WO2011078982A1 - Post deposition wafer cleaning formulation - Google Patents
Post deposition wafer cleaning formulation Download PDFInfo
- Publication number
- WO2011078982A1 WO2011078982A1 PCT/US2010/059968 US2010059968W WO2011078982A1 WO 2011078982 A1 WO2011078982 A1 WO 2011078982A1 US 2010059968 W US2010059968 W US 2010059968W WO 2011078982 A1 WO2011078982 A1 WO 2011078982A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- solution
- surfactant
- capping layer
- complexing agent
- acid
- Prior art date
Links
- 230000008021 deposition Effects 0.000 title claims description 53
- 238000004140 cleaning Methods 0.000 title abstract description 53
- 239000000203 mixture Substances 0.000 title description 13
- 238000009472 formulation Methods 0.000 title description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 94
- 238000005260 corrosion Methods 0.000 claims abstract description 72
- 230000007797 corrosion Effects 0.000 claims abstract description 72
- 239000008139 complexing agent Substances 0.000 claims abstract description 65
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 53
- 238000009736 wetting Methods 0.000 claims abstract description 14
- 239000010410 layer Substances 0.000 claims description 87
- 239000003989 dielectric material Substances 0.000 claims description 13
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 239000002094 self assembled monolayer Substances 0.000 claims description 9
- 239000013545 self-assembled monolayer Substances 0.000 claims description 9
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 8
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002280 amphoteric surfactant Substances 0.000 claims description 7
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 5
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 5
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical group O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 claims description 5
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical group O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 5
- 235000002949 phytic acid Nutrition 0.000 claims description 5
- 229940068041 phytic acid Drugs 0.000 claims description 5
- 239000000467 phytic acid Substances 0.000 claims description 5
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 5
- 229910000531 Co alloy Inorganic materials 0.000 claims description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 4
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 4
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 4
- XOHQAXXZXMHLPT-UHFFFAOYSA-N ethyl(phosphonooxy)phosphinic acid Chemical compound CCP(O)(=O)OP(O)(O)=O XOHQAXXZXMHLPT-UHFFFAOYSA-N 0.000 claims description 3
- 238000012864 cross contamination Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 65
- 229910021645 metal ion Inorganic materials 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 18
- 238000003795 desorption Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 description 170
- 235000012431 wafers Nutrition 0.000 description 52
- 238000000151 deposition Methods 0.000 description 50
- 239000000047 product Substances 0.000 description 37
- 239000004065 semiconductor Substances 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 17
- 238000012545 processing Methods 0.000 description 17
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- 239000010949 copper Substances 0.000 description 11
- 125000000524 functional group Chemical group 0.000 description 10
- 230000002378 acidificating effect Effects 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 150000007513 acids Chemical class 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
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- -1 Teflon- AF Polymers 0.000 description 5
- 238000005137 deposition process Methods 0.000 description 5
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- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 description 4
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical group [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
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- 150000001875 compounds Chemical class 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 description 3
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- 229910000990 Ni alloy Inorganic materials 0.000 description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
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- 125000000217 alkyl group Chemical group 0.000 description 2
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- 239000000956 alloy Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- UMIVXZPTRXBADB-UHFFFAOYSA-N benzocyclobutene Chemical compound C1=CC=C2CCC2=C1 UMIVXZPTRXBADB-UHFFFAOYSA-N 0.000 description 2
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920003209 poly(hydridosilsesquioxane) Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 230000036962 time dependent Effects 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910018916 CoOOH Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- CPJYFACXEHYLFS-UHFFFAOYSA-N [B].[W].[Co] Chemical compound [B].[W].[Co] CPJYFACXEHYLFS-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000005380 borophosphosilicate glass Substances 0.000 description 1
- YTIVTFGABIZHHX-UHFFFAOYSA-N butynedioic acid Chemical compound OC(=O)C#CC(O)=O YTIVTFGABIZHHX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- NVIVJPRCKQTWLY-UHFFFAOYSA-N cobalt nickel Chemical compound [Co][Ni][Co] NVIVJPRCKQTWLY-UHFFFAOYSA-N 0.000 description 1
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical group CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 description 1
- 229940073507 cocamidopropyl betaine Drugs 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- BZCOSCNPHJNQBP-OWOJBTEDSA-N dihydroxyfumaric acid Chemical compound OC(=O)C(\O)=C(/O)C(O)=O BZCOSCNPHJNQBP-OWOJBTEDSA-N 0.000 description 1
- FFDGPVCHZBVARC-UHFFFAOYSA-N dimethylaminoacetic acid Natural products CN(C)CC(O)=O FFDGPVCHZBVARC-UHFFFAOYSA-N 0.000 description 1
- 108700003601 dimethylglycine Proteins 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
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- 230000002708 enhancing effect Effects 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
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- 238000005805 hydroxylation reaction Methods 0.000 description 1
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- 238000012423 maintenance Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229940078490 n,n-dimethylglycine Drugs 0.000 description 1
- 239000008208 nanofoam Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 238000007704 wet chemistry method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C11D1/88—Ampholytes; Electroneutral 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/042—Acids
-
- 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
-
- 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
-
- 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
- C11D3/2082—Polycarboxylic acids-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
- 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
- C11D3/2086—Hydroxy carboxylic acids-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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/24—Organic compounds containing halogen
- C11D3/245—Organic compounds containing halogen containing fluorine
-
- 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
- C11D3/34—Organic compounds containing sulfur
- C11D3/3409—Alkyl -, alkenyl -, cycloalkyl - or terpene sulfates or sulfonates
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/36—Organic compounds containing phosphorus
- C11D3/362—Phosphates or phosphites
-
- 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
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
-
- 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
Definitions
- the present invention relates to semiconductor fabrication. More specifically, the present invention relates to formulations and methods for cleaning a substrate surface, and more specifically, for removal of corrosion products from a substrate surface.
- Semiconductor devices are used in products such as cell phones, radios, televisions, etc.
- the semiconductor devices include integrated circuits that are connected by conductive wires embedded in insulating material.
- low dielectric constant (low k) interlayer dielectric (ILD) insulating materials With the reduction of semiconductor device size and the use of low dielectric constant (low k) interlayer dielectric (ILD) insulating materials, obtaining reliable semiconductor devices is becoming more and more challenging. In particular, reliability problems occur at interfaces of the copper (Cu) wires and low k ILD material in the form of leakage, electromigration, stress migration, break down voltage, and time dependent dielectric breakdown (TDDB), etc.
- Cu copper
- TDDB time dependent dielectric breakdown
- the dielectric layers are subject to surface contamination during the manufacturing process (e.g., Cu chemical mechanical polishing (CMP) or electroless plating of a metallic capping layer, such as cobalt tungsten phosphorous (CoWP)).
- CMP chemical mechanical polishing
- CoWP cobalt tungsten phosphorous
- Electroless plated caps can be used in electronic devices to improve the electromigration and stress-migration properties of metallization structures. Electroless deposition processes are wet chemical processes. Such processes are often used with wet cleaning processes to clean the substrates. Although liquid solutions are known for numerous cleaning applications, the present inventors have recognized a need for new and/or improved cleaning solution formulations and methods suitable to clean substrates for the manufacture of electronic devices.
- This invention pertains to fabrication of electronic devices. More specifically, the invention pertains to treatment solutions for removing corrosion product from substrate surfaces.
- a treatment solution is configured for application onto a wafer surface which includes a metallic capping layer.
- the treatment solution is effective for rinsing corrosion product of the metallic capping layer from the wafer surface while reducing corrosion of the metallic capping layer.
- the solution includes a surfactant.
- the surfactant is configured to enhance wetting of the wafer surface and to inhibit further corrosion of the capping layer. Additionally, the solution is maintained at a pH of approximately less than 3 during the application onto the wafer surface.
- the surfactant is configured to form a self-assembled monolayer on the metallic capping layer.
- the surfactant is an amphoteric surfactant.
- the concentration of the surfactant in the solution is approximately in the range of 10 ppm to 2000 ppm. In another embodiment, the concentration of the surfactant in the solution is approximately in the range of 300 ppm to 700 ppm.
- the treatment solution further includes a complexing agent.
- the complexing agent is configured to bind to corrosion product which has dissolved off of the wafer surface and into the solution.
- the complexing agent may be configured to prevent redeposition of the corrosion product.
- the complexing agent is selected from the group consisting of hydroxyethyl diphosphonic acid, oxalic acid dihydrate, phytic acid, and pyrophosphoric acid.
- the concentration of the complexing agent is approximately in the range of 0.05 g/L to 20 g/L. In another embodiment, the concentration of the complexing agent is approximately 1 g/L.
- the treatment solution further includes a pH adjusting agent.
- the pH adjusting agent may be configured to reduce the pH of the solution to approximately less than 3 during the application onto the wafer surface.
- the pH adjusting agent is selected from the group consisting of hypophosphorous acid, methane sulfonic acid, sulfuric acid, triflic acid, and trifluoroacetic acid.
- the concentration of the pH adjusting agent is approximately in the range of 0.01 g/L to 20 g/L. In another embodiment, the concentration of the pH adjusting agent is approximately 8 ml/L 50 w/w .
- a treatment solution includes a surfactant and further includes a complexing agent configured to bind to corrosion product which has dissolved off of the wafer surface and into the solution, the complexing agent being selected from the group consisting of hydroxyethyl diphosphonic acid, oxalic acid dihydrate, phytic acid, and pyrophosphoric acid.
- the treatment solution further includes a pH adjusting agent, the pH adjusting agent configured to reduce the pH of the solution to approximately less than 3 during the application onto the wafer surface, the pH adjusting agent selected from the group consisting of hypophosphorous acid, methane sulfonic acid, sulfuric acid, triflic acid, and trifluoroacetic acid.
- the solution does not significantly inhibit the functionality of a recirculated deposition solution used to generate the metallic capping layer in the case of cross-contamination with the deposition solution.
- the wafer surface includes regions of a dielectric material, the regions of the dielectric material having the corrosion product of the capping layer situated thereon prior to application of the solution.
- the dielectric material has a K value of approximately less than or equal to 3.0.
- the metallic capping layer consists of cobalt or a cobalt alloy.
- Figure 1A illustrates a close-up view of a semiconductor interconnect after a CMP step, in accordance with an embodiment of the present invention.
- Figure IB illustrates a close-up view of a semiconductor interconnect after an oxide removal step, in accordance with an embodiment of the present invention.
- Figure 1C illustrates a close-up view of a semiconductor interconnect after a capping step, in accordance with an embodiment of the present invention.
- Figure 2A illustrates a treatment solution applied on a wafer surface, in accordance with an embodiment of the present invention.
- Figure 2B illustrates a treatment solution applied on a wafer surface, in accordance with an embodiment of the present invention.
- Figures 3A and 3B illustrate a mechanism for desorption of corrosion product from the surface of a substrate is illustrated, in accordance with an embodiment of the invention.
- Figure 4 illustrates a treatment solution for cleaning corrosion product from the surface of a substrate, in accordance with an embodiment of the invention.
- Figure 5A illustrates a cross-sectional view of a processing chamber during a deposition process, in accordance with an embodiment of the present invention.
- Figure 5B illustrates a cross-sectional view of a processing chamber during a cleaning process, in accordance with an embodiment of the present invention.
- Figure 6 illustrates an example of a pattern for aiding in detection of the outer frame of a display, in accordance with an embodiment of the invention.
- the present invention pertains to interconnect metallization that uses an electrically conductive metal with a cap and a dielectric forming a damascene metallization structure for electronic devices such as integrated circuits. More specifically, the present invention is directed toward cleaning solution formulations for cleaning substrates for electronic devices.
- the interconnect metallization layers include a dielectric and a metal, such as copper.
- the metallization layers for the integrated circuits include copper for metal lines formed into damascene and/or dual damascene dielectric structures.
- the copper metal lines have electrolessly deposited caps.
- Some preferred caps are multi-element alloys such as cobalt alloy, cobalt-tungsten alloy, cobalt-tungsten-phosphorous-boron alloy, cobalt- nickel alloy, and nickel alloy.
- the dielectric is a low k dielectric material such as a carbon doped silicon oxide (SiOC:H).
- SiOC:H carbon doped silicon oxide
- cleaning solutions according to embodiments of the present invention can be used to clean substrates after deposition of the cap.
- the cleaning solutions may be capable of removing contaminants such as ions left on the dielectric surface between the capped copper interconnect structures. The removal of such contaminants may produce results such as improved leakage current properties, improved voltage breakdown properties, and improved time-dependent dielectric breakdown performance.
- cleaning solutions according to embodiments of the present invention may be used in conjunction with wet transfer systems, wherein a wafer is transferred or otherwise transitioned from one processing step to another while maintained in a wet state (i.e. with a solution such as the presently described cleaning solutions present on the surface of the wafer).
- the cleaning solution may act to reduce or prevent contamination of the wafer surface and other problems associated with dry transfer of a wafer, such as contamination by droplets, airborne particles, and the attendant complexities of drying and rewetting the wafer surface, etc. Additional details regarding wet transfer systems are provided with reference to U.S. provisional patent application no.
- FIG. 1A a close up view of a semiconductor interconnect 10 after a CMP step is shown, in accordance with an embodiment of the present invention.
- a semiconductor wafer 12 may be of a material such as silicon, gallium arsenide, diamond, etc.
- the semiconductor wafer 12 has been processed to form semiconductor elements, such as transistors, in and above it.
- the dielectric layer 14 is of dielectric materials such as silicon oxide (SiO x ), tetraethoxysilane (TEOS), borophosphosilicate (BPSG) glass, etc. with dielectric constants from about 4.2 to 3.9 or low dielectric constant dielectric materials such as fluorinated tetraethoxysilane (FTEOS), hydrogen silsesquioxane (HSQ), benzocyclobutene (BCB), carbon-doped silicon dioxide, etc. with dielectric constants below about 3.9.
- Ultra-low dielectric constant dielectric materials are dielectric materials having dielectric constants below about 2.5.
- Examples of such materials include commercially available Teflon, Teflon- AF, Teflon microemulsion, polimide nanofoams, silica aerogels, silica xerogels, and mesoporous silica.
- the dielectric layer 14 has been processed to have a channel or via formed therein, which is lined with a barrier layer 16.
- the barrier layer 16 may be composed of materials such as tantalum (Ta), tantalum nitride (TaN), titanium (Ti), tungsten (W), alloys thereof, and compounds thereof.
- the barrier layer 16 is filled with a conductor 18 such as copper (Cu), aluminum (Al), gold (Au), silver (Ag), alloys thereof, and compounds thereof.
- a conductor 18 such as copper (Cu), aluminum (Al), gold (Au), silver (Ag), alloys thereof, and compounds thereof.
- FIG. IB a close-up view of the semiconductor interconnect 10 after an oxide removal step is shown, in accordance with an embodiment of the present invention.
- the oxide removal step removes the oxide layer 20 of Figure 1 A.
- FIG. 1C therein is shown a close up view of the semiconductor interconnect 10 after a capping step according to a first embodiment of the present invention.
- a capping layer 22 is then deposited on the barrier layer 16 and the conductor 18.
- the capping layer 22 can be a metal or metal compound such as cobalt (Co) or cobalt tungsten phosphorous (CoWP), cobalt tungsten boron (CoWB), cobalt tungsten phosphorous boron (CoWPB), etc., deposited by electroless deposition.
- a treatment solution 30 is shown, in accordance with an embodiment of the present invention.
- the treatment solution 30 includes a surfactant 32 that also acts as a corrosion inhibitor, a complexing agent 34, and a pH adjuster 36.
- the cleaning solution is an aqueous solution.
- other embodiments of the present invention may be non-aqueous cleaning solutions wherein a non-aqueous liquid is used instead of water.
- the treatment solution 30 is applied to the surface of a substrate 40.
- the exposed surface of the substrate 40 includes regions of a dielectric 14 and regions of a metallic capping layer 20.
- corrosion of the capping layer 22 may occur.
- the resulting corrosion product 38 may consist of various oxides and hydroxylated metal ions which are adsorbed on the surface of the substrate 40.
- the resulting corrosion products of cobalt may include various hydroxides and oxides such as Co(OH) 2 , Co(OH) 3 , CoOOH, CoO, Co 2 0 3 , Co 3 0 4 , etc.
- treatment solutions according to embodiments of the present invention have a pH of approximately less than or equal to 3.
- the pH of the treatment solution may be less than or equal to 2 for some embodiments.
- Some embodiments of the present invention include the treatment solution having a pH of about 1.8 to 1.9. In certain embodiments, the pH may be approximately 1.85.
- the low pH of the treatment solution promotes desorption of the corrosion product 38 from the surface of the substrate 40, due to the effects of the high concentration of hydrogen ions.
- the high concentration of hydrogen ions causes the surface of the substrate 40 to be positively charged.
- the available hydrogen ions promote a dehydration reaction with hydroxylated metal ions, thus releasing the metal ions; and as the metal ions are positively charged, they are electrostatically repelled from the positively charged surface of the substrate 40.
- the treatment solution 30 includes a surfactant 32 which also acts as a corrosion inhibitor.
- the treatment solution 30 may contain more than one surfactant.
- the surfactant 32 reduces the surface tension of the treatment solution 30, thereby promoting adequate wetting of both the dielectric and capping regions of the substrate 40 when applied. By promoting wetting of the substrate 40, the surfactant 32 thus provides for even cleaning of the substrate surface, as well as protection of the substrate surface from droplets and airborne particles.
- One of the functions of the surfactant 32 may be to substantially protect the capping layer 22 and inhibit the corrosion of the capping layer 22 in the treatment solution 30.
- the treatment solutions according to embodiments of the present invention are configured so as to clean the substrate with negligible or substantially no reduction in the thickness of the capping layer 22.
- the one or more surfactants may be included in embodiments of the present invention for this purpose.
- the surfactant 32 may be configured to selectively bind to the capping layer 22 at low pH. More specifically, the polar end of the surfactant 32 binds to the capping layer 22, while the hydrophobic end of the surfactant is oriented away from the capping layer 22.
- the surfactant 32 thus forms a protective layer 42 (as shown at Figure 2B) on the capping layer 22, which inhibits the corrosion of the capping layer 22 due to the presence of the treatment solution 30 and its low pH, without affecting the dielectric regions of the substrate 40.
- Embodiments of the invention include the surfactant 32 being configured to form a self- assembled monolayer (SAM) on the capping layer 22, wherein the polar ends of the surfactant molecules are directed towards the capping layer 22 and the hydrophobic tails are directed away from the capping layer 22.
- SAM self- assembled monolayer
- the surfactant 32 may be configured so as to remain bound to the capping layer 22 until the pH is raised to alkaline levels. Thus, during a subsequent rinse step with DI water (during which it is possible to further corrode the capping layer 22), the capping layer 22 remains protected by the surfactant layer 42. However, when an alkaline solution such as a deposition solution is applied to the surface of the substrate 40, then the surfactant layer 42 is disrupted and dissociates from the capping layer 22.
- the surfactant may be configured so as to be compatible with a deposition solution for the capping layer. In other words, when limited amounts of the surfactant contaminate the deposition solution, the functionality of the deposition solution is not significantly inhibited.
- a list of surfactants for embodiments of the present invention includes, but is not limited to, anionic surfactants, cationic surfactants, nonionic surfactants, amphoteric surfactants, zwitterions and combinations thereof.
- Some of the surfactants for some embodiments of the present invention are surfactants that have sulfate or sulfonate head groups.
- the surfactant preferably consists of an amphoteric surfactant having an acidic functional group.
- the amphoteric surfactant may include an acidic functional group for purposes of enhancing compatibility with an alkaline deposition solution for the capping layer, and for affecting the pH of the treatment solution.
- the acidic functional group may be configured so as to allow the protective layer formed by the surfactant on the capping layer to be disrupted when exposed to an alkaline deposition solution.
- the surfactant may be a betaine, or a zwitterion of a substituted alkyl derivative of N, N-dimethyl glycine.
- the surfactant is cocamidopropyl betaine.
- the surfactant may contain alkyl, fluoroalkyl, or partially fluorinated alkyl groups.
- Surfactants in accordance with embodiments of the invention may include an acidic functional group.
- the acidic functional group may be one of various acidic functional groups, such as carboxyl, phosphate, phosphite, sulfonate, etc.
- Treatment solutions according to some embodiments of the present invention include one or more surfactants present in amounts ranging from about 10 ppm to about 2000 ppm for the active component of the formulation for each surfactant. The molecular weight of the surfactant is not always known.
- an effective amount of surfactant is provided in treatment solutions according to the present invention.
- the amount of surfactant in the treatment solution is selected so that the solution is effective in cleaning the substrate and providing satisfactory prevention of corrosion of the cap.
- the treatment solutions contain one or more surfactants with each of the surfactants present in the treatment solution in a concentration range of about 10 parts per million (ppm) to about 2000 ppm.
- the surfactant is present at a concentration between about 300 ppm and about 700 ppm and all sub-ranges subsumed therein.
- the configuration and concentration of the surfactant is selected so as to provide the desired pH level for the treatment solution.
- the pH level may be adjusted by the presence of the surfactant so as to promote desorption of corrosion product from the surface of the wafer.
- Treatment solutions according to embodiments of the present invention may optionally also include a complexing agent 34.
- the complexing agent 34 according to some embodiments of the present invention includes functional groups so as to be capable of forming complexes with metal ions.
- the complexing agent 34 acts to stabilize the metal ions in solution. This serves to prevent the metal ions from redepositing onto the wafer surface. Such redeposition may be prone to occurring during subsequent steps (such as a DI water rinse step) when the pH may increase and cause hydroxylation and oxidation of the metal ions and consequent redeposition of corrosion product on the surface of the wafer.
- embodiments of the invention include the complexing agent 34 being configured so as to effectively bind to metal ions across a broad range of pH values, including pH values of both less than and greater than 3.
- the corrosion product 38 is desorbed from the surface of the substrate 40, and subsequently forms a complex 44 with the complexing agent 34.
- the complexing agent 34 may also have one or more functional groups so as to be capable of adjusting the pH of the cleaning solution. More specifically, the complexing agent is also capable of contributing to and affecting the pH of the solution so as to maintain the pH of the cleaning solution at or below about 3.
- a list of complexing agents capable of affecting the pH of the solution includes, but is not limited to, phytic acid, oxalic acid (CAS # [6153-56-6]), pyrophosphoric acid, hydroxyethylidene diphosphonic acid (CAS # [2809-21-4] also known as etidronic acid, ethane- 1 -hydroxy- 1,1 -diphosphonic acid, or HEDPA), phytic acid, malonic acid, maleic acid, and mixtures thereof.
- cleaning solutions according to embodiments of the present invention contain an effective amount of complexing agent capable of functioning to form complexes with the metal ions removed from the surface of the substrate and to contribute to the maintenance of the pH at the desired level (so as to facilitate the removal of metal ions from the surface of the substrate).
- the specific amount required depends upon the properties of the complexing agent.
- the concentration of complexing agent ranges from about 0.05 g/L to 20 g/L. In other embodiments the concentration of complexing agent may range from approximately 0.5 g/L to 2 g/L, and all subranges included therein.
- Treatment solutions in accordance with embodiments of the invention may optionally also include a pH adjuster 36 (or multiple pH adjusters).
- the pH adjusters in cleaning solutions according to some embodiments of the present invention have functional groups so as to be capable of maintaining the pH of the cleaning solution at a desired level.
- the desired pH level may be less than about 3 or 2.
- this may mean that the pH adjuster 36 has functional groups for producing an acidic cleaning solution.
- the pH adjuster may also have capabilities as a complexing agent.
- a list of pH adjusters for embodiments of the present invention includes, but is not limited to, sulphuric acid, sulfonic acids such as but not limited to methanesulfonic acid, benzene sulfonic acid, and triflic acid, hypophosphorous acid, oxalic acid, halogenated carboxylic acids such as but not limited to trifluoroacetic acid, triflic acid, acetylenedicarboxylic acid, squaric acid, dihydroxyfumaric acid, maleic acid, and mixtures thereof.
- the pH adjuster may include one or more acids having pK a about equal to or less than 2, where pK a is the negative logarithm of the acid ionization constant, K a , and the one or more acids being capable so as to adjust the cleaning solution to the desired acidic pH.
- the pH adjuster may include one or more acids having pK a equal to or less than 1.5 and the one or more acids being capable so as to adjust the cleaning solution to the desired acidic pH.
- the pH adjuster is configured so as to be compatible with a deposition solution.
- the pH adjuster is selected such that in the case of contamination of the deposition solution by the treatment solution, the functionality of the deposition solution is not significantly inhibited.
- cleaning solutions according to embodiments of the present invention contain an effective amount of pH adjuster so as to maintain the pH at the desired level.
- the specific amount required depends upon the properties of the pH adjuster and the desired pH level.
- the amount of pH adjuster is between about 0.01 g/L and 20 g/L.
- the concentration of pH adjuster ranges from approximately 3 g/L to 5 g/L.
- the inclusion of the pH adjuster may be a cost-effective way of adjusting the pH level of the treatment solution to the desired level.
- either or both of the surfactant or the complexing agent may function as agents which lower the pH of the solution.
- a relatively inexpensive pH adjuster may be chosen so as to adjust the pH to the desired level at lower cost than would be possible with a solution consisting of only the surfactant and the complexing agent.
- Treatment solutions according to embodiments of the present invention may have any one of numerous specific formulations.
- the treatment solution includes one or more surfactants.
- the surfactant is configured to promote wetting of the wafer surface and to protect the capping layer from corrosion, while simultaneously producing a low pH in order to effect desorption of corrosion product from the surface of the wafer.
- the specific configuration and concentration of the surfactant may be chosen so as to provide sufficiently low pH as well as adequate inhibition of corrosion of the capping layer.
- the surfactant may be configured so as to be compatible with a deposition solution for the capping layer, in the case of contamination of the deposition solution with the treatment solution.
- the treatment solution includes both a surfactant and a pH adjuster.
- the surfactant promotes wetting of the wafer surface and inhibits corrosion of the capping layer, but by itself does not produce the desired pH level for the treatment solution.
- the pH adjuster is configured to adjust the pH of the solution to the desired level (e.g. less than 3.0).
- the configuration and specific concentrations of the surfactant and the pH adjuster may be chosen so as to provide adequate wetting, sufficient inhibition of corrosion of the capping layer, and sufficiently low pH.
- the surfactant and the pH adjuster may be configured so as to be compatible with a deposition solution for the capping layer, in the case of contamination of the deposition solution with the treatment solution.
- the treatment solution includes both a surfactant and a complexing agent.
- the surfactant is configured to promote wetting of the wafer surface and inhibit corrosion of the capping layer.
- the complexing agent is configured to bind to metal ions in solution so as to prevent their deposition (or redeposition) onto the wafer surface.
- Either or both of the surfactant and the complexing agent may also be configured so as to produce the desired pH level for the treatment solution.
- the specific configuration and concentrations of the surfactant and complexing agent may be chosen so as to provide adequate wetting, adequate inhibition of corrosion of the capping layer, sufficient prevention of redeposition of corrosion product, and the desired pH level.
- the surfactant and complexing agent may be selected so as to be compatible with a deposition solution for the capping layer, in the case of contamination of the deposition solution with the treatment solution.
- the treatment solution includes a surfactant, a complexing agent, and a pH adjuster.
- the surfactant is configured to promote wetting of the wafer surface and to inhibit corrosion of the capping layer.
- the complexing agent is configured to bind to metal ions in the treatment solution.
- the pH adjuster is configured to adjust the pH of the treatment solution to the desired level. Either of the surfactant or the complexing agent, or both, may also be configured to affect the pH level.
- the specific configurations and concentrations of the surfactant, the complexing agent, and the pH adjuster may be chosen so as to provide adequate wetting, adequate inhibition of corrosion of the capping layer, sufficient prevention of redeposition of corrosion product onto the wafer surface, and the desired pH level. Additionally, the surfactant, complexing agent, and the pH adjuster may be selected so as to be compatible with a deposition solution for the capping layer, in the case of contamination of the deposition solution with the treatment solution.
- a substrate surface 50 includes a dielectric such as silicon dioxide.
- a dielectric such as silicon dioxide.
- other dielectrics and surface materials may compose the substrate surface 50.
- Silicon dioxide as one example, has a point of zero charge of approximately pH 2 to 3. Thus, at a pH of approximately 2 to 3, the substrate surface 50 is neutrally charged.
- the exposed hydroxyl groups 52 of the silicon dioxide surface exhibit a net zero charge.
- metallic corrosion product such as metal hydroxides which precipitate from solution
- metallic corrosion product may be present on the substrate surface 50.
- steps such as a rinse step with DI water to halt the deposition process and to remove the deposition solution.
- steps may also promote corrosion of the capping layer, resulting in the formation of corrosion product.
- the corrosion product 54 includes Co(OH)2 which has resulted from corrosion of a cobalt-containing capping layer.
- the cobalt ions form aqua ions in aqueous solution and undergo a hydrolysis reaction to form the cobalt hydroxide which precipitates onto the substrate surface 50.
- the corrosion product may include various metal hydroxides and complexes which result from corrosion of metallic surfaces.
- the corrosion product 54 is adsorbed on the substrate surface 50.
- the released metal ion (Co 2+ in the illustrated example) is electrostatically repelled from the positively charged substrate surface.
- the low pH of approximately less than 2 facilitates the desorption of corrosion product 54 from the substrate surface 50.
- a treatment solution 60 is shown for cleaning corrosion product from the surface of a substrate, in accordance with an embodiment of the invention.
- the surface of the substrate includes regions of a dielectric 70 and a capping layer 74.
- the capping layer 74 consists of cobalt or a cobalt alloy, and protects a conductive layer, such as a copper layer 72 from oxidation and electromigration.
- the treatment solution 60 includes a surfactant 62, a complexing agent 64, and a pH adjuster 66.
- the surfactant 62 promotes wetting to facilitate coverage of the substrate surface by the treatment solution 60.
- the surfactant 62 is configured to selectively bind to the capping layer 74, and form a self-assembled monolayer so as to protect the capping layer 74 from corrosion.
- the treatment solution is configured to have a pH of approximately less than 2 to 3.
- a low pH promotes desorption of corrosion product (such as metal hydroxide) which is adsorbed on the surface of the dielectric 70. The desorption may occur via a dehydration reaction as illustrated at reference numeral 68.
- the low pH of the treatment solution would also promote further corrosion of the capping layer 74; however, the surfactant SAM on the capping layer acts to inhibit such corrosion as would otherwise occur due to the low pH of the treatment solution.
- the desorption of the corrosion product from the substrate surface causes metal ions to be released into the treatment solution.
- the complexing agent 64 binds to the metal ions, forming complexes which stabilize the metal ions in the treatment solution and inhibit their reprecipitation as hydroxides onto the surface of the substrate, as would otherwise likely occur when the pH is adjusted upwards in subsequent steps (e.g. a rinse step or subsequent processing step with a higher pH liquid such as DI water).
- the complexing agent is configured to bind to metal ions at low pH, such as a pH of approximately less than 2 to 3. Additionally, the complexing agent may be an acidic compound, thereby affecting the overall pH of the treatment solution.
- reaction may proceed according to the following formula:
- a c is a complexing agent configured to bind to cobalt ions.
- the treatment solution 60 may also include an optional pH adjuster 66.
- the pH adjuster 66 is provided so as to adjust the pH of the treatment solution to the desired level.
- the complexing agent 64 may be an acid, in some embodiments it may be undesirable to concentrate the complexing agent 64 to provide the desired pH level due to efficiency and cost considerations. Therefore, it may be advantageous to utilize a pH adjuster 66 in order to more efficiently achieve the desired pH level for promoting desorption of corrosion product from the substrate surface.
- the treatment solution 60 does not include a pH adjuster. Rather, the complexing agent or surfactant is configured as an acidic compound and concentrated to an appropriate concentration so as to provide the desired pH level.
- the treatment solution 60 in accordance with embodiments of the invention may be configured so as to be compatible with a deposition solution for the capping layer in the case of contamination of the deposition solution with the treatment solution. Such contamination may be of concern when the application of the deposition and the cleaning solution take place in the same device, and the deposition solution is recirculated. Thus, it may be desirable to configure the treatment solution so that the functionality of the deposition solution is not substantially inhibited by inadvertent contamination with the treatment solution.
- each of the components of the treatment solution may be configured so as to be compatible with the deposition solution.
- the surfactant, the complexing agent, and the pH adjuster may be configured so as to not substantially inhibit the functionality of the deposition solution.
- the surfactant is configured so as to selectively bind to the metallic capping layer at low pH.
- the surfactant forms a surfactant SAM on the capping layer which may remain on the capping layer even at neutral pH.
- the surfactant may be configured so that the surfactant SAM is disrupted at alkaline pH.
- the deposition solution may be configured to have an alkaline pH, and as such causes disruption of the surfactant SAM when applied to the substrate surface. In this manner, the surfactant does not hinder the activity of the deposition solution.
- the complexing agent is configured so as to bind to metallic ions in solution only at low pH.
- the complexing agent of the treatment solution contaminates the deposition solution, the complexing agent is rendered inactive by the alkaline pH of the deposition solution.
- the complexing agent does not interfere with metallic ions present in the deposition solution, and so does not substantially inhibit their functionality in the deposition solution.
- the pH adjuster is configured so as to not substantially interfere with the functionality of the deposition solution. In some embodiments, this may be accomplished by selecting the pH adjuster to be an acid which is already present in the deposition solution.
- FIG. 5A illustrates the wafer processing chamber 80 during a deposition process.
- the processing chamber 80 includes a wafer support 82 for holding a wafer 83, the wafer support 82 being configured to rotate the wafer 83 as various processing solutions are applied to the surface of the wafer 83.
- the processing chamber 80 also includes an upper divider 84 and a lower divider 86.
- the upper divider 84 is movable so as to form a seal with the lower divider 86.
- Figure 5A illustrates the processing chamber 80 in a "closed" position wherein the upper divider 84 is sealed against the lower divider 86.
- the upper divider 84 and the lower divider 86 together define an inner chamber 88 and an outer chamber 92.
- the inner chamber 88 contains the wafer support 82 and the wafer 83.
- FIG. 5A illustrates the processing chamber 80 during a deposition process, wherein the processing chamber 80 is in a closed position, and a deposition solution is being applied to the surface of the wafer 83.
- the deposition solution flows off the edges of the wafer 83. Because the upper divider 84 and lower divider 86 are sealed together, the deposition solution stays within the inner chamber 88, and flows downward, and exits the inner chamber via inner chamber drain 90.
- the deposition solution flows to a deposition storage 96, from which the deposition solution is recirculated back into the wafer processing chamber 80.
- FIG. 5B illustrates the processing chamber 80 during a cleaning process, wherein the processing chamber 80 is in an open position, such that the upper divider 84 is raised and separated from the lower divider 86.
- a cleaning solution is being applied to the surface of the wafer 83.
- the wafer 83 is rotated by the wafer support 82, the majority of the cleaning solution flows off of the edges of the wafer 83 and into the outer chamber 92, and exits the outer chamber 92 via outer chamber drain 94.
- some of the cleaning solution may fall within the inner chamber 88, and therefore contaminate the deposition solution as it is recirculated. For this reason, it is desirable to formulate a cleaning solution in accordance with embodiments of the present invention, such that the cleaning solution is compatible with the deposition solution in the event of such contamination.
- a surfactant is provided.
- the surfactant may be configured to enhance wetting of a substrate, as well as inhibit corrosion of a capping layer.
- the surfactant is an amphoteric surfactant.
- a complexing agent is provided.
- the complexing agent may be configured to bind to corrosion product of the capping layer which is released from dielectric regions of the surface of the substrate.
- a pH adjuster is provided.
- the pH adjuster is configured to adjust the pH of a mixture of the surfactant, the complexing agent, and the pH adjuster, to a desired level.
- the desired level may be that level of pH at which corrosion product is desorbed from the surface of the substrate.
- the mixture including the surfactant, the complexing agent, and the pH adjuster is formed.
- the mixture is applied to the surface of the substrate/wafer for a period of time, so as to accomplish removal of corrosion product from the substrate surface.
- the process of cleaning substrates using cleaning solutions according to embodiments of the present invention can be performed using a brush to apply the cleaning solution to the substrate.
- the process can be performed by applying the cleaning solution to the substrate by methods such as dipping or immersing the substrate into the cleaning solution, such as rinsing the substrate with the cleaning solution, such as spraying the cleaning solution onto the substrate, and such as applying the cleaning solution using a proximity head.
- the cleaning efficiency of cleaning solutions according to embodiments of the present invention can be enhanced further by using processes such as applying ultrasonic or megasonic energy to the substrate during cleaning and/or by using elevated temperatures during the cleaning.
- the cleaning solutions are used at temperatures in the range from about 5°C to about 90°C.
- Cleaning solutions according to embodiments of the present invention can be applied to clean substrates after deposition of a cap layer.
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Abstract
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Priority Applications (4)
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JP2012546015A JP5879269B2 (en) | 2009-12-23 | 2010-12-10 | Post-deposition wafer cleaning compound |
SG2012045845A SG181854A1 (en) | 2009-12-23 | 2010-12-10 | Post deposition wafer cleaning formulation |
CN201080058890.1A CN102792431B (en) | 2009-12-23 | 2010-12-10 | Post-depositional chip cleaning formula |
KR1020127016399A KR101801413B1 (en) | 2009-12-23 | 2010-12-10 | Post deposition wafer cleaning formulation |
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US28998209P | 2009-12-23 | 2009-12-23 | |
US61/289,982 | 2009-12-23 |
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PCT/US2010/059968 WO2011078982A1 (en) | 2009-12-23 | 2010-12-10 | Post deposition wafer cleaning formulation |
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US (2) | US8921296B2 (en) |
JP (1) | JP5879269B2 (en) |
KR (1) | KR101801413B1 (en) |
CN (2) | CN105820886A (en) |
SG (2) | SG10201408636XA (en) |
TW (1) | TWI583785B (en) |
WO (1) | WO2011078982A1 (en) |
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JP6044337B2 (en) * | 2012-12-28 | 2016-12-14 | 三菱瓦斯化学株式会社 | Etching solution and etching method for oxide of indium and gallium and oxygen or indium and gallium, zinc and oxygen |
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JP6350008B2 (en) * | 2014-06-20 | 2018-07-04 | 三菱瓦斯化学株式会社 | Etching solution and etching method of oxide containing at least indium, gallium, zinc and silicon |
CN106463368B (en) * | 2014-07-25 | 2020-06-16 | 英特尔公司 | Tungsten alloy in semiconductor device |
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Also Published As
Publication number | Publication date |
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US20150111805A1 (en) | 2015-04-23 |
SG10201408636XA (en) | 2015-02-27 |
CN102792431A (en) | 2012-11-21 |
CN102792431B (en) | 2016-04-27 |
JP2013515855A (en) | 2013-05-09 |
TW201125970A (en) | 2011-08-01 |
US8921296B2 (en) | 2014-12-30 |
JP5879269B2 (en) | 2016-03-08 |
US20110152151A1 (en) | 2011-06-23 |
SG181854A1 (en) | 2012-07-30 |
KR101801413B1 (en) | 2017-12-20 |
TWI583785B (en) | 2017-05-21 |
KR20120107975A (en) | 2012-10-04 |
US9476018B2 (en) | 2016-10-25 |
CN105820886A (en) | 2016-08-03 |
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