TW202323513A - 清洗液及其應用 - Google Patents
清洗液及其應用 Download PDFInfo
- Publication number
- TW202323513A TW202323513A TW111146814A TW111146814A TW202323513A TW 202323513 A TW202323513 A TW 202323513A TW 111146814 A TW111146814 A TW 111146814A TW 111146814 A TW111146814 A TW 111146814A TW 202323513 A TW202323513 A TW 202323513A
- Authority
- TW
- Taiwan
- Prior art keywords
- acid
- triazole
- ammonium
- cleaning solution
- amino
- Prior art date
Links
- 238000004140 cleaning Methods 0.000 title claims abstract description 68
- 239000010941 cobalt Substances 0.000 claims abstract description 46
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 46
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000005260 corrosion Methods 0.000 claims abstract description 27
- 230000007797 corrosion Effects 0.000 claims abstract description 27
- 239000003112 inhibitor Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 3
- 125000001424 substituent group Chemical group 0.000 claims abstract description 3
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 22
- -1 nitrogen-containing heterocyclic azole compound Chemical class 0.000 claims description 17
- LJVQHXICFCZRJN-UHFFFAOYSA-N 1h-1,2,4-triazole-5-carboxylic acid Chemical compound OC(=O)C1=NC=NN1 LJVQHXICFCZRJN-UHFFFAOYSA-N 0.000 claims description 12
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 12
- QMPFMODFBNEYJH-UHFFFAOYSA-N methyl 1h-1,2,4-triazole-5-carboxylate Chemical compound COC(=O)C1=NC=NN1 QMPFMODFBNEYJH-UHFFFAOYSA-N 0.000 claims description 12
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 11
- 239000012964 benzotriazole Substances 0.000 claims description 11
- 239000002738 chelating agent Substances 0.000 claims description 10
- MVRGLMCHDCMPKD-UHFFFAOYSA-N 3-amino-1h-1,2,4-triazole-5-carboxylic acid Chemical compound NC1=NNC(C(O)=O)=N1 MVRGLMCHDCMPKD-UHFFFAOYSA-N 0.000 claims description 9
- GIAFURWZWWWBQT-UHFFFAOYSA-N 2-(2-aminoethoxy)ethanol Chemical compound NCCOCCO GIAFURWZWWWBQT-UHFFFAOYSA-N 0.000 claims description 8
- BJFLSHMHTPAZHO-UHFFFAOYSA-N benzotriazole Chemical compound [CH]1C=CC=C2N=NN=C21 BJFLSHMHTPAZHO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 7
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 claims description 7
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 claims description 7
- 229940090948 ammonium benzoate Drugs 0.000 claims description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 6
- LRUDIIUSNGCQKF-UHFFFAOYSA-N 5-methyl-1H-benzotriazole Chemical compound C1=C(C)C=CC2=NNN=C21 LRUDIIUSNGCQKF-UHFFFAOYSA-N 0.000 claims description 6
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical group CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 6
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 6
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 6
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 6
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 229960003330 pentetic acid Drugs 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- VKZRWSNIWNFCIQ-UHFFFAOYSA-N 2-[2-(1,2-dicarboxyethylamino)ethylamino]butanedioic acid Chemical compound OC(=O)CC(C(O)=O)NCCNC(C(O)=O)CC(O)=O VKZRWSNIWNFCIQ-UHFFFAOYSA-N 0.000 claims description 5
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 5
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 5
- 239000005695 Ammonium acetate Substances 0.000 claims description 5
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 5
- WDLRUFUQRNWCPK-UHFFFAOYSA-N Tetraxetan Chemical compound OC(=O)CN1CCN(CC(O)=O)CCN(CC(O)=O)CCN(CC(O)=O)CC1 WDLRUFUQRNWCPK-UHFFFAOYSA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- 229940043376 ammonium acetate Drugs 0.000 claims description 5
- 235000019257 ammonium acetate Nutrition 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- FKPSBYZGRQJIMO-UHFFFAOYSA-M benzyl(triethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC1=CC=CC=C1 FKPSBYZGRQJIMO-UHFFFAOYSA-M 0.000 claims description 5
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 claims description 5
- JVQOASIPRRGMOS-UHFFFAOYSA-M dodecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCC[N+](C)(C)C JVQOASIPRRGMOS-UHFFFAOYSA-M 0.000 claims description 5
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 claims description 5
- WJLUBOLDZCQZEV-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)C WJLUBOLDZCQZEV-UHFFFAOYSA-M 0.000 claims description 5
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 5
- RNMCCPMYXUKHAZ-UHFFFAOYSA-N 2-[3,3-diamino-1,2,2-tris(carboxymethyl)cyclohexyl]acetic acid Chemical compound NC1(N)CCCC(CC(O)=O)(CC(O)=O)C1(CC(O)=O)CC(O)=O RNMCCPMYXUKHAZ-UHFFFAOYSA-N 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 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Natural products NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- IWUCXVSUMQZMFG-AFCXAGJDSA-N Ribavirin Chemical compound N1=C(C(=O)N)N=CN1[C@H]1[C@H](O)[C@H](O)[C@@H](CO)O1 IWUCXVSUMQZMFG-AFCXAGJDSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- HIMXGTXNXJYFGB-UHFFFAOYSA-N alloxan Chemical compound O=C1NC(=O)C(=O)C(=O)N1 HIMXGTXNXJYFGB-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 4
- DHZYWCBUDKTLGD-UHFFFAOYSA-N ethyl 1h-1,2,4-triazole-5-carboxylate Chemical compound CCOC(=O)C1=NC=NN1 DHZYWCBUDKTLGD-UHFFFAOYSA-N 0.000 claims description 4
- MLVNUTAJXZZPCJ-UHFFFAOYSA-N ethyl 3-amino-1h-1,2,4-triazole-5-carboxylate Chemical compound CCOC(=O)C1=NC(N)=NN1 MLVNUTAJXZZPCJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 claims description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 4
- 229960000329 ribavirin Drugs 0.000 claims description 4
- HZCAHMRRMINHDJ-DBRKOABJSA-N ribavirin Natural products O[C@@H]1[C@H](O)[C@@H](CO)O[C@H]1N1N=CN=C1 HZCAHMRRMINHDJ-DBRKOABJSA-N 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 4
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 claims description 4
- WITMXBRCQWOZPX-UHFFFAOYSA-N 1-phenylpyrazole Chemical compound C1=CC=NN1C1=CC=CC=C1 WITMXBRCQWOZPX-UHFFFAOYSA-N 0.000 claims description 3
- UHGULLIUJBCTEF-UHFFFAOYSA-N 2-aminobenzothiazole Chemical compound C1=CC=C2SC(N)=NC2=C1 UHGULLIUJBCTEF-UHFFFAOYSA-N 0.000 claims description 3
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 claims description 3
- LBOQZDCAYYCJBU-UHFFFAOYSA-N 4-methyl-2h-benzotriazole;5-methyl-2h-benzotriazole Chemical compound C1=C(C)C=CC2=NNN=C21.CC1=CC=CC2=NNN=C12 LBOQZDCAYYCJBU-UHFFFAOYSA-N 0.000 claims description 3
- WZUUZPAYWFIBDF-UHFFFAOYSA-N 5-amino-1,2-dihydro-1,2,4-triazole-3-thione Chemical compound NC1=NNC(S)=N1 WZUUZPAYWFIBDF-UHFFFAOYSA-N 0.000 claims description 3
- QZBGOTVBHYKUDS-UHFFFAOYSA-N 5-amino-1,2-dihydropyrazol-3-one Chemical compound NC1=CC(=O)NN1 QZBGOTVBHYKUDS-UHFFFAOYSA-N 0.000 claims description 3
- QMTMACYGCXTDJL-UHFFFAOYSA-N 5-methyl-1h-1,2,4-triazole-3-carboxylic acid Chemical compound CC1=NC(C(O)=O)=NN1 QMTMACYGCXTDJL-UHFFFAOYSA-N 0.000 claims description 3
- XZGLNCKSNVGDNX-UHFFFAOYSA-N 5-methyl-2h-tetrazole Chemical compound CC=1N=NNN=1 XZGLNCKSNVGDNX-UHFFFAOYSA-N 0.000 claims description 3
- AOCDQWRMYHJTMY-UHFFFAOYSA-N 5-nitro-2h-benzotriazole Chemical compound C1=C([N+](=O)[O-])C=CC2=NNN=C21 AOCDQWRMYHJTMY-UHFFFAOYSA-N 0.000 claims description 3
- AJNQPSCMOSUVKK-UHFFFAOYSA-N 5-propan-2-yl-1h-1,2,4-triazole Chemical compound CC(C)C=1N=CNN=1 AJNQPSCMOSUVKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004251 Ammonium lactate Substances 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 claims description 3
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 claims description 3
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims description 3
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical group [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 3
- 229940059265 ammonium lactate Drugs 0.000 claims description 3
- 235000019286 ammonium lactate Nutrition 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 3
- 150000003863 ammonium salts Chemical class 0.000 claims description 3
- RZOBLYBZQXQGFY-HSHFZTNMSA-N azanium;(2r)-2-hydroxypropanoate Chemical compound [NH4+].C[C@@H](O)C([O-])=O RZOBLYBZQXQGFY-HSHFZTNMSA-N 0.000 claims description 3
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 235000005985 organic acids Nutrition 0.000 claims description 3
- XCRBXWCUXJNEFX-UHFFFAOYSA-N peroxybenzoic acid Chemical compound OOC(=O)C1=CC=CC=C1 XCRBXWCUXJNEFX-UHFFFAOYSA-N 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 239000001393 triammonium citrate Substances 0.000 claims description 3
- 235000011046 triammonium citrate Nutrition 0.000 claims description 3
- 229940116269 uric acid Drugs 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 2
- FMCUPJKTGNBGEC-UHFFFAOYSA-N 1,2,4-triazol-4-amine Chemical compound NN1C=NN=C1 FMCUPJKTGNBGEC-UHFFFAOYSA-N 0.000 claims description 2
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 claims description 2
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 2
- AFBBKYQYNPNMAT-UHFFFAOYSA-N 1h-1,2,4-triazol-1-ium-3-thiolate Chemical compound SC=1N=CNN=1 AFBBKYQYNPNMAT-UHFFFAOYSA-N 0.000 claims description 2
- XNCSCQSQSGDGES-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O XNCSCQSQSGDGES-UHFFFAOYSA-N 0.000 claims description 2
- FCKYPQBAHLOOJQ-UWVGGRQHSA-N 2-[[(1s,2s)-2-[bis(carboxymethyl)amino]cyclohexyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)[C@H]1CCCC[C@@H]1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UWVGGRQHSA-N 0.000 claims description 2
- SDXAWLJRERMRKF-UHFFFAOYSA-N 3,5-dimethyl-1h-pyrazole Chemical compound CC=1C=C(C)NN=1 SDXAWLJRERMRKF-UHFFFAOYSA-N 0.000 claims description 2
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 2
- YZTYEGCWRPJWEE-UHFFFAOYSA-N 5-(benzotriazol-2-yl)pentan-1-amine Chemical compound C1=CC=CC2=NN(CCCCCN)N=C21 YZTYEGCWRPJWEE-UHFFFAOYSA-N 0.000 claims description 2
- FLDCSPABIQBYKP-UHFFFAOYSA-N 5-chloro-1,2-dimethylbenzimidazole Chemical compound ClC1=CC=C2N(C)C(C)=NC2=C1 FLDCSPABIQBYKP-UHFFFAOYSA-N 0.000 claims description 2
- WXSBVEKBZGNSDY-UHFFFAOYSA-N 5-phenyl-2h-benzotriazole Chemical compound C1=CC=CC=C1C1=CC2=NNN=C2C=C1 WXSBVEKBZGNSDY-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 239000001741 Ammonium adipate Substances 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 claims description 2
- FTEDXVNDVHYDQW-UHFFFAOYSA-N BAPTA Chemical compound OC(=O)CN(CC(O)=O)C1=CC=CC=C1OCCOC1=CC=CC=C1N(CC(O)=O)CC(O)=O FTEDXVNDVHYDQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 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 2
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 2
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 2
- DCXYFEDJOCDNAF-REOHCLBHSA-N L-asparagine Chemical compound OC(=O)[C@@H](N)CC(N)=O DCXYFEDJOCDNAF-REOHCLBHSA-N 0.000 claims description 2
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims description 2
- LEVWYRKDKASIDU-IMJSIDKUSA-N L-cystine Chemical compound [O-]C(=O)[C@@H]([NH3+])CSSC[C@H]([NH3+])C([O-])=O LEVWYRKDKASIDU-IMJSIDKUSA-N 0.000 claims description 2
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Abstract
Description
本發明涉及化學清洗液領域,尤其涉及一種清洗液及其應用。
光刻膠硬掩模通常用於對半導體材料或電介質進行圖案化處理,目前光刻膠硬掩模被用於雙鑲嵌工藝中以在微電子器件的後端金屬化中形成互連。隨著尺寸越來越小,積體電路(IC)的可靠性越來越受到IC製造技術的關注。跟蹤互連故障機制對器件性能和可靠性的影響需要更多來自集成方案、互連材料和工藝,需要最佳的Low-k介電材料及其相關的沉積、圖案光刻、蝕刻和清潔來形成雙鑲嵌互連圖案。互連圖案晶圓製造的硬掩模方案方法是能夠以最嚴格的最佳尺寸控制將圖案轉移到底層。
隨著技術節點發展到14nm、7nm甚至更小線寬,深寬比增加,TiN等金屬硬掩模材料被用於在圖案蝕刻過程中獲得更好的蝕刻/去除選擇性、更好的圖案保留和對Low-k材料的輪廓控制。需要對TiN硬掩模進行修飾甚至完全去除,同時對銅、鈷、鉭、銣等金屬材料,TEOS、BDII等Low-k介電材料具有良好的相容性。此外,由於蝕刻殘留物的低表面能和交聯性質,以及殘留物成分物理和化學性質的變化,加之清洗液與設備膜材料和結構之間的相容性問題,使得開發能夠有效去除光刻膠刻蝕殘留物的同時又能保護Low-k介電材料和非金屬材料,並且金屬材料表面殘留低的清洗液越來越具有挑戰性。
國內外對高端半導體清洗液的報導主要以歐美國家為主。美國專利US10920141B2公開了一種用於選擇性刻蝕氮化鈦,保護鈷的組合物和方法。該清洗液主要以雙氧水作為氧化劑,TMAH和含氟組分作為蝕刻劑,添加唑類和陽離子季鹽作為腐蝕抑制劑,有機酸作為螯合劑,加之溶劑水,可選擇性去除氮化鈦和光致抗蝕劑刻蝕殘留物。從公開的專利來看,該清洗液可在pH值5~12、20℃~100℃溫度範圍內工作,50℃條件下測試的TiN蝕刻速率大於200Å/min,Cu蝕刻速率小於1Å/min,Co蝕刻速率小於0.5Å/min,SiN蝕刻速率小於0.8Å/min,Low-k介電材料的蝕刻速率小於1Å/min。該公司產品主要在歐美國家使用,在半導體清洗液領域仍佔據較大市場份額。
最新報導中,美國Versum Material公司在專利US11017995B2中公開了一種用於從電子電路器件除去TiN硬掩模的組合物、方法和系統。該組合物pH值範圍為5.5~14,使用工藝溫度為35℃~70℃,適用範圍較廣,可用於半導體基板或晶圓、平板顯示器、相變記憶體、太陽能電池板、微電子、積體電路或電腦晶片等領域。該清洗液主要以雙氧水作為氧化劑,大分子有機酸作為雙氧水穩定劑,唑類和多元醇類作為金屬腐蝕抑制劑,季銨氫氧化物和銨鹽作為蝕刻劑,水作為溶劑,加之以任選氟化物來增強清洗能力,選擇性地除去氮化鈦和來自等離子體刻蝕過程中的殘留物,同時使Cu、Co、Low-k介電材料等第二材料得到有效保護。
為了保證較好的晶圓表面處理,在14nm及以下技術節點IC領域使用較多的是配置以雙氧水,採用“To drain”模式來清洗圖案晶圓。德國巴斯夫公司在專利CN110713868A中公開了一種可迴圈使用的清洗液組合物,該組合物主要為A劑和B劑H2O2按體積比1:1組合,採用“Recycle”模式來調節Cu、Co、Ru和TiN的蝕刻速率。其中A劑組合物包括有機胺4-甲基嗎啉4-氧化物、聚乙烯亞胺+唑類作為腐蝕抑制劑、TMAH+磷酸二氫銨作為緩衝劑、有機酸銨鹽作為蝕刻劑、乙二醇醚作為有機溶劑、任選非質子溶劑和水,對碳氟(CFx)聚合物和有機殘渣具有良好的清潔性能,能夠完全或部分去除TiN,同時保護Cu、Co、Ru等金屬材料,該產品目前主要在臺灣積體電路製造股份有限公司用於加工半導體晶圓。
因此,本發明的主要目的是,提供一種清洗液,能夠選擇性去除TiN硬掩模,同時能夠保護金屬材料、非金屬材料以及Low-k介質材料的前提下,能夠有效降低金屬鈷表面有機物的殘留。
其中,R
1、R
2、R
3表示氫原子或取代基。
在一些實施例中,所述第一化合物選自1,2,4-三氮唑-3-羧酸、1,2,4-三氮唑-3-羧酸甲酯、1,2,4-三氮唑-3-羧酸乙酯、5-氨基-1,2,4-三氮唑-3-羧酸、5-氨基-1H--1,2,4-三氮唑-3-羧酸甲酯、5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯、2,3,5-三-O-三乙醯-B-D-呋喃核糖基-1,2,4-三氮唑-3-羧酸甲酯(利巴韋林縮合物)、5-氨基-1H-1,2,4-三氮唑-3-羧酸醯胺、N-(2',4'-二氯苯亞甲基)-5-氨基-1H-1,2,4-三氮唑-3-羧酸、5-X-1H-1,2,4-三氮唑-3-羧酸乙酯(X=Cl,Br,I)、5-甲基-2H-1,2,4-三氮唑-3-羧酸中的一種或多種。
在一些實施例中,所述第一化合物的質量百分比含量為0.01 wt%-10 wt%。
在一些實施例中,所述氧化劑選自H
2O
2、N-甲基嗎啉氧化物、過氧化苯甲醯、過乙酸、過氧化脲、硝酸、過氧乙酸、過氧苯甲酸、四氧嘧啶中的一種或多種;更加優選的,所述氧化劑為H
2O
2。
在一些實施例中,所述氧化劑的質量百分比含量為0.1 wt%-30 wt%。
在一些實施例中,所述鈷腐蝕抑制劑為含氮雜環唑類化合物。
在一些實施例中,所述鈷腐蝕抑制劑選自苯並三氮唑(BTA)、1,2,4-三氮唑、5-甲基苯並三氮唑(TTA)、羥基苯並三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4-三唑、苯並噻唑、甲基-1H-苯並三唑(TTL)、2-氨基苯並噻唑、2-巰基苯並噻唑、3-氨基-5-羥基吡唑、1-苯基吡唑、巰基苯並咪唑、5-氨基四唑、3-巰基-1,2,4-三唑、 3-異丙基-1,2,4-三唑、2-(5-氨基-戊基)-苯並三唑、5-苯硫醇-苯並三唑、甲基四唑、5-苯基-苯並三唑、5-硝基-苯並三唑、3-氨基-5-巰基-1,2,4-三唑、1-氨基-1,2,4三唑、1-氨基-1,2,3-苯並三唑、噻唑中的一種或多種;更加優選的,所述鈷腐蝕抑制劑為苯並三氮唑。
在一些實施例中,所述鈷腐蝕抑制劑的質量百分比含量為0.01 wt%-10 wt%。
在一些實施例中,還包括螯合劑,所述螯合劑為有機酸。
在一些實施例中,所述螯合劑為選自甘氨酸、絲氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬醯胺、穀氨醯胺、纈氨酸、賴氨酸、胱氨酸、乙二胺四乙酸(EDTA)、反式-1,2環己二胺四乙酸(CDTA)、尿酸、吡啶甲酸、次氮基三乙酸(NTA)、乙二胺-N,N’-二琥鉑酸(EDDS)、谷氨酸、二乙烯三胺五乙酸(DTPA)、羥乙基乙二胺三乙酸(HEDTA)、亞氨基二乙酸(IDA)、氨三乙酸、水楊酸、葡萄糖酸、煙酸、酒石酸、檸檬酸、1,4,7,10-四氮雜環十二烷-1,4,7,10-四乙酸(DOTA)、乙二醇四乙酸(EGTA)、1,2-雙(鄰氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、乙二胺-N,N’-雙(2-羥基苯乙酸)(HDDHA)、丙二胺四乙酸中的一種或多種。
在一些實施例中,所述螯合劑的質量百分比含量為0.05-1000ppm;更加優選的,所述螯合劑的質量百分比含量為0.1-100ppm。
在一些實施例中,進一步包括有機堿,選自季胺氫氧化合物、有機胺、有機醇胺中的一種或多種;更加優選金屬離子含量少(<50ppb)的有機堿。
在一些實施例中,所述季胺氫氧化合物選自四甲基氫氧化銨(TMAH)、四乙基氫氧化銨(TEAH)、三甲基苯基氫氧化銨(TMPAH)、四丙基氫氧化銨(TPAH)、四丁基氫氧化銨(TBAH)、苄基三甲基氫氧化銨(BTMAH)、苄基三乙基氫氧化銨(BTEAH)、膽鹼氫氧化物、氫氧化銨、十二烷基三甲基氫氧化銨(DTAH)、十六烷基三甲基氫氧化銨(CTOH)中的一種或多種;
所述有機胺選自單乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羥乙基乙二胺、環己胺、1,2-丙二胺、五甲基二乙烯三胺中的一種或多種;
所述有機醇胺選自單乙醇胺(MEA)、二乙醇胺(DEA)、三乙醇胺(TEA)、二甘醇胺(DGA)、異丙醇胺、N-甲基乙醇胺中的一種或多種。
在一些實施例中,所述有機堿的質量百分比含量為0.1 wt%-10 wt%。
在一些實施例中,進一步包括有機酸銨鹽。
在一些實施例中,所述有機酸銨鹽選自甲酸銨、草酸銨、乳酸銨、酒石酸銨、檸檬酸三銨、乙酸銨、氨基甲酸銨、碳酸銨、苯甲酸銨、EDTA四銨、EDTA三銨、EDTA二銨、琥珀酸銨、1-H-吡唑-3-甲酸銨、丙二酸銨、己二酸銨、亞氨基二乙酸銨中的一種或多種。
在一些實施例中,所述有機酸銨鹽的質量百分比含量為0.01 wt%-50 wt%。
本發明的另一方面,提供一種將以上任一所述的化學清洗液用於清洗鈷的應用方法。
在一些實施例中,應用的溫度為20-80℃;應用的pH值為4~12
通過添加三氮唑化合物,可有效降低鈷表面有機物的殘留,配合以氧化劑、鈷腐蝕抑制劑、水等,可有效去除氮化鈦硬掩模和光致抗蝕劑刻蝕殘留物,並且在高速旋轉單片機清洗中對金屬材料、非金屬材料以及Low-k介電材料等均表現出較小的腐蝕速率,提高了半導體器件的電性能,產品良率也有較大提升,操作視窗較大,在積體電路14nm及以下技術節點等高端半導體清洗領域具有良好的應用前景。
以下結合具體實施例進一步闡述本發明的優點。
應當注意的是,本發明的實施例有較佳的實施性,且並非對本發明作任何形式的限制,任何熟悉該領域的技術人員可能利用上述揭示的技術內容變更或修飾為等同的有效實施例,但凡未脫離本發明技術方案的內容,依據本發明的技術實質對以上實施例所作的任何修改或等同變化及修飾,均仍屬於本發明技術方案的範圍內。
以下結合具體實施例及附圖進一步闡述本發明的優點。
根據表1中的各組分及其含量配製實施例1-30及對比例1-3的清洗液。並且在相應溫度下使用。
表1 實施例1-30及對比例1-3中清洗液的組分及其含量
第一化合物,wt% | 氧化劑wt% | 螯合劑/ppm | 有機堿 wt% | 鈷腐蝕抑制劑wt% | 有機酸銨鹽wt% | 水 wt% | 溫度 | ||
實施例1 | 1,2,4-三氮唑-3-羧酸:0.1 | H 2O 2:3.1 | 甘氨酸:0.05 | TMAH:0.4 | BTA:0.2 | / | 96.2 | 50℃ | |
實施例2 | 1,2,4-三氮唑-3-羧酸甲酯:1 | H 2O 2:6.2 | EDTA:1 | / | 1,2,4-三氮唑:0.5 | 草酸銨:0.2 | 92.1 | 50℃ | |
實施例3 | 1,2,4-三氮唑-3-羧酸乙酯:0.8 | H 2O 2:9.3 | / | TBPH:1 | 吡唑:1 | 乳酸銨:2 | 85.9 | 50℃ | |
實施例4 | 5-氨基-1,2,4-三氮唑-3-羧酸:0.5 | H 2O 2:12.4 | 尿酸:0.5 | BTMAH:0.5 | 甲基四唑:0.1 | 酒石酸銨:1 | 85.5 | 50℃ | |
實施例5 | 5-氨基-1H-1,2,4-三氮唑-3-羧酸甲酯:0.05 | H 2O 2:15.5 | / | BTEAH:10 | 3-氨基-5-羥基吡唑:2 | 檸檬酸銨:1 | 71.45 | 50℃ | |
實施例6 | 5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯:1.5 | H 2O 2:18.6 | / | / | 5-氨基四唑:0.01 | / | 79.89 | 50℃ | |
實施例7 | 利巴韋林縮合物:5 | H 2O 2:21.7 | EDDS:8 | DTAH:1 | 甲苯三唑:1 | 氨基甲酸銨:1 | 70.3 | 50℃ | |
實施例8 | 5-氨基-1H-1,2,4-三氮唑-3-羧酸醯胺:6 | H 2O 2:24.8 | / | CTOH:1 | 2-氨基苯並噻唑:0.5 | / | 67.7 | 50℃ | |
實施例9 | 5-Cl-1H-1,2,4-三氮唑-3-羧酸乙酯:10 | H 2O 2:27.9 | DTPA:8 | 單乙胺:10 | 1-苯基吡唑:0.8 | 苯甲酸銨:1 | 50.3 | 50℃ | |
實施例10 | 5-甲基-2H-1,2,4-三氮唑-3-羧酸:5 | 過乙酸:0.1 | HEDTA:1000 | / | 5-甲基苯並三氮唑:0.5 | / | 94.3 | 20℃ | |
實施例11 | 1,2,4-三氮唑-3-羧酸:0.1 | 過氧乙酸:30 | / | / | BTA:0.5 | EDTA三銨:1 | 68.4 | 30℃ | |
實施例12 | 1,2,4-三氮唑-3-羧酸甲酯:1 | 過氧苯甲酸:5.3 | IDA:80 | 環己胺:1 | 5-硝基-苯並三唑:0.5 | EDTA二銨:0.01 | 92.19 | 40℃ | |
實施例13 | 1,2,4-三氮唑-3-羧酸乙酯:0.8 | H 2O 2:18.6 | 氨三乙酸:5 | MEA:0.1 | 3-異丙基-1,2,4-三唑:1 | / | 79.5 | 50℃ | |
實施例14 | 1,2,4-三氮唑-3-羧酸:0.1 | H 2O 2:18.6 | / | DEA:0.5 | 甲基-1H-苯並三唑:0.5 | / | 80.3 | 50℃ | |
實施例15 | 1,2,4-三氮唑-3-羧酸甲酯:1 | H 2O 2:18.6 | 酒石酸:20 | / | 1,2,4-三氮唑:0.5 | 丙二酸銨:2.5 | 77.4 | 20℃ | |
實施例16 | 1,2,4-三氮唑-3-羧酸乙酯:0.8 | H 2O 2:3.1 | / | DGA:2 | 2-巰基苯並噻唑:1 | / | 93.1 | 30℃ | |
實施例17 | 5-氨基-1,2,4-三氮唑-3-羧酸:0.5 | 四氧嘧啶:8 | DOTA:40 | / | 甲基-1H-苯並三唑:0.1 | / | 91.4 | 40℃ | |
實施例18 | 5-氨基-1H-1,2,4-三氮唑-3-羧酸甲酯:0.05 | H 2O 2:18.6 | DTPA:10 | / | BTA:2 | 苯甲酸銨:20 | 59.35 | 50℃ | |
實施例19 | 5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯:1.5 | 硝酸:5 | HDDHA:60 | DEA:8 | 吡唑:10 | 苯甲酸銨:50 | 25.5 | 60℃ | |
實施例20 | 利巴韋林縮合物:5 | NMO:5.5 | / | TMAH:10 | 1-氨基-1,2,4三唑:2 | 乙酸銨:1 | 76.5 | 80℃ | |
實施例21 | 1,2,4-三氮唑-3-羧酸:0.1 | H 2O 2:18.6 | EDTA:5 | DGA:0.4 | TTA:0.5 | 酒石酸銨:1 | 79.4 | 50℃ | |
實施例22 | 1,2,4-三氮唑-3-羧酸甲酯:0.2 | NMO:5.4 | CDTA:10 | MEA:0.3 | BTA:0.5 | 苯甲酸銨:1 | 92.6 | 50℃ | |
實施例23 | 5-氨基-1,2,4-三氮唑-3-羧酸:0.5 | H 2O 2:18.6 | DPTA:8 | TMAH:0.6 | TTL:0.7 | 乙酸銨:1 | 79 | 50℃ | |
實施例24 | 1,2,4-三氮唑-3-羧酸:0.2 | H 2O 2:18.6 | / | TMAH:0.4 | 1,2,4-三氮唑:0.5 | 酒石酸銨:1 | 79.3 | 50℃ | |
實施例25 | 1,2,4-三氮唑-3-羧酸甲酯:0.01 | H 2O 2:18.6 | IDA:25 | / | 吡唑:0.5 | 檸檬酸三銨:1 | 79.89 | 50℃ | |
實施例26 | 1,2,4-三氮唑-3-羧酸:0.3 | H 2O 2:18.6 | HDDHA:500 | TEA:0.4 | 3-氨基-5-巰基-1,2,4-三唑:0.5 | / | 80.2 | 50℃ | |
實施例27 | 5-氨基-1,2,4-三氮唑-3-羧酸:0.3 | H 2O 2:18.6 | EGTA:200 | / | BTA:0.5 | / | 79.2 | 50℃ | |
實施例28 | 1,2,4-三氮唑-3-羧酸甲酯:0.3 | H 2O 2:18.6 | / | DGA:0.4 | 甲基-1H-苯並三唑:0.5 | / | 79.2 | 50℃ | |
實施例29 | 1,2,4-三氮唑-3-羧酸甲酯:0.05 | H 2O 2:18.6 | / | / | 1,2,4-三氮唑:0.01 | 甲酸銨:0.5 | 80.84 | 50℃ | |
實施例30 | 1,2,4-三氮唑-3-羧酸甲酯:0.01 | H 2O 2:18.6 | / | / | 吡唑:0.1 | / | 81.29 | 50℃ | |
對比例1 | / | H 2O 2:18.6 | EDTA:5 | DGA:0.4 | TTA:0.5 | 酒石酸銨:1 | 79.5 | 50℃ | |
對比例2 | / | NMO:5.4 | CDTA:10 | MEA:0.3 | BTA:0.5 | 苯甲酸銨:1 | 92.8 | 50℃ | |
對比例3 | / | H 2O 2:18.6 | DPTA:8 | TMAH:0.6 | TTL:0.7 | 乙酸銨:1 | 79.5 | 50℃ | |
為了進一步測試上述清洗液的拋光性能,用實施例21-23清洗液對不同的材料進行蝕刻測試。具體測試條件如下:
用於測試蝕刻速率的測試物件及其來源:
TiN(氮化鈦)空白晶片——Ramco Specialties Inc.(美國拉姆科專業有限公司)
Cu(銅)空白晶片——Ramco Specialties Inc.
Co(鈷)空白晶片——Ramco Specialties Inc.
SiON(氮氧化矽)空白晶片——Ramco Specialties Inc.
TEOS(二氧化矽)空白晶片——Ramco Specialties Inc.
BDII(低介電常數氧化矽)空白晶片——Ramco Specialties Inc.
TiN、Cu、Co等金屬蝕刻速率測試方法:
(1)利用Napson四點探針儀測試5*5cm金屬空白晶片(TiN空白晶片、Cu空白晶片、Co空白晶片)的電阻初值(Rs1);
(2)將該5*5cm金屬空白晶片在迷你單片機mini-SWT上400rpm,TiN空白晶片經清洗液處理5min,Cu空白晶片和Co空白晶片化學處理10min;
(3)取出該5*5cm金屬空白晶片,用去離子水(DIW)清洗,高純氮氣吹幹,再利用Napson四點探針儀測試5*5cm金屬空白晶片的電阻值(Rs2);
(4)將上述電阻值和蝕刻時間輸入到合適的程式可計算出金屬的蝕刻速率。
SiON、TEOS、BDII等非金屬蝕刻速率測試方法:
1) 按照標準開啟Nanospec6100測厚儀,選用合適的測試程式,將5*5cm非金屬空白晶片(SiON空白晶片、TEOS空白晶片、BDII空白晶片)放入Nanospec6100測厚儀上測試非金屬空白晶片厚度,將非金屬空白晶片旋轉90°繼續測試,連續測試4次,記錄數值;
2) 若非金屬空白晶片為BDII,需用水沖洗乾淨,馬弗爐350℃處理20min,乾燥器冷卻至室溫再測試前值;(其他晶片無需步驟2)
3) 將該5*5cm非金屬空白晶片在mini-SWT上400rpm,清洗液處理10min;
4) 取出該5*5cm非金屬空白晶片,用DIW清洗,高純氮氣吹幹,在Nanospec6100測厚儀上按程式1測試晶片厚度,記錄數值;
5) 若非金屬空白晶片為BDII,需用水沖洗乾淨,馬弗爐350℃處理20min,乾燥器冷卻至室溫再測試後值;(其他晶片無需步驟5)
6) 將上述前後厚度值和蝕刻時間輸入合適的程式中,蝕刻速率計算為厚度變化除以化學處理時間。
按照上述蝕刻速率測試方法測試不同空白晶片的蝕刻速率。由於鈷腐蝕抑制劑基本都是含N的雜環化合物,利用X射線光電子能譜分析儀(XPS)測試清洗液中的金屬緩蝕劑在鈷表面的吸附情況,基於N元素的信號強度如圖1~圖3所示。同時在50℃、400rpm/min的條件下,使用mini-SWT單片機清洗圖案晶圓90s,水漂洗乾淨,氮氣吹幹,SEM觀察評估晶圓清洗效果。不同空白晶片的蝕刻速率、表面吸附結果及清洗效果見表2。
表2 實施例21-23與對比例1-3的蝕刻測試及清洗結果
清洗液 | 氮化鈦蝕刻速率 (Å/min) | 金屬蝕刻速率 (Å/min) | 非金屬蝕刻速率 (Å/min) | 金屬鈷表面吸附結果 | 圖形晶圓清洗結果 | |||
TiN ER | Cu ER | Co ER | SiON ER | TEOS ER | BDII ER | XPS(基於N) | 大馬士革工藝金屬孔道 | |
實施例21 | 277.63 | 0.83 | 0.22 | -0.03 | 0.22 | 0.15 | ◎ | ◎ |
實施例22 | 281.15 | 0.84 | 0.26 | 0.16 | 0.16 | -0.08 | ◎ | ◎ |
實施例23 | 278.47 | 0.95 | 0.23 | 0.07 | 0.18 | -0.06 | ◎ | ◎ |
對比例1 | 286.74 | 0.74 | 0.19 | 0.02 | 0.06 | 0.12 | ○ | ○ |
對比例2 | 292.66 | 0.66 | 0.20 | -0.04 | -0.08 | 0.17 | ○ | ○ |
對比例3 | 289.31 | 0.72 | 0.18 | 0.11 | 0.13 | 0.07 | ○ | ○ |
金屬鈷表面吸附結果(XPS) | 晶圓清洗結果 |
◎ 基本無吸附 | ◎ 基本清洗乾淨 |
○ 輕微吸附 | ○ 少量殘留物 |
△ 較多吸附 | △ 較多殘留物 |
× 嚴重吸附 | × 大量殘留物 |
從表2中可以看出:本發明的清洗液在TiN硬掩模完全去除的情況下,對半導體制程中所用的金屬材料(如Cu和Co)和非金屬材料(SiON、TEOS、BDII)基本沒有刻蝕,其腐蝕情況均滿足半導體業界通常在高速旋轉單片機清洗的要求。
對比例1與實施例21對照表明,添加了1,2,4-三氮唑-3-羧酸的體系,晶圓的蝕刻速率變化不大,均滿足刻蝕要求。結合圖1可知,添加了1,2,4-三氮唑-3-羧酸的清洗液處理的鈷表面N元素相對強度要弱,說明有機物在金屬鈷表面的吸附量實施例21比不添加1,2,4-三氮唑-3-羧酸體系的對比例1要少很多,進而在鈷表面的有機殘留物要更少。從表2的圖形晶圓的清洗效果也可以看出,添加了1,2,4-三氮唑-3-羧酸的體系處理的圖形晶圓基本清洗乾淨,這樣有利於提高半導體器件的良率。
對比例2與實施例22對照表明,添加了1,2,4-三氮唑-3-羧酸甲酯的體系,處理的晶圓蝕刻速率與不添加該組分的體系處理的基本一致,變化不大。結合X射線光電子能譜分析儀分析結果圖2可知,添加了1,2,4-三氮唑-3-羧酸甲酯的體系實施例22處理的鈷表面N元素相對強度要弱一些,有機物在鈷表面的吸附量比不添加的體系對比例2要更低,圖形晶圓的大馬士革金屬孔道清洗效果更好,鈷表面的有機殘留物得到進一步的改善。
對比例3與實施例23對照表明,添加了5-氨基-1,2,4-三氮唑-3-羧酸與不添加的體系晶圓蝕刻速率變化不大。從圖3的X射線光電子能譜分析儀結果分析可知,添加了5-氨基-1,2,4-三氮唑-3-羧酸的體系處理的金屬鈷表面N元素的相應強度要弱一些,表明有機物的吸附要更少,有利於提高圖形晶圓的導電性能。
含N唑類雜環化合物是很好的金屬鈷保護劑,其吸附在金屬鈷表面可有效控制鈷的腐蝕,但該有機保護膜也影響了半導體器件的導電性能。XPS結果顯示N元素的吸收峰回應強度能夠反映有機物保護膜在金屬鈷表面的吸附程度,三氮唑化合物中存在活性陰離子,在金屬鈷表面與鈷腐蝕抑制劑形成競爭性吸附,使得金屬緩蝕劑在保護鈷的同時可以在短時間內從鈷表面脫附,進一步降低了金屬鈷表面有機物的殘留。
綜上,本發明的積極進步效果在於:通過添加第一化合物,可有效降低鈷表面有機物的殘留。配合以氧化劑、鈷腐蝕抑制劑、水等,可有效去除氮化鈦硬掩模和光致抗蝕劑刻蝕殘留物,並且在高速旋轉單片機清洗中對金屬材料、非金屬材料以及Low-k介電材料等均表現出較小的腐蝕速率,提高了半導體器件的電性能,產品良率也有較大提升,操作視窗較大,在積體電路14nm及以下技術節點等高端半導體清洗領域具有良好的應用前景。
以上對本發明的具體實施例進行了詳細描述,但其只是作為範例,本發明並不限制於以上描述的具體實施例。對於本領域技術人員而言,任何對本發明進行的等同修改和替代也都在本發明的範疇之中。因此,在不脫離本發明的精神和範圍下所作的均等變換和修改,都應涵蓋在本發明的範圍內。
圖1為經本發明實施例21與對比例1清洗液清洗後鈷表面的XPS圖譜;
圖2為經本發明實施例22與對比例2清洗液清洗後鈷表面的XPS圖譜;
圖3為經本發明實施例23與對比例3清洗液清洗後鈷表面的XPS圖譜。
Claims (19)
- 如請求項1所述的清洗液,其中,所述第一化合物選自1,2,4-三氮唑-3-羧酸、1,2,4-三氮唑-3-羧酸甲酯、1,2,4-三氮唑-3-羧酸乙酯、5-氨基-1,2,4-三氮唑-3-羧酸、5-氨基-1H--1,2,4-三氮唑-3-羧酸甲酯、5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯、2,3,5-三-O-三乙醯-B-D-呋喃核糖基-1,2,4-三氮唑-3-羧酸甲酯(利巴韋林縮合物)、5-氨基-1H-1,2,4-三氮唑-3-羧酸醯胺、N-(2',4'-二氯苯亞甲基)-5-氨基-1H-1,2,4-三氮唑-3-羧酸、5-X-1H-1,2,4-三氮唑-3-羧酸乙酯(X=Cl,Br,I)、5-甲基-2H-1,2,4-三氮唑-3-羧酸中的一種或多種。
- 如請求項1所述的清洗液,其中,所述第一化合物的質量百分比含量為0.01 wt%-10 wt%。
- 如請求項1所述的清洗液,其中,所述氧化劑選自H 2O 2、N-甲基嗎啉氧化物、過氧化苯甲醯、過乙酸、過氧化脲、硝酸、過氧乙酸、過氧苯甲酸、四氧嘧啶中的一種或多種。
- 如請求項1所述的清洗液,其中,所述氧化劑的質量百分比含量為0.1 wt%-30 wt%。
- 如請求項1所述的清洗液,其中,所述鈷腐蝕抑制劑為含氮雜環唑類化合物。
- 如請求項6所述的清洗液,其中,所述鈷腐蝕抑制劑選自苯並三氮唑(BTA)、1,2,4-三氮唑、5-甲基苯並三氮唑(TTA)、羥基苯並三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4-三唑、苯並噻唑、甲基-1H-苯並三唑(TTL)、2-氨基苯並噻唑、2-巰基苯並噻唑、3-氨基-5-羥基吡唑、1-苯基吡唑、巰基苯並咪唑、5-氨基四唑、3-巰基-1,2,4-三唑、 3-異丙基-1,2,4-三唑、2-(5-氨基-戊基)-苯並三唑、5-苯硫醇-苯並三唑、甲基四唑、5-苯基-苯並三唑、5-硝基-苯並三唑、3-氨基-5-巰基-1,2,4-三唑、1-氨基-1,2,4三唑、1-氨基-1,2,3-苯並三唑、噻唑中的一種或多種。
- 如請求項1所述的清洗液,其中,所述鈷腐蝕抑制劑的質量百分比含量為0.01 wt%-10 wt%。
- 如請求項1所述的清洗液,其中,還包括螯合劑,所述螯合劑為有機酸。
- 如請求項9所述的清洗液,其中,所述螯合劑為選自甘氨酸、絲氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬醯胺、穀氨醯胺、纈氨酸、賴氨酸、胱氨酸、乙二胺四乙酸(EDTA)、反式-1,2環己二胺四乙酸(CDTA)、尿酸、吡啶甲酸、次氮基三乙酸(NTA)、乙二胺-N,N’-二琥鉑酸(EDDS)、谷氨酸、二乙烯三胺五乙酸(DTPA)、羥乙基乙二胺三乙酸(HEDTA)、亞氨基二乙酸(IDA)、氨三乙酸、水楊酸、葡萄糖酸、煙酸、酒石酸、檸檬酸、1,4,7,10-四氮雜環十二烷-1,4,7,10-四乙酸(DOTA)、乙二醇四乙酸(EGTA)、1,2-雙(鄰氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、乙二胺-N,N’-雙(2-羥基苯乙酸)(HDDHA)、丙二胺四乙酸中的一種或多種。
- 如請求項9所述的清洗液,其中,所述螯合劑的質量百分比含量為0.05-1000ppm。
- 如請求項1所述的清洗液,其中,進一步包括有機堿,選自季胺氫氧化合物、有機胺、有機醇胺中的一種或多種。
- 如請求項12所述的清洗液,其中,所述季胺氫氧化合物選自四甲基氫氧化銨(TMAH)、四乙基氫氧化銨(TEAH)、三甲基苯基氫氧化銨(TMPAH)、四丙基氫氧化銨(TPAH)、四丁基氫氧化銨(TBAH)、苄基三甲基氫氧化銨(BTMAH)、苄基三乙基氫氧化銨( BTEAH)、膽鹼氫氧化物、氫氧化銨、十二烷基三甲基氫氧化銨(DTAH)、十六烷基三甲基氫氧化銨(CTOH)中的一種或多種; 所述有機胺選自單乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羥乙基乙二胺、環己胺、1,2-丙二胺、五甲基二乙烯三胺中的一種或多種; 所述有機醇胺選自單乙醇胺(MEA)、二乙醇胺(DEA)、三乙醇胺(TEA)、二甘醇胺(DGA)、異丙醇胺、N-甲基乙醇胺中的一種或多種。
- 如請求項12所述的化學清洗液,其中,所述有機堿的質量百分比含量為0.1 wt%-10 wt%。
- 如請求項1所述的清洗液,其中,進一步包括有機酸銨鹽。
- 如請求項15所述的清洗液,其中,所述有機酸銨鹽選自甲酸銨、草酸銨、乳酸銨、酒石酸銨、檸檬酸三銨、乙酸銨、氨基甲酸銨、碳酸銨、苯甲酸銨、EDTA四銨、EDTA三銨、EDTA二銨、琥珀酸銨、1-H-吡唑-3-甲酸銨、丙二酸銨、己二酸銨、亞氨基二乙酸銨中的一種或多種。
- 如請求項15所述的清洗液,其中,所述有機酸銨鹽的質量百分比含量為0.01 wt%-50 wt%。
- 一種將請求項1-17中任一項所述的清洗液用於清洗鈷的應用方法。
- 如請求項18所述的應用方法,其中,應用的溫度為20-80℃,pH值為4~12。
Applications Claiming Priority (2)
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US11017995B2 (en) * | 2018-07-26 | 2021-05-25 | Versum Materials Us, Llc | Composition for TiN hard mask removal and etch residue cleaning |
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