CN112639068A - 清洗液组合物 - Google Patents
清洗液组合物 Download PDFInfo
- Publication number
- CN112639068A CN112639068A CN201980054513.1A CN201980054513A CN112639068A CN 112639068 A CN112639068 A CN 112639068A CN 201980054513 A CN201980054513 A CN 201980054513A CN 112639068 A CN112639068 A CN 112639068A
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- CN
- China
- Prior art keywords
- cleaning liquid
- cleaning
- liquid composition
- substrate
- wiring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000004140 cleaning Methods 0.000 title claims abstract description 129
- 239000000203 mixture Substances 0.000 title claims abstract description 79
- 239000007788 liquid Substances 0.000 title claims abstract description 77
- 239000000758 substrate Substances 0.000 claims abstract description 68
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 35
- 239000004065 semiconductor Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 37
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- 238000004519 manufacturing process Methods 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 239000011550 stock solution Substances 0.000 claims description 7
- 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 6
- 239000002253 acid Substances 0.000 claims description 5
- CFOCOVNPZDVGDV-UHFFFAOYSA-N 3,4,5-trihydroxy-2-methylbenzoic acid Chemical compound CC1=C(O)C(O)=C(O)C=C1C(O)=O CFOCOVNPZDVGDV-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- 229940079877 pyrogallol Drugs 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
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- 239000006061 abrasive grain Substances 0.000 abstract description 13
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- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 12
- 239000000463 material Substances 0.000 description 10
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- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 8
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 5
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
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- 125000003118 aryl group Chemical group 0.000 description 3
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
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- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005540 GaP Inorganic materials 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 1
- 239000005441 aurora Substances 0.000 description 1
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 239000001569 carbon dioxide Substances 0.000 description 1
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- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 description 1
- 125000000457 gamma-lactone group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
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- 230000003595 spectral effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Images
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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
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- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2096—Heterocyclic compounds
-
- 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
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
-
- 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
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/16—Sulfonic acids or sulfuric acid esters; Salts thereof derived from divalent or polyvalent alcohols
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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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/08—Liquid soap, e.g. for dispensers; capsuled
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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
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- C11D3/0042—Reducing agents
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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
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- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/378—(Co)polymerised monomers containing sulfur, e.g. sulfonate
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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
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/08—Acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D7/00—Compositions of detergents based essentially on non-surface-active 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
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- 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
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
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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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- C11D7/265—Carboxylic acids or salts thereof
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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
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- C11D7/266—Esters or carbonates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D7/267—Heterocyclic 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
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- C11D7/32—Organic compounds containing nitrogen
- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
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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
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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
- H01L21/02057—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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- 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
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02074—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a planarization of conductive layers
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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
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Detergent Compositions (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
本发明的目的在于,提供短时间内有效地去除在具有Co接触插头或Co布线的半导体基板中的来源于浆料的有机残留物或磨粒的清洗液。本发明涉及包含一种或两种以上的还原剂及水的用于清洗具有Co接触插头和/或Co布线的基板的清洗液组合物。并且,本发明涉及包含一种或两种以上的还原剂及水,pH为3以上且小于12的用于清洗具有Co且不具有Cu的基板的清洗液组合物。
Description
技术领域
本发明涉及用于清洗具有Co的基板的清洗液组合物。
背景技术
近年来,随着装置的小型化及多层布线结构化的发展,在每个工序中都需要对基板表面进行精确的平坦化处理,作为半导体基板制造工序中的一项新技术,已经引入了如下的化学机械研磨(chemical mechanical polish,CMP)技术:在供给磨料颗粒及化学药品的混合物浆料的同时将晶圆压接到称为抛光布轮的抛光布上,通过旋转以结合化学作用及物理作用来抛光并平坦化绝缘膜或金属材料。
以往,钨(W)已被用作用于将诸如晶体管的栅极、源极及漏极等的电极拉到绝缘膜上的接触插头,但是随着小型化,钴(Co)已被用作电阻比先进设备中的W低的材料。
进一步,电连接这些接触插头与上层部的布线(中线(Middle of Line),MOL)也随着小型化而从铜(Cu)向Co转移。
在形成该设备的工艺中,与以往一样,通过使用诸如氧化铝或氧化硅等的硅化合物或诸如氧化铈等的铈化合物作为磨粒的浆料来进行化学机械研磨。
经化学机械研磨后的基板表面被浆料中所含的氧化铝,二氧化硅或氧化铈颗粒为代表的颗粒,待抛光的表面的组成物质或浆料中所含的来自药品的金属杂质污染。由于这些污染物会导致图案缺陷或附着力不良、电气特性不良等,在进入下一个工序之前,需要将其彻底去除。作为用于去除这些污染物的常规化学机械研磨后清洗,通过联用清洗液的化学作用及由聚乙烯醇制成的海绵刷等物理作用来进行刷洗。
迄今为止,在半导体制造过程中,Co已被用作阻挡金属以防止金属在Cu布线中扩散,尽管已经提出了用于Cu及Co的清洗液(专利文献1~4),但是似乎很难将这些清洗液用于使用Co的接触插头或MOL中。
这是因为用作阻挡金属或衬里的Co非常薄,相对于由浆料产生的称为有机残留物的异物或磨粒很难残留在Co上,由于在接触插头或MOL中,Co的面积大于衬里的面积,并且容易残留有机残留物或磨粒,因此,很难想到可以用于使用Co的阻挡金属或衬里的清洗液是合适的,实际上,事实证明了确实如此。因此,尽管需要与Co接触插头或使用Co的布线(以下、称为Co布线)相对应的清洗液,但是尚未提出这种清洗液。
现有技术文献
专利文献
专利文献1:特表2008-528762号公报
专利文献2:特表2008-543060号公报
专利文献3:特表2015-519723号公报
专利文献4:特表2015-524165号公报
发明内容
技术问题
因此,本发明的目的在于,提供短时间内有效地去除在具有Co接触插头或Co布线的半导体基板中的来源于浆料的有机残留物或磨粒的清洗液。尤其,提供有效去除有机残留物的清洗液。
解决问题的方案
在解决上述问题的认真研究中,本发明人们发现:通过使包含一种或两种以上的还原剂及水的清洗液组合物作用于作为因化学机械研磨产生的Co离子及浆料中所含的防腐剂以复杂方式键合的聚合物的有机残留物上而改变Co离子的化合价,可弱化形成聚合物的化学键,可短时间内有效地去除含Co的来源于浆料的有机残留物或磨粒,进一步进行研究的结果,完成了本发明。
即,本发明涉及以下内容。
[1]包含一种或两种以上的还原剂及水的用于清洗具有Co接触插头和/或Co布线的基板的清洗液组合物。
[2]包含一种或两种以上的还原剂及水,pH为3以上且小于12的用于清洗具有Co且不具有Cu的基板的清洗液组合物。
[3]基板具有Co接触插头和/或Co布线的上述[2]所述的清洗液组合物。
[4]还原剂包含选自由两个以上的羟基直接键合于环上的五元环或六元环化合物组成的组中的一种或两种以上的上述[1]~[3]中任一项所述的清洗液组合物。
[5]还原剂为选自由抗坏血酸、邻苯三酚及甲基没食子酸组成的群中的一种或两种以上的上述[4]所述的清洗用组合物。
[6]还包含一种或两种以上的聚磺酸化合物的上述[1]~[5]中任一项所述的清洗液组合物,作为表面活性剂。
[7]用于通过将其稀释10倍~1000倍来获得上述清洗液组合物的[1]~[6]中任一项所述的清洗液组合物用的原液组合物。
[8]包括使上述[1]~[6]中任一项所述的清洗液组合物与具有Co接触插头和/或Co布线的基板相接触的工序的半导体基板的制造方法。
[9]在与具有Co接触插头和/或Co布线的基板相接触的工序之前,包括化学机械研磨(CMP)具有Co接触插头和/或Co布线的基板的工序的上述[8]所述的半导体基板的制造方法。
[10]与具有Co接触插头和/或Co布线的基板相接触的工序为清洗具有Co接触插头和/或Co布线的基板的工序的上述[8]或[9]所述的半导体基板的制造方法。
发明的效果
本发明的清洗液组合物用于清洗在半导体器件等的电子装置的制造工艺中进行了磨料处理、蚀刻处理及化学机械研磨(CMP)处理等的基板的金属材料表面的过程中短时间内有效地去除金属杂质、微颗粒、其中包含作为Co与有机防腐剂的反应产物的Co的有机残留物或磨粒。并且,本发明的清洗液组合物不仅可以清洗基板而且可以在所有应用中用于溶解含Co的有机残留物。
尤其,适合去除具有Co接触插头和/或Co布线的基板中的含Co的有机残留物或磨粒。
附图说明
图1为示出含有清洗液组合物的还原剂的种类及pH与清洗性之间的关系的图。
图2为示出有无含有清洗液组合物的还原剂、有无表面活性剂及其他成分的种类与清洗性之间的关系的图。
图3为示出有无含有清洗液组合物的还原剂及其他成分的种类与X射线光电子能谱法(XPS)光谱之间的关系的图。
图4为示出有无清洗液组合物的还原剂、有无表面活性剂及pH与Co、SiO2及SiN的每个颗粒的ζ电位之间的关系的图。
具体实施方式
以下,将基于本发明的优选的实施方式详细说明本发明。
首先,将说明本发明的清洗液组合物及原液组合物。
本发明的清洗液组合物为用于清洗具有Co接触插头和/或Co布线的基板的清洗液组合物,是包含一种或两种以上的还原剂及水的清洗液组合物。
对本发明中所使用的还原剂没有特别限制,只要其能够改变Co离子的化合价即可,但是可包含诸如两个以上的羟基直接键合于环上的五元环或六元环化合物等。这些还原剂既可以使用一种或也可以使用两种以上。
两个以上的羟基直接键合于环上的五元环或六元环既可以是饱和或不饱和的五元环或六元环,并且,也可以是芳香族五元环或六元环。在本发明中,优选使用两个以上的羟基直接键合于环上的芳香族五元环或芳香族六元环,诸如包含但不限于γ内脂基及苯基等。并且,只要两个以上的羟基直接键合于环上,除羟基以外的取代基也可以直接键合于环上。
本发明中所使用的还原剂优选为抗坏血酸、邻苯三酚及甲基没食子酸,从清洗液的稳定性的观点出发,特别优选为邻苯三酚、甲基没食子酸。
在本发明中,清洗液组合物的pH优选小于12,更优选3以上且小于12。从含有Co的有机残留物及磨粒的清洗性的观点出发,当pH为4~9时可获得更高的清洗性,pH特别优选为6~9。
并且,为了提高微颗粒的去除性,本发明的清洗液组合物也可包含表面活性剂。表面活性剂的种类根据待去除的微颗粒或基板适当地进行选择,优选但不限于聚磺酸化合物。作为聚磺酸化合物可包括诸如萘磺酸甲醛缩合物、聚苯乙烯磺酸、木质素磺酸及其盐等。
有机残留物可包含但不限于含有Co的有机残留物,上述含有Co的有机残留物为通过在化学机械研磨过程中使Co与苯并三唑(BTA)等的有机类防腐剂反应生成的由Co交联的有机金属络合物的二聚体或低聚物,且难溶。作为根据本发明的清洗液组合物的对象的基板的有机残留物可包含高浓度的Co。为了在清洗液中溶解其含有Co的有机残留物,有一种通过改变清洗液的pH来切断Co与有机类防腐剂之间的配位键合以使其低分子化的方法。
在含有Co的有机残留物中,作为通过在化学机械研磨过程中使Co与苯并三唑(BTA)等的有机类防腐剂反应生成的由Co交联的有机金属络合物的二聚体或低聚物,可包括但不限于诸如Co-苯并三唑(BTA)复合体。
Co-苯并三唑复合体是指通过交联等形成的Co及苯并三唑(BTA)复合体,可包括但不限于在Co-苯并三唑(Co-BTA)络合物及Cu-苯并三唑(Co-BTA)络合物中混合有源自诸如SiO2等浆料的无机物的化合物等。
本发明中具有Co接触插头和/或Co布线的基板,只要是在化学机械研磨(CMP)后获得的基板就可以,可包括但不限于诸如紧接在化学机械研磨之后的基板及在形成Co接触插头和/或Co布线之后,紧接在通过干蚀刻加工上层的绝缘膜之后的基板等。其中,优选紧接在化学机械研磨之后的基板。
本发明中的化学机械研磨(CMP)可根据公知的化学机械研磨而进行,可包括但不限于诸如使用SiO2或Al2O3等磨粒的抛光方法、及使用电解水的无磨粒的抛光方法等。其中,优选使用SiO2或Al2O3等磨粒的抛光方法。
本发明的原液组合物为通过稀释获得本发明的清洗液组合物的组合物,可以但不限于通过将上述原液组合物稀释10倍以上,优选10~1000倍,更优选50~200倍而获得本发明的清洗液组合物,根据所构成的成分可适当地确定。
由于本发明的清洗液组合物主要由水构成,因此,在电子装置的生产线中设置稀释用混合装置的情况下,由于以原液组合物供给并在即将使用之前通过稀释成含水的希釈液(上述希釈液包含仅由超纯水组成的稀释液)来使用,因此,具有可赋予减少运输成本、减少运送过程中的二氧化碳气体、及减少电子装置制造商的制造成本的优点。
本发明的清洗液组合物可用于诸如具有Co接触插头和/或Co布线的基板上,尤其适用于具有Co接触插头和/或Co布线且无Cu的基板上。并且,适用于化学机械研磨(CMP)之后的基板上,其中,在化学机械研磨之后的基板表面上除基板表面的各种布线和阻挡金属材料(Co、Ti基化合物、Ta基化合物、Ru等)及绝缘膜材料(SiO2、低介电常数(low-可)之外,可能存在浆料中所包含的微颗粒或金属杂质。微颗粒主要为诸如氧化铝、二氧化硅及氧化铈等,金属杂质可包含抛光过程中溶解并重新附着在浆料中的Cu、源自浆料中的氧化剂的Fe、并且,浆料中所含的Co防腐剂与Co反应的Co有机金属络合物等。
在本发明中,阻挡金属为使用在半导体基板的接触插头或布线与绝缘膜之间形成的层(阻挡金属层)以防止接触插头或布线中的金属扩散到绝缘膜中的Co、Ti基化合物、Ta基化合物、Ru等。
并且,低介电常数材料为用于层间绝缘膜等的具有低介电常数的材料,可包含但不限于诸如多孔硅、含硅有机聚合物、四乙氧基硅烷(TEOS)等。具体地,可包含黑钻(由应用材料公司制造)、及Aurora(由美国金属协会制造)等。
接下来,将说明根据本发明的半导体基板的制造方法。
根据本发明的半导体基板的制造方法为包括使本发明的清洗液组合物与具有Co接触插头和/或Co布线的基板相接触的工序的半导体基板的制造方法。
并且,在根据本发明的半导体基板的制造方法中,在使本发明的清洗液组合物与具有Co接触插头和/或Co布线的基板相接触的工序之前,包括化学机械研磨(CMP)具有Co接触插头和/或Co布线的基板的工序。
作为使其相接触的工序,可包括但不限于诸如化学机械研磨之后的清洗工序及通过干蚀刻加工Co接触插头上层的绝缘膜之后的清洗工序。作为用于使其相接触的方法,可包括但不限于诸如并用刷子擦洗的单晶片清洗法、由喷雾或喷嘴喷射清洗液的单晶片清洗法、间歇式喷雾清洗法、间歇式浸入清洗法等。其中,优选并用刷子擦洗的单晶片清洗法及由喷雾或喷嘴喷射清洗液的单晶片清洗法,特别优选并用刷子擦洗的单晶片清洗法。
作为使其接触的气氛,可包括但不限于诸如空气中,氮气氛中及真空中等。其中,优选为空气中及氮气氛中。
接触时间根据目的而适当地进行选择,因此,在并用刷子擦洗的单晶片清洗法及由喷雾或喷嘴喷射清洗液的单晶片清洗法的情况下,为0.5~5分钟,在间歇式喷雾清洗法及间歇式浸入清洗法的情况下,为0.5~30分钟,但并不限于此。
温度根据目的而适当地进行选择,没有特别的限制,在并用刷子擦洗的单晶片清洗法及由喷雾或喷嘴喷射清洗液的单晶片清洗法的情况下,为20℃~50℃,在间歇式喷雾清洗法及间歇式浸入清洗法的情况下,为20℃~100℃。
上述接触条件可根据目的适当地进行组合。
作为半导体基板,可包括但不限于诸如硅、碳化硅、氮化硅、砷化镓、氮化镓、磷镓及铟磷等。其中,优选为硅、碳化硅、砷化镓及氮化镓,特别优选为硅及碳化硅。
接下来,将说明根据本发明的用于溶解含有Co的有机残留物的方法。
溶解本发明的含有Co的有机残留物的方法包括使包含一种或两种以上还原剂及水且pH为4~9的清洗液组合物与含有Co的有机残留物相接触的工序。
作为清洗液组合物只要是如上所述的,就没有特别限制,可使用详述的本发明的清洗液组合物。
作为使其相接触的方法没有特别限制,只要是如上所述的方法即可。
实施例
接下来,对于本发明的清洗液组合物,将通过下述例更详细地说明本发明,但是本发明并不限于此。
评价A:清洗液组合物的清洗性(清洗Co晶圆之后的缺陷数量)
(化学机械研磨抛光液的制备)
利用超纯水(DIW)将使用平均粒径为70nm的氧化硅的浆料(型号:HS-CB915-B,由日立化成株式会社制造)稀释3倍,与过氧化氢溶液混合,得到了化学机械研磨抛光液。
(准备待抛光的晶圆)
准备了具有如下成分的Co基板(PVD-Co2k/Ti/Th-SiO2/Si、由Advancedmaterials Technology Co.,Ltd.制备)。
(晶圆的抛光)
使用上述化学机械研磨抛光液,通过抛光装置(型号:ARW-681MSII,由Matt Co.,Ltd.制造的化学机械研磨抛光装置)将待抛光的上述抛光对象晶圆30秒中,完成抛光后,在旋转晶圆的同时使用100mL的超纯水(DIW)冲洗10秒钟。使用表1及表2的清洗液组合物(除例11及12之外,使用盐酸及四甲基氢氧化铵(TMAH)将pH调节至预定pH。并且,例11及12为不包含关东化学制造的还原剂的化学机械研磨之后的清洗液,分别为用于Co阻挡金属的碱性Cu化学机械研磨之后的清洗液、用于Ta阻挡金属的酸性Cu化学机械研磨之后的清洗液。),通过在旋转冲洗的晶圆的同时转动由聚乙烯醇制成的刷子(由Aion制造)来清洗晶圆60秒钟。在旋转清洗后的晶圆的同时利用300mL的超纯水(DIW)冲洗30秒钟,通过再次旋转的同时在25℃中干燥30秒钟来获得用于测量的晶圆。
(晶圆表面缺陷数量的测量)
通过表面检查装置(型号:WM-10,由Topcon制造)测量上述用于测量的晶圆表面的缺陷数量,评价清洗液组合物的清洗性。评价结果如图1及图2所示。
(结果)
如表1、表2、图1及图2所示,可确认:在pH值为相同的12的情况下,在含有还原剂的清洗液组合物中清洗的晶圆表面的缺陷数量比在不含还原剂的清洗液组合物中清洗的晶圆表面的缺陷数量小(例10、11及13)。即,可以确认:含有还原剂的清洗液组合物的清洗性比不含还原剂的清洗液组合物的清洗性高。并且,可以确认,即使在含有还原剂的清洗液组合物中,pH为4、6、9的清洗液组合物的清洗性比pH为12的清洗液组合物的清洗性高。通常,用于清洗Cu的清洗液(例11及例12)并不适合用作Co的清洗液,并具有比本发明的清洗液组合物的清洗液更优秀的清洗性能。
表1
表2
评价B:清洗液组合物的有机残留物的去除性(Co-苯并三唑的去除性)
(Co-苯并三唑基板的準備)
将由以下成分构成的Co基板(PVD-Co2k/Ti/Th-SiO2/Si、由Advanced materialsTechnology Co.,Ltd.制造)切割成1.0×1.0cm2,在将这些基板浸入到1%的草酸水溶液中10秒钟之后,用超纯水(DIW)冲洗1分钟,然后浸入到苯并三唑水溶液(浓度为10mM、pH为8)中2分钟之后,再次用超纯水(DIW)冲洗1分钟,通过吹氮气干燥,获得Co-苯并三唑基板。
(评价用基板的准备)
将由以下成分构成的Co基板(PVD-Co2k/Ti/Th-SiO2/Si、由Advanced materialsTechnology Co.,Ltd.制造)切割成1.0×1.0cm2,在将这些基板浸入到1%的草酸水溶液中10秒钟之后,用超纯水(DIW)冲洗一分钟,然后浸入到苯并三唑水溶液(浓度为10mM、pH未8)中2分钟之后,再之后,用超纯水(DIW)冲洗1分钟,浸入到表3及表4的各清洗液组合物(使用盐酸及四甲基氢氧化铵(TMAH)将pH调节至预定pH)中1分钟之后,再次用超纯水(DIW)冲洗一分钟,通过吹氮气干燥,获得评价用基板。
(Co-苯并三唑的去除性评价)
使用X射线光电子能谱法(X射线光电子能谱、型号:JPS-9200,由日本电子制造)测量上述各基板的N1s光谱。比较当以获得的Co-苯并三唑基板的光谱为基准时的评价用基板的光谱強度,从强度的减少程度来评价Co-苯并三唑的去除性。
(结果)
可确认:与Co-苯并三唑的光谱相比,如图3所示的pH4至pH9的例18~20的X射线光电子能谱法光谱的光谱强度正在减少。可确认:与Co-苯并三唑的光谱相比,不含还原剂的例14~16的X射线光电子能谱法光谱的光谱正在减少,但相比例18~20,其减少程度少。从上述结果可确认:还原剂对去除Co-苯并三唑(源自浆料的有机残留物)有效。
表3
表4
评价C:在清洗液组合物中的Co、SiO2及SiN的每个颗粒的ζ电位的测量
将0.05g平均粒径为50nm的钴(由西格玛奥德里奇会社(SIGMA-ALDRICH)制造)与20ml的超纯水(DIW)混合,在使用超音波装置搅拌10分钟以使其均匀分散之后,收集20μL的上述溶液,并将其添加到50mL的具有表5所示的成分的清洗液组合物中(使用盐酸及四甲基氢氧化铵(TMAH)将pH调节至预定pH)。进一步搅拌这些溶液并使其均匀,使用ζ电位测量装置(型号:ELS-Z,由大塚电子会社制造)测量钴的ζ电位。
对于氧化硅及氮化硅的每个颗粒,以钴相同的方法测量了ζ电位(mV)。
结果示于表5及图4中。
(结果)
从表5及图4中确认:对于钴,含有还原剂和/或表面活性剂的清洗液组合物中的ζ电位低于不含还原剂及表面活性剂中任意一个的清洗液组合物中的ζ电位。对于氧化硅,未观察到根据清洗液组合物的组成引起的ζ电位的大的差异。已确认:对于氮化硅,含有还原剂和/或表面活性剂的清洗液组合物中的ζ电位低于不含还原剂及表面活性剂中任意一个的清洗液组合物中的ζ电位。
并且,特别是在钴及氮化硅的情况下,含有还原剂的清洗液组合物的ζ电位在酸性区域超过0,相反,含有还原剂和/或表面活性剂的清洗液组合物的ζ电位在pH6~12的宽范围pH区域内呈现出大的负的ζ电位。因此,包含钴布线或氮化硅的清洗对象物中同样呈现出负的ζ电位。由于钴磨料浆料中所含的二氧化硅磨粒通常具有负的ζ电位,因此,通过使用还原剂和/或表面活性剂的本清洗液组合物,在通过二氧化硅磨粒与清洗对象物之间的负的ζ电位引起的排斥作用来提高二氧化硅磨粒的剥离效果的同时期待防止再次附着到清洗对象物的效果,并提高清洗性能。
表5
Claims (10)
1.一种用于清洗具有Co接触插头和/或Co布线的基板的清洗液组合物,其特征在于,
包含一种或两种以上的还原剂及水。
2.一种用于清洗具有Co且不具有Cu的基板的清洗液组合物,其特征在于,包含一种或两种以上的还原剂及水,pH为3以上且小于12。
3.根据权利要求2所述的清洗液组合物,其特征在于,基板具有Co接触插头和/或Co布线。
4.根据权利要求1至3中任一项所述的清洗液组合物,其特征在于,还原剂包含选自由两个以上的羟基直接键合于环上的五元环或六元环化合物组成的组中的一种或两种以上。
5.根据权利要求4所述的清洗液组合物,其特征在于,还原剂为选自由抗坏血酸、邻苯三酚及甲基没食子酸组成的组中的一种或两种以上。
6.根据权利要求1至5中任一项所述的清洗液组合物,其特征在于,还包含一种或两种以上的聚磺酸化合物作为表面活性剂。
7.一种权利要求1至6中任一项所述的清洗液组合物用原液组合物,其特征在于,用于通过将其稀释10倍~1000倍来获得上述清洗液组合物。
8.一种半导体基板的制造方法,其特征在于,
包括使权利要求1至6中任一项所述的清洗液组合物与具有Co接触插头和/或Co布线的基板相接触的工序。
9.根据权利要求8所述的半导体基板的制造方法,其特征在于,在与具有Co接触插头和/或Co布线的基板相接触的工序之前,包括化学机械研磨具有Co接触插头和/或Co布线的基板的工序。
10.根据权利要求8或权利要求9所述的半导体基板的制造方法,其特征在于,与具有Co接触插头和/或Co布线的基板相接触的工序为清洗具有Co接触插头和/或Co布线的基板的工序。
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