JP6414072B2 - 半導体基板用洗浄剤および半導体基板表面の処理方法 - Google Patents
半導体基板用洗浄剤および半導体基板表面の処理方法 Download PDFInfo
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- JP6414072B2 JP6414072B2 JP2015546707A JP2015546707A JP6414072B2 JP 6414072 B2 JP6414072 B2 JP 6414072B2 JP 2015546707 A JP2015546707 A JP 2015546707A JP 2015546707 A JP2015546707 A JP 2015546707A JP 6414072 B2 JP6414072 B2 JP 6414072B2
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- cleaning agent
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- copper
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- 239000000758 substrate Substances 0.000 title claims description 191
- 239000012459 cleaning agent Substances 0.000 title claims description 139
- 239000004065 semiconductor Substances 0.000 title claims description 118
- 238000003672 processing method Methods 0.000 title claims description 8
- -1 1,2,3-trihydroxypropyl group Chemical group 0.000 claims description 129
- 229910052751 metal Inorganic materials 0.000 claims description 106
- 239000002184 metal Substances 0.000 claims description 106
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 104
- 229910052802 copper Inorganic materials 0.000 claims description 104
- 239000010949 copper Substances 0.000 claims description 102
- 238000000034 method Methods 0.000 claims description 75
- 125000004432 carbon atom Chemical group C* 0.000 claims description 73
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 65
- 229910017052 cobalt Inorganic materials 0.000 claims description 61
- 239000010941 cobalt Substances 0.000 claims description 61
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 59
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 58
- 125000000217 alkyl group Chemical group 0.000 claims description 58
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 57
- 239000012964 benzotriazole Substances 0.000 claims description 52
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 51
- 239000007864 aqueous solution Substances 0.000 claims description 47
- 150000007524 organic acids Chemical class 0.000 claims description 33
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- 150000002443 hydroxylamines Chemical class 0.000 claims description 29
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- 150000004985 diamines Chemical class 0.000 claims description 20
- 125000002947 alkylene group Chemical group 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 18
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- 239000000126 substance Substances 0.000 claims description 10
- 229920001174 Diethylhydroxylamine Polymers 0.000 claims description 8
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 8
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 8
- FVCOIAYSJZGECG-UHFFFAOYSA-N diethylhydroxylamine Chemical group CCN(O)CC FVCOIAYSJZGECG-UHFFFAOYSA-N 0.000 claims description 8
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 6
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 6
- 229940079877 pyrogallol Drugs 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 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 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 3
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 claims description 3
- 229940074391 gallic acid Drugs 0.000 claims description 3
- 235000004515 gallic acid Nutrition 0.000 claims description 3
- 229960004337 hydroquinone Drugs 0.000 claims description 3
- 229940075579 propyl gallate Drugs 0.000 claims description 3
- 235000010388 propyl gallate Nutrition 0.000 claims description 3
- 239000000473 propyl gallate Substances 0.000 claims description 3
- 125000004742 propyloxycarbonyl group Chemical group 0.000 claims description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 2
- IAJILQKETJEXLJ-RSJOWCBRSA-N aldehydo-D-galacturonic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-RSJOWCBRSA-N 0.000 claims description 2
- 239000000174 gluconic acid Substances 0.000 claims description 2
- 235000012208 gluconic acid Nutrition 0.000 claims description 2
- 238000006392 deoxygenation reaction Methods 0.000 claims 1
- 239000010408 film Substances 0.000 description 247
- 238000005260 corrosion Methods 0.000 description 71
- 230000007797 corrosion Effects 0.000 description 70
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(i) oxide Chemical compound [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 68
- 235000012431 wafers Nutrition 0.000 description 60
- 230000008569 process Effects 0.000 description 40
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 31
- 239000005751 Copper oxide Substances 0.000 description 30
- 150000001412 amines Chemical group 0.000 description 30
- 229910000431 copper oxide Inorganic materials 0.000 description 30
- 238000011156 evaluation Methods 0.000 description 30
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 27
- 239000002253 acid Substances 0.000 description 24
- 238000004140 cleaning Methods 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 24
- 230000001681 protective effect Effects 0.000 description 24
- 229910052757 nitrogen Inorganic materials 0.000 description 20
- 239000002245 particle Substances 0.000 description 19
- 125000003277 amino group Chemical group 0.000 description 18
- 238000000576 coating method Methods 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 150000001409 amidines Chemical class 0.000 description 17
- 239000012535 impurity Substances 0.000 description 17
- 229910000428 cobalt oxide Inorganic materials 0.000 description 16
- 125000004433 nitrogen atom Chemical group N* 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 150000003216 pyrazines Chemical class 0.000 description 14
- 150000003230 pyrimidines Chemical class 0.000 description 14
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 13
- 239000004094 surface-active agent Substances 0.000 description 13
- GQHTUMJGOHRCHB-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine Chemical compound C1CCCCN2CCCN=C21 GQHTUMJGOHRCHB-UHFFFAOYSA-N 0.000 description 12
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 12
- 229910044991 metal oxide Inorganic materials 0.000 description 12
- 150000004706 metal oxides Chemical class 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 description 11
- 239000010419 fine particle Substances 0.000 description 11
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 11
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 description 10
- 229910002065 alloy metal Inorganic materials 0.000 description 10
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 10
- 159000000000 sodium salts Chemical class 0.000 description 10
- 239000010936 titanium Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 150000003851 azoles Chemical class 0.000 description 9
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 9
- 235000005985 organic acids Nutrition 0.000 description 9
- 238000007747 plating Methods 0.000 description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 150000003863 ammonium salts Chemical class 0.000 description 8
- 125000004122 cyclic group Chemical group 0.000 description 8
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- 230000000694 effects Effects 0.000 description 8
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 8
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 8
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- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
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- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 8
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 6
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical compound NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 description 6
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 description 6
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- 150000005215 alkyl ethers Chemical class 0.000 description 6
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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
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- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
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- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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Images
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
-
- 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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- C11D7/261—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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
-
- 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
-
- 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
- C11D3/26—Organic compounds containing nitrogen
-
- 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
- C11D3/26—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
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- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
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- C11D7/32—Organic compounds containing nitrogen
-
- 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
-
- 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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- C11D7/22—Organic compounds
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- C11D7/3218—Alkanolamines or alkanolimines
-
- 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
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- 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
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Description
(1)CMP工程後の半導体基板(ウエハ)表面に残存するシリカやアルミナ等の研磨微粒子(パーティクル)および金属不純物(金属残渣)、ならびにCMP工程において、銅配線膜表面または銅合金配線膜表面に形成される、BTAなどの防食剤を含む被膜(保護膜)の除去性に優れる。
(2)CMP工程において、銅配線膜表面または銅合金配線膜表面に形成される酸化銅(I)と、例えばコバルトを主成分とするバリアメタル表面等に形成される酸化コバルト(II)との異種金属接触腐食(ガルバニック腐食)を引き起こしにくい。
(3)防食剤を含む被膜(保護膜)の除去後に基板(ウエハ)表面に露出する酸化銅(I)からなる金属酸化物をほとんど除去しない。すなわち、防食剤を含む被膜(保護膜)を除去し、酸化銅(I)からなる金属酸化物の被膜(酸化銅(I)膜)をほとんど除去しない。
上述したごとき効果を奏する本発明の半導体基板用洗浄剤を用いることにより、異種金属接触腐食(ガルバニック腐食)に起因する腐食を抑制し、銅配線膜表面または銅合金配線膜表面が、十分な膜厚を有する酸化銅(I)からなる金属酸化物で保護されるため、銅配線膜または銅合金配線膜の経時安定性が高く、結果として、銅配線または銅合金配線間の短絡が生じにくい半導体基板を得ることができるという効果を奏する。
本発明の半導体基板用洗浄剤は、銅配線膜または銅合金配線膜と、コバルト含有膜とを有する半導体基板の化学機械研磨工程の後工程において使用される洗浄剤であって、(A)一般式(1)で示される有機酸、(B)(B-1)一般式(2)で示されるジアミン類、(B-2)一般式(3)で示されるアミジン類、(B-3)一般式(4)で示されるアゾ−ル類および(B-4)一般式(5)で示されるピラジン類またはピリミジン類から選ばれるアミン、(C)ヒドロキシルアミン誘導体、ならびに(D)一般式(6)で示される脱酸素剤を含有し、pHが10以上の水溶液である。
本発明の半導体基板用洗浄剤において、洗浄対象である半導体基板は、半導体基板を構成するウエハの上部に、少なくとも銅配線膜または銅合金配線膜と、コバルト含有膜とを有し、当該銅配線膜または銅合金配線膜と、コバルト含有膜とが、基板表面において接触している状態の基板(以下、本発明にかかる半導体基板と略記する場合がある。)などである。
本発明の半導体基板用洗浄剤は、化学機械研磨(CMP)工程の後工程において使用される洗浄剤である。具体的には、本発明の半導体基板用洗浄剤は、銅配線膜または銅合金配線膜と、コバルト含有膜とを有する半導体基板をCMP工程に付した後の洗浄工程に用いられるものである。本発明の半導体基板用洗浄剤をCMP工程の後工程である洗浄工程に用いることにより、(1)CMP工程後の半導体基板(ウエハ)表面に残存するシリカやアルミナ等の研磨微粒子(パーティクル)および金属不純物(金属残渣)、ならびにCMP工程において銅配線膜表面または銅合金配線膜表面に形成される、BTAなどの防食剤を含む被膜(保護膜)を十分に除去でき、(2)異種金属接触腐食(ガルバニック腐食)に起因する腐食を抑制し、(3)十分な膜厚を有する酸化銅(I)からなる金属酸化物で保護された、銅配線膜または銅合金配線膜を有する半導体基板が得られるので、銅配線膜または銅合金配線膜の経時安定性が高く、結果として、銅配線または銅合金配線間の短絡が生じにくい半導体基板を得ることができる。
本発明の半導体基板表面の処理方法は、(A)上記一般式(1)で示される有機酸、(B)(B-1)上記一般式(2)で示されるジアミン類、(B-2)上記一般式(3)で示されるアミジン類、(B-3)上記一般式(4)で示されるアゾ−ル類および(B-4)上記一般式(5)で示されるピラジン類またはピリミジン類から選ばれるアミン、(C)ヒドロキシルアミン誘導体、および(D)上記一般式(6)で示される脱酸素剤、ならびに必要に応じて(E)アルカリ化合物および(F)界面活性剤を含有し、pHが10以上の水溶液である洗浄剤を用いることを特徴とする、銅配線膜または銅合金配線膜と、コバルト含有膜とを有する半導体基板表面の処理方法である。すなわち、本発明の半導体基板表面の処理方法は、本発明の半導体基板用洗浄剤を用いることを特徴とするものであり、処理方法自体には特に制限はない。
直径8インチの銅めっき基板(銅めっき膜:1.5μm/銅シード層/チタンバリア層/シリコン酸化膜:300nmを有するシリコン基板)を2cm×2cmに細片化し、細片化した基板を0.1N塩酸に1分間浸漬し、基板表面の酸化膜を除去した。次いで、該基板をUVオゾンクリーナー(フィルジェン株式会社製UV253)を用いて3時間処理し、5%ジエチルヒドロキシルアミン(DEHA)水溶液に1時間浸漬した後、純水で10秒間リンスし、基板を乾燥させることによって、酸化銅(I)膜を有する基板を作製した。該基板を評価基板Aとした。
特開2011−3665号公報に準じて作製した模擬スラリーで、直径4インチの銅めっき基板(銅めっき膜:1.5μm/銅シード層/チタンバリア層/シリコン酸化膜:300nmを有するシリコン基板)の表面を1分間研磨して平坦化した後、純水で10秒間リンスし、基板を乾燥させた。次いで、該基板を2cm×2cmに細片化することによって、銅めっき表面にベンゾトリアゾールおよび銅(I)とベンゾトリアゾールとの錯体が付着した基板を作製した。該基板を評価基板Bとした。
直径8インチのコバルトスパッタ基板を2cm×2cmに細片化し、細片化した基板を0.1N塩酸に1分間浸漬し、基板表面の酸化膜を除去した。次いで、該基板をUVオゾンクリーナー(フィルジェン株式会社製UV253)を用いて3時間処理することによって、酸化コバルト(II)膜を有する基板を作製した。該基板を評価基板Cとした。
直径4インチのシリコン酸化膜基板の表面に、スピンコーター(ミカサ株式会社製MS-A200)を用い、500rpm/5秒、3000rpm/30秒の条件で、レジストLORおよびTSMR7cpを順に塗布した。次いで、該基板を、マスクを介して両面アライナー(スーズ・マイクロテック社製SUSS MA6/BA6)により露光した後(露光量:50mJ/cm2)、2.4%テトラメチルアンモニウムヒドロキシド(TMAH)水溶液に100秒間浸漬することで現像処理した。現像処理後の該基板を、小型ドライエッチング装置(株式会社アルバック製CSE-1210型)を用いて30秒間エッチングすることによりレジスト表面の有機物を分解し、次いで、電子ビーム蒸着装置(株式会社アルバック製EX-550-D10)を用いておよそ6nmの膜厚を有する金属銅膜を蒸着した後、アセトンに20分間浸漬することでレジストをリフトオフした。次いで、金属銅膜付きの該基板を1cm×1cmに細片化し、細片化した基板をUVオゾンクリーナー(フィルジェン株式会社製UV253)を用いて1時間処理することによって、酸化銅(I)膜を有する基板を作製した。該基板を評価基板Dとした。
(a)酸化銅(I)の溶解性の評価
表1または表2に示す各種有機酸、アミン、ヒドロキシルアミンまたはヒドロキシルアミン誘導体および脱酸素剤を、表1または表2に示す重量%を含有し、かつコリンで所定のpH値となるように調整した水溶液(洗浄剤)を40mLずつ用意した。次いで、これらの水溶液(洗浄剤)に評価基板Aを入れ、撹拌しながら室温で3分間浸漬した後、該水溶液(洗浄剤)8mLをサンプリングした。その後、サンプリングした水溶液(洗浄剤)に濃硝酸100μLを添加して、溶液のpHを酸性にした後、誘導結合プラズマ発光分光分析装置(ICP-AES)(SII製SPS-3100)を用いて酸化銅(I)に含まれる銅の溶解量を測定した。その結果を表1および表2に示す。なお、現在求められている銅配線の配線幅は10〜20nmであり、その場合のCMP工程後の銅配線膜表面の酸化銅(I)の膜厚はおよそ5〜7nmと推測される。また、CMP工程後の洗浄工程を経た基板が安定な酸化銅(I)表面を維持するためには、該基板の酸化銅(I)は、1nm以上の膜厚を有する必要があると考えられる。よって、一般的な実用機の洗浄時間1〜2分間において、基板(ウエハ)表面の酸化銅(I)膜の溶解を少なくとも4nm以下に抑える必要があると考えられる。使用した評価基板Aの面積(2cm×2cm)および水溶液(洗浄剤)の体積(40mL)を考慮して、抑制すべき酸化銅(I)の溶解量を算出すると、溶解量を少なくとも0.4ppm以下に抑える必要がある。以上より、酸化銅(I)の溶解量が0.4ppm以下の水溶液(洗浄剤)は、銅配線の経時安定性および腐食抑制能において「良好」であると判定し、酸化銅(I)の溶解量が0.4ppmを超えてしまう水溶液(洗浄剤)は、銅配線の経時安定性および腐食抑制能において「不良」であると判定した。
表1または表2に示す各種有機酸、アミン、ヒドロキシルアミンまたはヒドロキシルアミン誘導体および脱酸素剤を、表1または表2に示す重量%を含有し、かつコリンで所定のpH値となるように調整した水溶液(洗浄剤)を10mLずつ用意した。次いで、これらの水溶液(洗浄剤)に評価基板Bを入れ、撹拌しながら室温で1分間浸漬した後、評価基板Bを水溶液(洗浄剤)から取り出し、純水で10秒間流水リンスして、窒素ガスで乾燥した。その後、評価基板Bを0.1N塩酸1.5mLに室温で5分間浸漬し、該評価基板Bに残存するベンゾトリアゾールを抽出し、次いで、抽出液1.5mLのうちの1mLに1N水酸化ナトリウム水溶液100μLを添加して、溶液を中和した後、高速液体クロマトグラフィー(展開溶媒;アセトニトリル:水=1:9、flow speed;1.2mL/min、UV detect;254nm、保持時間;11min)により、抽出液に含まれるベンゾトリアゾールの量を定量した。その結果を表1および表2に示す。なお、CMP工程後の銅配線表面に対するベンゾトリアゾール(ベンゾトリアゾールそのものおよび銅(I)とベンゾトリアゾールとの錯体)の付着量は、スラリーに依存するものの、およそ60ng/cm2である。一般的な実用機を用いた洗浄では、ブラシを用いて1〜2分間洗浄するが、本評価実験では1分間の浸漬洗浄により簡易評価した。該簡易評価において、ベンゾトリアゾール(ベンゾトリアゾールそのものおよび銅(I)とベンゾトリアゾールとの錯体)の除去率が75%以上(ベンゾトリアゾールの残存量が15ng/cm2以下)の評価結果が得られた水溶液(洗浄剤)を用いて、一般的な実用機によるベンゾトリアゾールの除去性の評価を行ったところ、基板(ウエハ)から完全にベンゾトリアゾール(ベンゾトリアゾールそのものおよび銅(I)とベンゾトリアゾールとの錯体)が除去されたことを確認した。以上より、本簡易評価において、ベンゾトリアゾールの除去率が75%以上(ベンゾトリアゾールの残存量が15ng/cm2以下)の水溶液(洗浄剤)は、ベンゾトリアゾールの除去性能において「良好」であると判定し、ベンゾトリアゾールの除去率が75%未満(ベンゾトリアゾールの残存量が15ng/cm2より多い)の水溶液(洗浄剤)は、ベンゾトリアゾールの除去性能において「不良」であると判定した。
表1または表2に示す各種有機酸、アミン、ヒドロキシルアミンまたはヒドロキシルアミン誘導体および脱酸素剤を、表1または表2に示す重量%を含有し、かつコリンで所定のpH値となるように調整した水溶液(洗浄剤)を1mLずつ用意した。次いで、ポテンシオスタットの三極式セルを使用し、作用極に評価基板Aまたは評価基板C、対極に白金ワイヤー、参照極に飽和銀・塩化銀電極を用いて、これらの三極式セルを上記水溶液(洗浄剤)に浸漬し、評価基板Aおよび評価基板Cの酸化還元電位(腐食電位)をそれぞれ測定して、その電位差を求めた。その結果を表1および表2に示す。また、実施例6の水溶液(洗浄剤)に、酸化銅(I)と酸化コバルト(II)のCMP処理済パターンウエハ(フィルテック社製)を入れ、攪拌しながら室温で3分間浸漬した。次いで、該パターンウエハを水溶液(洗浄剤)から取り出した後、純水で10秒間流水リンスし、窒素ガスで乾燥した。乾燥後のパターンウエハを電解放出型走査電子顕微鏡(FE-SEM)(株式会社日立ハイテクノロジーズ製S-4800)により腐食度合いを観察した。その結果を図1に示す。あわせて、比較例4および比較例9の水溶液(洗浄剤)を用いてパターンウエハを浸漬した場合の腐食度合いを観察した図をそれぞれ図2および図3に示す。なお、図1〜3において、写真中央にある白色部分は銅を表し、銅を表す白色部分に沿った筋形の黒色部分はコバルトを表し、コバルトを表す黒色部分に沿った筋形の白色部分はコバルトの下層にあるチタンを表す。図1〜3からわかるように、実施例6の水溶液(洗浄剤)を用いてパターンウエハを浸漬した場合には、コバルトが腐食されなかった。その一方で、比較例4および比較例9の水溶液(洗浄剤)を用いてパターンウエハを浸漬した場合には、酸化銅(I)と酸化コバルト(II)との異種金属接触腐食(ガルバニック腐食)により、コバルトが腐食されてしまい、下層にあるチタン層が露出してしまった。腐食のなかった実施例6の水溶液(洗浄剤)と、腐食のあった比較例4および比較例9の水溶液(洗浄剤)の電位差は、それぞれ0.05V、0.08V、0.19Vであった。以上より、酸化銅(I)と酸化コバルト(II)との酸化還元電位(腐食電位)の電位差が0.05V以下の水溶液(洗浄剤)は、異種金属接触腐食(ガルバニック腐食)の抑制能において「良好」であると判定し、酸化銅(I)と酸化コバルト(II)との酸化還元電位(腐食電位)の電位差が0.05Vを超えてしまう水溶液(洗浄剤)は、異種金属接触腐食(ガルバニック腐食)の抑制能において「不良」であると判定した。
原子間力顕微鏡(AFM)(アサイラムテクノロジー社製MFP-3D-CF)を用いて、評価基板Dにおける酸化銅(I)の膜厚を測定した。次いで、表1の実施例1の水溶液(洗浄剤)および表2の比較例15の水溶液(洗浄剤)を10mLずつ用意し、これらの水溶液(洗浄剤)に評価基板Dを入れ、撹拌しながら室温で1分間浸漬した。浸漬後の評価基板を、原子間力顕微鏡(AFM)(アサイラムテクノロジー社製MFP-3D-CF)を用いて酸化銅(I)の膜厚を測定し、浸漬前と浸漬後との間の膜厚の変化量(エッチング量)を算出した。その結果を表3に示す。
Claims (20)
- 銅配線膜または銅合金配線膜と、コバルト含有膜とを有する半導体基板の化学機械研磨工程の後工程において使用される洗浄剤であって、(A)一般式(1)で示される有機酸、(B-1)一般式(2)で示されるジアミン類、(C)ヒドロキシルアミン誘導体、ならびに(D)一般式(6)で示される脱酸素剤を含有し、pHが10以上の水溶液であることを特徴とする半導体基板用洗浄剤。
(式中、R1は、カルボキシル基、1,2,3-トリヒドロキシプロピル基または3-オキソ-1,2-ジヒドロキシプロピル基を表す。)
(式中、R2およびR3はそれぞれ独立して、水素原子、炭素数1〜4のアルキル基または炭素数6〜10のアリール基を表し、R4は、水素原子、ヒドロキシル基またはヒドロキシル基を有していてもよい炭素数1〜4のアルキル基を表し、R5およびR6はそれぞれ独立して、水素原子または炭素数1〜4のアルキル基を表し、R2とR3、R3とR6、またはR4とR6は、炭素数1〜3のアルキレン鎖を形成していてもよく、mは、0または1を表し、nは、0〜2の整数を表す。)
(式中、R19は、水素原子またはヒドロキシル基を表し、R20は、水素原子またはヒドロキシル基を表し、R21は、水素原子、ヒドロキシル基、カルボキシル基またはプロポキシカルボニル基を表す。ただし、R19〜R21の少なくとも1つはヒドロキシル基を表す。) - (A)一般式(1)で示される有機酸が、酒石酸、グルコン酸およびガラクツロン酸から選ばれるものである、請求項1に記載の洗浄剤。
- (A)一般式(1)で示される有機酸が、酒石酸である、請求項1に記載の洗浄剤。
- (B-1)一般式(2)で示されるジアミン類が、ピペラジンである、請求項1に記載の洗浄剤。
- (C)ヒドロキシルアミン誘導体が、ジエチルヒドロキシルアミンである、請求項1に記載の洗浄剤。
- (D)一般式(6)で示される脱酸素剤が、ピロガロール、ピロカテコール、ヒドロキノン、没食子酸および没食子酸プロピルから選ばれるものである、請求項1に記載の洗浄剤。
- (D)一般式(6)で示される脱酸素剤が、ピロガロールである、請求項1に記載の洗浄剤。
- 洗浄剤が、さらに(E)アルカリ化合物を含有するものである、請求項1に記載の洗浄剤。
- (E)アルカリ化合物が、第4級アンモニウム塩である、請求項10に記載の洗浄剤。
- pHが、10以上13以下である、請求項1に記載の洗浄剤。
- (A)一般式(1)で示される有機酸0.001〜5重量%、(B-1)一般式(2)で示されるジアミン類0.0005〜5重量%、(C)ヒドロキシルアミン誘導体0.01〜25重量%、ならびに(D)一般式(6)で示される脱酸素剤0.0001〜1重量%を含有するものである、請求項1に記載の洗浄剤。
- 洗浄剤が、さらに(E)アルカリ化合物0.1〜5重量%を含有するものである、請求項13に記載の洗浄剤。
- (A)一般式(1)で示される有機酸、(B-1)一般式(2)で示されるジアミン類、(C)ヒドロキシルアミン誘導体、(D)一般式(6)で示される脱酸素剤、(E)アルカリ化合物、ならびに水のみからなる、請求項10に記載の洗浄剤。
- コバルト含有膜が、銅配線膜または銅合金配線膜のバリアメタルである、請求項1に記載の洗浄剤。
- 請求項1に記載の洗浄剤を用いることを特徴とする、銅配線膜または銅合金配線膜と、コバルト含有膜とを有する半導体基板表面の処理方法。
- コバルト含有膜が、銅配線膜または銅合金配線膜のバリアメタルである、請求項17に記載の処理方法。
- 半導体基板が、化学機械研磨後のものである、請求項17に記載の処理方法。
- ベンゾトリアゾールまたはその誘導体に由来する、銅配線膜表面または銅合金配線膜表面の被膜を除去する、請求項17に記載の処理方法。
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IL245473B (en) | 2021-07-29 |
EP3051577B1 (en) | 2017-10-18 |
US9862914B2 (en) | 2018-01-09 |
IL245473A0 (en) | 2016-06-30 |
TW201527520A (zh) | 2015-07-16 |
EP3051577A1 (en) | 2016-08-03 |
US20160272924A1 (en) | 2016-09-22 |
WO2015068823A1 (ja) | 2015-05-14 |
EP3051577A4 (en) | 2016-11-09 |
KR102256773B1 (ko) | 2021-05-27 |
KR20160083885A (ko) | 2016-07-12 |
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