CN113430070B - 一种CoWP兼容性的半水基清洗液、其制备方法及应用 - Google Patents
一种CoWP兼容性的半水基清洗液、其制备方法及应用 Download PDFInfo
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- CN113430070B CN113430070B CN202010209656.XA CN202010209656A CN113430070B CN 113430070 B CN113430070 B CN 113430070B CN 202010209656 A CN202010209656 A CN 202010209656A CN 113430070 B CN113430070 B CN 113430070B
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- semi
- cleaning solution
- water
- acid
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- 238000004140 cleaning Methods 0.000 title claims abstract description 92
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 39
- -1 alcohol amine Chemical class 0.000 claims abstract description 25
- 230000007797 corrosion Effects 0.000 claims abstract description 25
- 238000005260 corrosion Methods 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 239000002280 amphoteric surfactant Substances 0.000 claims abstract description 15
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 15
- 239000002738 chelating agent Substances 0.000 claims abstract description 14
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 12
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 5
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- 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 5
- 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 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000012964 benzotriazole Substances 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- GIAFURWZWWWBQT-UHFFFAOYSA-N 2-(2-aminoethoxy)ethanol Chemical compound NCCOCCO GIAFURWZWWWBQT-UHFFFAOYSA-N 0.000 claims description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical group C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims description 4
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- 239000011737 fluorine Substances 0.000 claims description 4
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- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 3
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- JQZUMFHYRULBEN-UHFFFAOYSA-N diethyl(methyl)silicon Chemical compound CC[Si](C)CC JQZUMFHYRULBEN-UHFFFAOYSA-N 0.000 claims description 3
- 229940102253 isopropanolamine Drugs 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
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- 238000004519 manufacturing process Methods 0.000 claims description 2
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims 1
- 239000000075 oxide glass Substances 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 14
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- 125000000217 alkyl group Chemical group 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
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- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 description 2
- JMTMSDXUXJISAY-UHFFFAOYSA-N 2H-benzotriazol-4-ol Chemical compound OC1=CC=CC2=C1N=NN2 JMTMSDXUXJISAY-UHFFFAOYSA-N 0.000 description 2
- KFJDQPJLANOOOB-UHFFFAOYSA-N 2h-benzotriazole-4-carboxylic acid Chemical compound OC(=O)C1=CC=CC2=NNN=C12 KFJDQPJLANOOOB-UHFFFAOYSA-N 0.000 description 2
- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 description 2
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- NPZTUJOABDZTLV-UHFFFAOYSA-N hydroxybenzotriazole Substances O=C1C=CC=C2NNN=C12 NPZTUJOABDZTLV-UHFFFAOYSA-N 0.000 description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- IIAPBJPXNIYANW-UHFFFAOYSA-M ethyl-(2-hydroxyethyl)-dimethylazanium;hydroxide Chemical compound [OH-].CC[N+](C)(C)CCO IIAPBJPXNIYANW-UHFFFAOYSA-M 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 1
- 229960001867 guaiacol Drugs 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 229960000448 lactic acid Drugs 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229960002510 mandelic acid Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- IBKQQKPQRYUGBJ-UHFFFAOYSA-N methyl gallate Natural products CC(=O)C1=CC(O)=C(O)C(O)=C1 IBKQQKPQRYUGBJ-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- KTDMLSMSWDJKGA-UHFFFAOYSA-M methyl(tripropyl)azanium;hydroxide Chemical compound [OH-].CCC[N+](C)(CCC)CCC KTDMLSMSWDJKGA-UHFFFAOYSA-M 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229960003540 oxyquinoline Drugs 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000473 propyl gallate Substances 0.000 description 1
- 235000010388 propyl gallate Nutrition 0.000 description 1
- 229940075579 propyl gallate Drugs 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229940117986 sulfobetaine Drugs 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- HPWUYZIJILJHNG-UHFFFAOYSA-M tributyl(2-hydroxyethyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](CCO)(CCCC)CCCC HPWUYZIJILJHNG-UHFFFAOYSA-M 0.000 description 1
- FYFNFZLMMGXBMT-UHFFFAOYSA-M tributyl(ethyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](CC)(CCCC)CCCC FYFNFZLMMGXBMT-UHFFFAOYSA-M 0.000 description 1
- QVOFCQBZXGLNAA-UHFFFAOYSA-M tributyl(methyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](C)(CCCC)CCCC QVOFCQBZXGLNAA-UHFFFAOYSA-M 0.000 description 1
- GRNRCQKEBXQLAA-UHFFFAOYSA-M triethyl(2-hydroxyethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CCO GRNRCQKEBXQLAA-UHFFFAOYSA-M 0.000 description 1
- JAJRRCSBKZOLPA-UHFFFAOYSA-M triethyl(methyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(CC)CC JAJRRCSBKZOLPA-UHFFFAOYSA-M 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- 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
- C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- 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
- C11D3/26—Organic compounds containing nitrogen
- C11D3/28—Heterocyclic compounds containing nitrogen in the ring
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- 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
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
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- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/90—Betaines
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D2111/10—Objects to be cleaned
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Abstract
本发明公开了一种CoWP兼容性的半水基清洗液、其制备方法及应用。本发明的半水基清洗液由下述原料制得,所述的原料包括以下质量分数的组分:5%‑70%的溶剂、0.5%‑20%的醇胺、0.1%‑20%的季铵碱、0.1%‑15%的缓蚀剂、0.1%‑10%的钝化剂、0.01%‑20%的螯合剂、0.1%‑10%的两性表面活性剂、0.1%‑10%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。本发明的半水基清洗液能适应CoWP等金属环境,对多种金属及电介质的缓蚀性强,清洗效果佳。
Description
技术领域
本发明涉及一种CoWP兼容性的半水基清洗液、其制备方法及应用。
背景技术
在芯片制造技术中,当线宽技术节点达到32nm及以下时,可能会引入CoWP等金属作为铜互联金属线的封盖层,以避免全铜互联金属线结构的电迁移等可靠性损失。但引入铜以外的金属,尤其是钴和钨,会对清洗制程(等离子刻蚀后残余物和/或灰化后残余物清洗)带来影响,以往适用于铜互联清洗的清洗液,往往可能会带来钴和钨的腐蚀及清洗异常。为了适应新的技术节点,需开发全新的清洗液。
另外,目前在等离子刻蚀残余物清洗液领域,市场上大多数清洗液均为水基含氟或含羟胺类清洗液,这类清洗液难以适用于多种金属及电介质共存的清洗环境,缓蚀性能存在缺陷,因此开发缓蚀性强的无氟无羟胺清洗液是市场需求所在。
发明内容
本发明所要解决的技术问题是克服现有的清洗液难以适用于多种金属及电介质共存的清洗环境、缓蚀性差等缺陷,而提供了一种CoWP兼容性的半水基清洗液、其制备方法及应用。本发明的半水基清洗液能适应CoWP等金属环境,对多种金属及电介质的缓蚀性强,清洗效果佳。
本发明通过以下技术方案来解决上述技术问题。
本发明提供了一种半水基清洗液,其由下述原料制得,所述的原料包括以下质量分数的组分:5%-70%的溶剂、0.5%-20%的醇胺、0.1%-20%的季铵碱、0.1%-15%的缓蚀剂、0.1%-10%的钝化剂、0.01%-20%的螯合剂、0.1%-10%的两性表面活性剂、0.1%-10%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比;
其中,所述的溶剂为甘油酸;
所述的钝化剂为三((5-(吡唑-4-基)吡啶-2-基)甲基);
所述的非离子型表面活性剂为EO-PO聚合物L42、EO-PO聚合物L43和EO-PO聚合物L44中的一种或多种。
所述的半水基清洗液中,所述的溶剂的质量分数可为10%-60%,优选20%-40%(例如20%、25%、40%),所述的质量分数为所述的溶剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的醇胺可为本领域常规使用的醇胺,优选单乙醇胺、二乙醇胺、三乙醇胺、2-氨基乙醇、1-氨基-2-丙醇、1-氨基-3-丙醇、2-(2-氨基乙氧基)乙醇、2-(2-氨基乙基氨基)乙醇、2-(2-氨基乙基氨基)乙胺、三甲醇胺、二甘醇胺、二内醇胺、正丙醇胺、异丙醇胺、二异丙醇胺、三异丙醇胺和二乙醇单异丙醇胺中的一种或多种,更优选单乙醇胺、三乙醇胺、二甘醇胺和异丙醇胺中的一种或多种。
所述的半水基清洗液中,所述的醇胺的质量分数可为1%-10%,优选5%-7%(例如5%、6%、7%),所述的质量分数为所述的醇胺的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的季铵碱可为本领域常规使用的季铵碱,优选氢氧化四甲基铵(TMAH)、三甲基-2-羟基乙基氢氧化铵(胆碱)、氢氧化三甲基-3-羟基丙基铵、氢氧化三甲基-3-羟基丁基铵、氢氧化三甲基-4-羟基丁基铵、氢氧化三乙基-2-羟基乙基铵、氢氧化三丙基-2-羟基乙基铵、氢氧化三丁基-2-羟基乙基铵、氢氧化二甲基乙基-2-羟基乙基铵、氢氧化二甲基二-(2-羟基乙基)铵、氢氧化单甲基三乙醇铵、氢氧化四乙基铵、氢氧化四丙基铵、氢氧化四丁基铵、氢氧化四乙醇铵、氢氧化单甲基三乙基铵、氢氧化单甲基三丙基铵、氢氧化单甲基三丁基铵、氢氧化单乙基三甲基铵、氢氧化单乙基三丁基铵、氢氧化二甲基二乙基铵、氢氧化二甲基二丁基铵和氢氧化苄基三甲基铵中的一种或多种,更优选氢氧化四甲基铵和/或胆碱,进一步优选氢氧化四甲基铵。
所述的半水基清洗液中,所述的季铵碱的质量分数可为1%-15%,优选5%-10%(例如5%、7.5%、10%),所述的质量分数为所述的季铵碱的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的缓蚀剂可为本领域常规使用的缓蚀剂,优选苯并三唑(BTA)、烷基苯并三唑(例如甲基苯并三唑,又例如4-或5-甲基苯并三唑)、羧基苯并三唑、苯并咪唑、四唑、羟基苯并三唑、2-巯基苯并三唑、2-巯基苯并咪唑、甲苯基三唑、巯基甲基苯并咪唑、1,2,4-三唑、3-氨基-1,2,4-三唑、1-苯基-1H-四唑-5-硫醇、邻苯二酚(儿茶酚)、连苯三酚、没食子酸、没食子酸烷基酯(例如没食子酸甲酯和/或没食子酸丙酯)和烷基邻苯二酚(例如甲基邻苯二酚、乙基邻苯二酚和叔丁基邻苯二酚中的一种或多种)中的一种或多种,更优选苯并三唑、羧基苯并三唑、苯并咪唑、四唑、羟基苯并三唑、2-巯基苯并三唑、2-巯基苯并咪唑和儿茶酚中的一种或多种,进一步优选苯并三唑和/或儿茶酚。
所述的半水基清洗液中,所述的缓蚀剂的质量分数可为1%-15%,优选5%-10%(例如5%、6.5%、10%),所述的质量分数为所述的缓蚀剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的钝化剂的质量分数可为0.5%-10%,优选2%-5%(例如2%、2.5%、5%),所述的质量分数为所述的钝化剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的螯合剂可为本领域常规使用的螯合剂,优选(乙二胺)四乙酸(EDTA)、丁二胺四乙酸、环己-1,2-二胺四乙酸(CyDTA)、二亚乙基三胺五乙酸(DETPA)、乙二胺四丙酸、(羟乙基)乙二胺三乙酸(HEDTA)、N,N,N',N'-乙二胺四(亚甲基膦酸)(EDTMP)、三亚乙基四胺六乙酸(TTHA)、1,3-二氨基-2-羟基丙烷-N,N,N',N'-四乙酸(DHPTA)、甲基亚氨基二乙酸、丙二胺四乙酸、次氮基三乙酸(NTA)、氨基三亚甲基膦酸、衣康酸、柠檬酸、酒石酸、葡萄糖酸、葡糖二酸、甘油酸、草酸、邻苯二甲酸、马来酸、扁桃酸、丙二酸、乳酸、水杨酸、8-羟基喹啉和半胱氨酸中的一种或多种,更优选衣康酸、丙二酸、马来酸和酒石酸中的一种或多种,进一步优选衣康酸、丙二酸和酒石酸中的一种或多种。
所述的半水基清洗液中,所述的螯合剂的质量分数可为1%-20%,优选5%-10%(例如5%、6%、10%),所述的质量分数为所述的螯合剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的两性表面活性剂可为本领域常规使用的两性表面活性剂,优选甜菜碱类【例如磺基甜菜碱(sulfobetaines)、烷基甜菜碱、酰胺基烷基甜菜碱(amidoalkyl betaines)、烷基磺基甜菜碱和酰胺基烷基磺基甜菜碱(amidoalkylsulfobetaines)中的一种或多种】、氨基羧酸衍生物(例如两性甘氨酸盐、两性丙酸盐、两性二甘氨酸盐和两性二丙酸盐中的一种或多种)、亚氨基二酸(例如烷氧基烷基亚氨基二酸和/或烷氧基烷基亚氨基二酸)、氧化胺(例如烷基胺氧化物和/或烷基酰胺基烷基胺氧化物)、氟代烷基磺酸盐和氟代烷基两性表面活性剂中的一种或多种,更优选为甜菜碱、椰油酰胺基丙基甜菜碱、椰油酰胺基丙基二甲基甜菜碱、椰油酰胺基丙基羟基磺基甜菜碱、辛酰两性二丙酸盐、椰油酰胺基二丙酸盐、椰油两性丙酸盐、椰油两性羟乙基丙酸盐、异癸氧基丙基亚氨基二丙酸、月桂基亚氨基二丙酸盐、椰油酰胺基丙胺氧化物和椰油胺氧化物和氟代烷基两性表面活性剂中的一种或多种,进一步优选甜菜碱。
所述的半水基清洗液中,所述的两性表面活性剂的质量分数可为1%-5%,优选1%-2%(例如1%、1.5%、2%),所述的质量分数为所述的两性表面活性剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的非离子型表面活性剂优选EO-PO聚合物L42和/或EO-PO聚合物L44。
所述的半水基清洗液中,所述的非离子型表面活性剂的质量分数可为1%-5%,优选1%-2%(例如1%、2%),所述的质量分数为所述的非离子型表面活性剂的质量占原料的总质量的百分比。
所述的半水基清洗液中,所述的水优选去离子水、纯水和超纯水中的一种或多种,更优选去离子水。
在本发明某些优选实施方案中,所述的半水基清洗液由下述原料制得,所述的原料包括以下质量分数的组分:10%-60%的溶剂、1%-10%的醇胺、1%-15%的季铵碱、1%-15%的缓蚀剂、0.5%-10%的钝化剂、1%-20%的螯合剂、1%-5%的两性表面活性剂、1%-5%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。
在本发明某些优选实施方案中,所述的半水基清洗液由下述原料制得,所述的原料包括以下质量分数的组分:20%-40%的溶剂、5%-7%的醇胺、5%-10%的季铵碱、5%-10%的缓蚀剂、2%-5%的钝化剂、5%-10%的螯合剂、1%-2%的两性表面活性剂、1%-2%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。
在本发明某些优选实施方案中,所述的半水基清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:5%-70%的溶剂、0.5%-20%的醇胺、0.1%-20%的季铵碱、0.1%-15%的缓蚀剂、0.1%-10%的钝化剂、0.01%-20%的螯合剂、0.1%-10%的两性表面活性剂、0.1%-10%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。
在本发明某些优选实施方案中,所述的半水基清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:10%-60%的溶剂、1%-10%的醇胺、1%-15%的季铵碱、1%-15%的缓蚀剂、0.5%-10%的钝化剂、1%-20%的螯合剂、1%-5%的两性表面活性剂、1%-5%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。
在本发明某些优选实施方案中,所述的半水基清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:20%-40%的溶剂、5%-7%的醇胺、5%-10%的季铵碱、5%-10%的缓蚀剂、2%-5%的钝化剂、5%-10%的螯合剂、1%-2%的两性表面活性剂、1%-2%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比。
本发明还提供了一种上述的半水基清洗液的制备方法,其包括以下步骤:将所述的原料混合,得到半水基清洗液即可。
其中,所述的混合优选将所述的原料组分中的固体组分加入到液体组分中,搅拌均匀,即可。
其中,所述的混合的温度可为室温。
本发明还提供了一种上述的半水基清洗液在清洗含有铜互联金属线结构的半导体器件中的应用。
其中,所述的铜互联金属线的覆盖层优选钴(Co)、钨(W)、钴钨磷化物(CoWP)、钴钨硼化物(CoWB)、钴钨磷硼化物(CoWPB)、多孔二乙基甲基硅烷(PDEMS)、正硅酸乙脂(TEOS)、氮氧化硅(SiON)和氟掺杂的氧化硅玻璃(FSG)中的一种或多种。
其中,所述的清洗的温度可为室温,优选20℃-40℃(例如25℃)。所述的清洗的时间可为1min-5min(例如2min)。
术语“烷基”是指具有指定的碳原子数的直链或支链烷基。烷基的实例包括甲基、乙基、正丙基、异丙基、正丁基、叔丁基、异丁基、仲丁基、正戊基、正己基、正庚基、正辛基及其类似烷基。
术语“酰胺基”是指烷基-C(=O)-NH-或烷基-NH-C(=O)-,其中,“烷基”的定义同上所述。
本发明中,如无特殊说明,“室温”是指10-40℃。
在符合本领域常识的基础上,上述各优选条件,可任意组合,即得本发明各较佳实例。
本发明所用试剂和原料均市售可得。
本发明的积极进步效果在于:本发明的半水基清洗液对铜、钴、钨、钴钨硼化物、钴钨磷化物等的腐蚀速率小,能适应CoWP等金属环境,对多种金属及电介质的缓蚀性强,且具有很好的兼容性,清洗效果佳。
具体实施方式
下面通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法,按照常规方法和条件,或按照商品说明书选择。
实施例中涉及的缩写如下:
TMAH-四甲基氢氧化铵;BTA-苯并三唑。
Cu-铜;Co-钴;W-钨;CoWP-钴钨磷化物薄膜;CoWB-钴钨硼化物薄膜;CoWPB-钴钨磷硼化物薄膜;PDEMS-多孔二乙基甲基硅烷薄膜;TEOS-正硅酸乙脂薄膜;SiON-氮氧化硅薄膜;FSG氟掺杂的氧化硅玻璃。
实施例中的EO-PO产品均购自南通锦莱化工有限公司。
实施例1-14
将半水基清洗液的原料组分:溶剂、醇胺、季铵碱、缓蚀剂、钝化剂、螯合剂、两性表面活性剂、非离子型表面活性剂的种类和含量列于表1和表2中;半水基清洗液中的水为去离子水,去离子水补足余量。
下述实施例中,半水基清洗液的制备方法均为将实施例中原料组分中的固体组分加入到液体组分中,搅拌均匀。
下述实施例中,未限定具体操作温度的,均是指在室温条件下进行。
表1半水基清洗液的各原料组分的种类
表2半水基清洗液的各原料组分的质量分数
应用实施例1-14
(1)刻蚀速率测定
刻蚀速率待检测样品:硅晶片上沉积了单一材料的dummy片子(假片),如铝、铜、氮化钛、钨、钴、介电材料(低k或高k)等。
刻蚀实验:将待检测样品在25℃下在半水基清洗液中静态浸渍60min,然后去离子水清洗后氮气吹干。
测量蚀刻速率(A/min)的方法:分别检测样品在刻蚀前后的厚度,其中金属样品采用四点探针仪器(日本Napson的CRESTEST-e)测试厚度,非金属样品采用光学膜厚测量仪(美国Filmetrics F20)测试厚度。
腐蚀效果分四个等级:A-相容性佳,无底切;B-有极轻微底切;C-有少量底切;D-底切较为明显和严重。
(2)清洗效果测定
清洗效果待检测样品:具有图形特征(金属线metal、孔via、金属垫pad或沟槽trench等)的具有等离子刻蚀后残余物和灰化后残余物的图案化晶片。
清洗效果实验方法:将样品在25℃下在半水基清洗液中静态浸渍2min,然后去离子水清洗后氮气吹干。用电子显微镜SEM观测清洗和腐蚀效果。
清洗效果分四个等级:A-观察不到残留物;B-观察到极少量残留物;C-观察到少量残留物;D-观察到有明显较多残留物。
实施例1-14的半水基清洗液的刻蚀速率(A/min)、刻蚀效果和清洗效果如表3所示。
表3
从以上各应用实施例(1-14)可以看出,本发明的半水基清洗液对Cu、Co、W、CoWP、CoWB、CoWPB、PDEMS、TEOS、SiON和FSG均具有较低的刻蚀速率,说明其缓蚀性能较佳;且用本发明的半水基清洗液清洗具有CoWP盖帽层的图案化晶片后,几乎未观察到底切现象,说明其对多种金属及电介质具有很好的兼容性。
另外,用本发明的半水基清洗液清洗具有CoWP盖帽层的图案化晶片后,几乎观察不到残留物,说明清洗效果佳。
对比实施例1-9
其制备方法参照实施例1-14。
表4半水基清洗液的各原料组分的种类
表5半水基清洗液的各原料组分的质量分数
将对比实施例1-9的半水基清洗液进行刻蚀速率(A/min)、刻蚀效果和清洗效果,测试方法同应用实施例1-14,结果如表6所示。
表6
由上表可以看出,相较于实施例1-14,对比实施例1-9的半水基清洗液对Co、W、CoWP、CoWB、CoWPB、PDEMS、TEOS、SiON和FSG的刻蚀速率明显增高,其缓蚀性能差。
并且,用对比实施例1-9的半水基清洗液清洗具有CoWP盖帽层的图案化晶片后,出现了较为严重的底切现象,有较多的残留物。
Claims (7)
1.一种半水基清洗液,其特征在于,其由下述原料制得,所述的原料包括以下质量分数的组分:20%-40%的溶剂、5%-7%的醇胺、5%-10%的季铵碱、5%-10%的缓蚀剂、2%-5%的钝化剂、5%-10%的螯合剂、1%-2%的两性表面活性剂、1%-2%的非离子型表面活性剂和余量的水,所述的质量分数为各组分质量占原料的总质量的百分比;
其中,所述的溶剂为甘油酸;
所述的钝化剂为三((5-(吡唑-4-基)吡啶-2-基)甲基);
所述的非离子型表面活性剂为EO-PO聚合物L42、EO-PO聚合物L43和EO-PO聚合物L44中的一种或多种;
所述的醇胺为单乙醇胺、三乙醇胺、二甘醇胺和异丙醇胺中的一种或多种;
所述的季铵碱为氢氧化四甲基铵和/或胆碱;
所述的缓蚀剂为苯并三唑和/或儿茶酚;
所述的螯合剂为衣康酸、丙二酸、马来酸和酒石酸中的一种或多种;
所述的两性表面活性剂为甜菜碱;
所述的水为去离子水。
2.如权利要求1所述的半水基清洗液,其特征在于,
所述的季铵碱为氢氧化四甲基铵;
和/或,所述的螯合剂为衣康酸、丙二酸和酒石酸中的一种或多种。
3.一种如权利要求1或2所述的半水基清洗液的制备方法,其特征在于,其包括以下步骤:将所述的原料混合,得到半水基清洗液即可。
4.如权利要求3所述的半水基清洗液的制备方法,其特征在于,
所述的混合为将所述的原料组分中的固体组分加入到液体组分中,搅拌均匀,即可;
和/或,所述的混合的温度为室温。
5.一种如权利要求1或2所述的半水基清洗液在清洗含有铜互联金属线结构的半导体器件中的应用。
6.如权利要求5所述的半水基清洗液在清洗含有铜互联金属线结构的半导体器件中的应用,其特征在于,
所述的铜互联金属线的覆盖层为钴、钨、钴钨磷化物、钴钨硼化物、钴钨磷硼化物、多孔二乙基甲基硅烷、正硅酸乙脂、氮氧化硅和氟掺杂的氧化硅玻璃中的一种或多种;
和/或,所述的清洗的温度为室温;
和/或,所述的清洗的时间为1 min-5 min。
7.如权利要求6所述的半水基清洗液在清洗含有铜互联金属线结构的半导体器件中的应用,其特征在于,所述的清洗的温度为20℃-40℃。
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