.01重量% |
实施例8 | 草酸0.03重量% | デモ-ルAS 0.001重量% |
实施例9 | 草酸3.40重量% | デモ-ルAS 0.1重量% |
实施例10 | 草酸0.34重量% | 肌醇六磷酸 0.01重量% |
实施例11 | 草酸0.34重量% | NIKKOL TDP-8 0.01重量% |
表1(续)
洗净液 | 有机酸化合物 | 分散剂、表面活性剂、螯合剂、水溶性醇 |
实施例12 | 草酸 0.34重量% | Newcol 560SF 0.01重量%肌醇六磷酸 0.01重量%2-丙醇 1.0重量% |
实施例13 | 丙二酸 0.5重量% | デモ-ルAS 0.1重量% |
实施例14 | 柠檬酸 10.0重量% | デモ-ルAS 1.0重量% |
实施例15 | 草酸铵 0.2重量% | Newcol 707SF 0.01重量% |
实施例16 | 草酸 0.134重量% | 乙二胺四乙酸铵 0.01重量%Newcol 560SF 1.0重量% |
实施例17 | 柠檬酸铵1.0重量% | 肌醇六磷酸 1.0重量%三乙酸胺 0.01重量% |
实施例18 | 草酸 2.0重量% | Newcol 560SF 0.01重量%肌醇六磷酸 0.01重量%2-丙醇 10.0重量% |
比较例1 | 草酸 0.34重量% | - |
比较例2 | 柠檬酸 0.50重量% | - |
比较例3 | - | デモ-ルAS 0.01重量% |
比较例4 | 草酸 0.34重量% | 十四烷基三甲基氯化铵0.01重量% |
注)Disrol H14N、Newcol 560SF、Newcol 707SF(日本乳化剂(株)制)
ボリティ550(狮王(株)制)
ソルボ-ル9047K(东邦化学工业(株)制)
レォド-ルス-バ-TW-0120、デモ-ルAS(花王(株)制)
NIKKOL TDP-8(日光化学品(株)制)
在以下的实验中使用配制成的各洗净液。
实验例1(颗粒去除能力1:氧化铝颗粒)
浸渍在キャボット制的CMP浆液(WA-355∶Fe-20=1∶1混合液氧化剂:硝酸铁,研磨颗粒:氧化铝)中,由此使带有氧化膜的硅片预先被颗粒污染(φ4英寸、0.24μm以上的颗粒附着数约10000个),然后用实施例1~18和比较例1~4的各洗净液在25℃洗净3分钟,进行水洗、干燥后,用基板表面检查装置Surfscan4500(ク-·ェル·ェ-·テンコ-ル社制)测定颗粒数。比较洗净前和洗净后的颗粒数,对利用各洗净液的颗粒去除能力进行评价。其结果示于表2。
表2
洗净液 | 颗粒(氧化铝)去除率(%) |
实施例1 | 98.8 |
实施例2 | 97.1 |
实施例3 | 95.0 |
实施例4 | 94.6 |
实施例5 | 97.8 |
实施例6 | 99.2 |
实施例7 | 90.1 |
实施例8 | 93.7 |
实施例9 | 99.6 |
实施例10 | 98.7 |
实施例11 | 94.3 |
表2(续)
洗净液 | 颗粒(氧化铝)去除率(%) |
实施例12 | 99.1 |
实施例13 | 95.6 |
实施例14 | 96.5 |
实施例15 | 92.2 |
实施例16 | 97.8 |
实施例17 | 98.2 |
实施例18 | 99.3 |
比较例1 | 42.0 |
比较例2 | 60.4 |
比较例3 | 46.7 |
比较例4 | 12.7 |
实验例2(颗粒去除能力2:二氧化硅)
浸渍在分散有二氧化硅颗粒(粒径0.3μm)的水溶液中,由此使带有氧化膜的硅片预先被二氧化硅颗粒污染(φ4英寸、0.24μm以上的颗粒附着数13000个),然后用实施例4、5、12~16、18和比较例1的洗净液在25℃洗净3分钟,进行水洗、干燥后,用基板表面检查装置Surfscan4500(ケ-·ェル·ェ-·テンコ-ル社制)测定颗粒数。比较洗净前和洗净后的颗粒数,对各洗净液的颗粒去除能力进行评价。其结果示于表3。
表3
洗净液 | 颗粒(二氧化硅)去除率(%) |
实施例4 | 91.9 |
实施例5 | 89.5 |
实施例12 | 98.1 |
实施例13 | 97.5 |
实施例14 | 98.3 |
实施例15 | 95.3 |
实施例16 | 97.9 |
实施例18 | 96.2 |
比较例1 | 54.2 |
实验例3(Fe去除能力)
浸渍在硝酸铁0.1重量%的水溶液中,由此使带有氧化膜的基片预先被金属(Fe)污染,然后使用全反射荧光X射线装置(テクノス制TREX-610T)测定其表面的Fe浓度。
用实施例1~6和比较例1~2的洗净液在25℃洗净3分钟,进行水洗、干燥后,测定基片表面的Fe浓度,对Fe的去除能力进行评价。其结果示于表4。
表4
洗净液 | Fe浓度(×1010原子/cm2) |
洗净前 | 约7600 |
实施例1 | 2.6 |
实施例2 | 3.0 |
实施例3 | 2.4 |
实施例4 | 2.8 |
实施例5 | 3.8 |
实施例6 | 2.7 |
比较例1 | 4.7 |
比较例2 | 321 |
如上所述,本发明的洗净液对金属杂质、颗粒具有优良的去除性能。
Claims (8)
1、洗净电子材料用基板的洗净液,该洗净液含有分散剂和表面活性剂中的至少一种及有机酸化合物,且该洗净液不含有碱;所述有机酸化合物是从草酸、丙二酸、苹果酸、酒石酸、柠檬酸及它们的铵盐组成的组中选择的1种或2种以上,且所述有机酸化合物的量是所述洗净液的总量的0.01~30重量%;所述表面活性剂是阴离子型或者非离子型表面活性剂;所述分散剂是磷酸酯,且所述分散剂和表面活性剂的量是所述洗净液的总量的0.0001~10重量%。
2、如权利要求1所述的洗净液,其还含有螯合剂。
3、如权利要求1所述的洗净液,其还含有水溶性醇。
4、如权利要求1~3中任一项所述的洗净液,其能够同时去除吸附在基板上的金属杂质和颗粒污染物。
5、如权利要求1~3中任一项所述的洗净液,其中,所述电子材料用基板是施加金属配线后的基板。
6、如权利要求4所述的洗净液,其中,所述电子材料用基板是施加金属配线后的基板。
7、如权利要求5所述的洗净液,其是在化学的机械研磨后使用。
8、如权利要求6所述的洗净液,其是在化学的机械研磨后使用。
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CN101113388B (zh) * | 2006-07-28 | 2010-11-03 | 比亚迪股份有限公司 | 一种黑孔碳粉清洗剂组合物及黑孔碳粉的清洗方法 |
TWI465562B (zh) * | 2012-03-29 | 2014-12-21 | Chi Mei Corp | 洗淨液組成物及基板之洗淨方法 |
CN113774391A (zh) * | 2021-08-12 | 2021-12-10 | 上海新阳半导体材料股份有限公司 | 一种化学机械抛光后清洗液的应用 |
CN113774391B (zh) * | 2021-08-12 | 2023-08-04 | 上海新阳半导体材料股份有限公司 | 一种化学机械抛光后清洗液的应用 |
Also Published As
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EP1047121A1 (en) | 2000-10-25 |
US7084097B2 (en) | 2006-08-01 |
JP2001007071A (ja) | 2001-01-12 |
EP1047121B1 (en) | 2005-12-14 |
JP4516176B2 (ja) | 2010-08-04 |
CN1271000A (zh) | 2000-10-25 |
TW541334B (en) | 2003-07-11 |
US20040167047A1 (en) | 2004-08-26 |
KR20010049276A (ko) | 2001-06-15 |
DE60024707D1 (de) | 2006-01-19 |
KR100750603B1 (ko) | 2007-08-20 |
DE60024707T2 (de) | 2006-09-14 |
US6730644B1 (en) | 2004-05-04 |
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