TW202134421A - 等離子體刻蝕殘留物清洗液 - Google Patents
等離子體刻蝕殘留物清洗液 Download PDFInfo
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- TW202134421A TW202134421A TW109143515A TW109143515A TW202134421A TW 202134421 A TW202134421 A TW 202134421A TW 109143515 A TW109143515 A TW 109143515A TW 109143515 A TW109143515 A TW 109143515A TW 202134421 A TW202134421 A TW 202134421A
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- Prior art keywords
- acid
- ammonium
- cleaning solution
- plasma etching
- solution according
- Prior art date
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- 238000004140 cleaning Methods 0.000 title claims abstract description 81
- 238000001020 plasma etching Methods 0.000 title claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 40
- 238000005260 corrosion Methods 0.000 claims abstract description 26
- 230000007797 corrosion Effects 0.000 claims abstract description 26
- -1 organic acid ammonium salt Chemical class 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- 239000007800 oxidant agent Substances 0.000 claims abstract description 12
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 3
- 239000012964 benzotriazole Substances 0.000 claims description 38
- 229920005862 polyol Polymers 0.000 claims description 17
- 150000003077 polyols Chemical class 0.000 claims description 17
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 16
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 14
- 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 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000003002 pH adjusting agent Substances 0.000 claims description 12
- 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 11
- 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 11
- 229940090948 ammonium benzoate Drugs 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229960003330 pentetic acid Drugs 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 10
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 10
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000811 xylitol Substances 0.000 claims description 10
- 235000010447 xylitol Nutrition 0.000 claims description 10
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 10
- 229960002675 xylitol Drugs 0.000 claims description 10
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical group NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 9
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- GIAFURWZWWWBQT-UHFFFAOYSA-N 2-(2-aminoethoxy)ethanol Chemical compound NCCOCCO GIAFURWZWWWBQT-UHFFFAOYSA-N 0.000 claims description 7
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 7
- 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 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
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- HIMXGTXNXJYFGB-UHFFFAOYSA-N alloxan Chemical compound O=C1NC(=O)C(=O)C(=O)N1 HIMXGTXNXJYFGB-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical group 0.000 claims description 6
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 6
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 6
- 150000002391 heterocyclic compounds Chemical class 0.000 claims description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 6
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 claims description 6
- 235000013772 propylene glycol Nutrition 0.000 claims description 6
- 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
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 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
- 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
- KYQODXQIAJFKPH-UHFFFAOYSA-N diazanium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [NH4+].[NH4+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O KYQODXQIAJFKPH-UHFFFAOYSA-N 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 5
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 5
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 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
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000600 sorbitol Substances 0.000 claims description 5
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 5
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 5
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- JMTMSDXUXJISAY-UHFFFAOYSA-N 2H-benzotriazol-4-ol Chemical compound OC1=CC=CC2=C1N=NN2 JMTMSDXUXJISAY-UHFFFAOYSA-N 0.000 claims description 4
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004251 Ammonium lactate Substances 0.000 claims description 4
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 4
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Natural products NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- 229930195725 Mannitol Natural products 0.000 claims description 4
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims description 4
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 claims description 4
- 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 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 4
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 claims description 4
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical group [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 4
- 229940059265 ammonium lactate Drugs 0.000 claims description 4
- 235000019286 ammonium lactate Nutrition 0.000 claims description 4
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- NHJPVZLSLOHJDM-UHFFFAOYSA-N azane;butanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCC([O-])=O NHJPVZLSLOHJDM-UHFFFAOYSA-N 0.000 claims description 4
- ZRDJERPXCFOFCP-UHFFFAOYSA-N azane;iodic acid Chemical compound [NH4+].[O-]I(=O)=O ZRDJERPXCFOFCP-UHFFFAOYSA-N 0.000 claims description 4
- RZOBLYBZQXQGFY-HSHFZTNMSA-N azanium;(2r)-2-hydroxypropanoate Chemical compound [NH4+].C[C@@H](O)C([O-])=O RZOBLYBZQXQGFY-HSHFZTNMSA-N 0.000 claims description 4
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims description 4
- 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 4
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004220 glutamic acid Substances 0.000 claims description 4
- 235000013922 glutamic acid Nutrition 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- WJLUBOLDZCQZEV-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)C WJLUBOLDZCQZEV-UHFFFAOYSA-M 0.000 claims description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- NPZTUJOABDZTLV-UHFFFAOYSA-N hydroxybenzotriazole Substances O=C1C=CC=C2NNN=C12 NPZTUJOABDZTLV-UHFFFAOYSA-N 0.000 claims description 4
- 229940102253 isopropanolamine Drugs 0.000 claims description 4
- 239000000594 mannitol Substances 0.000 claims description 4
- 235000010355 mannitol Nutrition 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 4
- 125000003831 tetrazolyl group Chemical group 0.000 claims description 4
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 4
- YHMYGUUIMTVXNW-UHFFFAOYSA-N 1,3-dihydrobenzimidazole-2-thione Chemical compound C1=CC=C2NC(S)=NC2=C1 YHMYGUUIMTVXNW-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- UHGULLIUJBCTEF-UHFFFAOYSA-N 2-aminobenzothiazole Chemical compound C1=CC=C2SC(N)=NC2=C1 UHGULLIUJBCTEF-UHFFFAOYSA-N 0.000 claims description 3
- SDXAWLJRERMRKF-UHFFFAOYSA-N 3,5-dimethyl-1h-pyrazole Chemical compound CC=1C=C(C)NN=1 SDXAWLJRERMRKF-UHFFFAOYSA-N 0.000 claims description 3
- GDDNTTHUKVNJRA-UHFFFAOYSA-N 3-bromo-3,3-difluoroprop-1-ene Chemical compound FC(F)(Br)C=C GDDNTTHUKVNJRA-UHFFFAOYSA-N 0.000 claims description 3
- 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 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
- 239000001741 Ammonium adipate Substances 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims description 3
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 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
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-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
- 235000019293 ammonium adipate Nutrition 0.000 claims description 3
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims description 3
- KHPLPBHMTCTCHA-UHFFFAOYSA-N ammonium chlorate Chemical compound N.OCl(=O)=O KHPLPBHMTCTCHA-UHFFFAOYSA-N 0.000 claims description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 3
- OEDPMSDASHAOCT-UHFFFAOYSA-N diazanium;2-(carboxylatomethylamino)acetate Chemical compound [NH4+].[NH4+].[O-]C(=O)CNCC([O-])=O OEDPMSDASHAOCT-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- 239000008103 glucose Substances 0.000 claims description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 3
- 239000011664 nicotinic acid Substances 0.000 claims description 3
- 229960003512 nicotinic acid Drugs 0.000 claims description 3
- 235000001968 nicotinic acid Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 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
- 229940081066 picolinic acid Drugs 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 229940116269 uric acid Drugs 0.000 claims description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-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
- WITMXBRCQWOZPX-UHFFFAOYSA-N 1-phenylpyrazole Chemical compound C1=CC=NN1C1=CC=CC=C1 WITMXBRCQWOZPX-UHFFFAOYSA-N 0.000 claims description 2
- HMBHAQMOBKLWRX-UHFFFAOYSA-N 2,3-dihydro-1,4-benzodioxine-3-carboxylic acid Chemical compound C1=CC=C2OC(C(=O)O)COC2=C1 HMBHAQMOBKLWRX-UHFFFAOYSA-N 0.000 claims description 2
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- 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 2
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- DEZDKWLZZLEVST-UHFFFAOYSA-N tetrabutyl(hydroxy)-$l^{5}-phosphane Chemical compound CCCCP(O)(CCCC)(CCCC)CCCC DEZDKWLZZLEVST-UHFFFAOYSA-N 0.000 claims description 2
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- SCZVXVGZMZRGRU-UHFFFAOYSA-N n'-ethylethane-1,2-diamine Chemical compound CCNCCN SCZVXVGZMZRGRU-UHFFFAOYSA-N 0.000 claims 1
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- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
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- FVCHPLIQTBSXKX-UHFFFAOYSA-N azanium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound N.OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O FVCHPLIQTBSXKX-UHFFFAOYSA-N 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
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- 125000003438 dodecyl 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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 235000019414 erythritol Nutrition 0.000 description 1
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- 150000007524 organic acids Chemical class 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
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- XKWFRVVFRZYIFP-UHFFFAOYSA-N triazanium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound N.N.N.OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O XKWFRVVFRZYIFP-UHFFFAOYSA-N 0.000 description 1
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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
- H01L21/02057—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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
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Abstract
本發明提供一種等離子體刻蝕殘留物清洗液,包括氧化劑、pH調節劑、穩定劑、有機酸銨鹽、金屬緩蝕劑、以及水。本發明提供了一種等離子體刻蝕殘留物清洗液,可有效去除晶圓清洗過程中的等離子體刻蝕殘留物,並且,在金屬孔道中的殘留物少;對氮化鈦的刻蝕具有高選擇性,能夠高效去除氮化鈦硬遮罩;並且在高轉速單片機清洗中對金屬材料和非金屬材料包括Low-k介質材料均有較小的腐蝕速率;操作視窗較大;本申請的清洗液中不含氟,可以適用於14nm及以下銅大馬士革清洗工藝。
Description
本發明涉及半導體製造過程中的晶圓清洗液領域,尤其涉及一種等離子體刻蝕殘留物清洗液。
晶圓清洗是積體電路製程中重複次數最多的工序,清洗效果的好壞較大程度地影響晶片製程及積體電路特性等品質問題。清洗液使用的各種化學品處理不當就會嚴重污染環境,清洗次數繁多消耗大量的化學品和水。面對刻線更細、集成度更高的IC製程,人們還在研究更有效的清洗方案。光致抗蝕劑遮罩通常用於半導體工業中以將諸如半導體或電解質材料形成圖案。在一種應用中,將光致抗蝕劑遮罩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聯。雙鑲嵌工藝涉及在金屬導體層如銅(Cu)層上面的低介電常數(Low-k)介電層上形成光致抗蝕劑遮罩。然後根據光致抗蝕劑遮罩對Low-k介電層進行刻蝕以形成通道和/或開槽以露出金屬導體層。通常使用兩個平板印刷對通常稱作雙鑲嵌結構的通道和開槽進行限定。然後將光致抗蝕劑遮罩從Low-k介電層去除,然後將導電材料沉積入通道和/或開槽以形成互聯。
隨著微電子器件尺寸的下降,實現通道和開槽的臨界尺寸變得更加困難。在半導體製造領域中使用金屬銅、Low-k介質材料越來越多。尤其是銅雙大馬士革工藝越來越廣泛的情況下,尋找能夠有效去除刻蝕殘留物的同時又能保護Low-k介質材料、其它非金屬材料和金屬材料的清洗液就越來越重要。同時隨著半導體製程尺寸越來越小,清洗方式也越來越廣泛的使用到高速旋轉單片清洗。由此,使用金屬硬遮罩以提供通道和開槽更好的輪廓控制。金屬硬遮罩由鈦或氮化鈦製成,並在形成雙鑲嵌結構的通道和/或開槽之後通過濕蝕刻法去除,其具體步驟一般為清洗液清洗/漂洗/去離子水漂洗。在此過程中,只能除去殘留的聚合物光阻層和無機物,而不能攻擊損害金屬層。關鍵的是,濕蝕刻法使用去除化學品,其有效去除金屬硬遮罩和/或光抗蝕劑蝕刻殘餘物而不影響下麵的金屬導電層和Low-k介電材料。換言之,需要去除化學品對金屬導電層和Low-k介電層具有較高的選擇性。
國內外對於半導體清洗液的報導較多,US20150027978A1公開了高選擇蝕刻TiN,主要通過加入銨鹽以及雙氧水的分解來提高TiN的蝕刻速率,加入5-甲基苯並三氮唑抑制銅的腐蝕,添加氟化銨來提高清洗能力。此配方雖然對銅有很好地保護,但是5-甲基苯並三氮唑會吸附在晶圓表面,難以脫附,會對電性能造成較大影響。WO201603729A1在此基礎上做了進一步的研究,公開了一種通過氟矽酸、碘酸銨、氧化釩、釩酸銨等來調整金屬和非金屬的蝕刻速率,此方法可以進一步提高TiN的蝕刻速率,對銅也有很好的保護,但是仍然沒有解決晶圓表面緩蝕劑吸附的問題,並且引入了新的金屬離子,從而影響電性能,也沒有解決在高速旋轉下清洗液對金屬腐蝕的控制情況。US20179546321B2公開的配方中有含氟組分、有機或無機酸等,可以較好地解決晶圓表面吸附問題,但是對厚TiN硬遮罩難以徹底去除,蝕刻不完全,清洗不乾淨,影響電性能。最新報導中,美國EKC公司在專利US10155921B2中公開了一種通過氧化劑、羧酸鹽以及金屬緩蝕劑來去除氮化鈦,同時相容銅和低k介電材料的方法。以雙氧水作為氧化劑,吡咯、吡唑、吲唑及其衍生物作為金屬緩蝕劑,配合以銨鹽作為氮化鈦蝕刻增強劑,在pH值7~12的環境下,20~60℃條件下選擇性去除硬遮罩及其殘留物而不影響下面的金屬導電層和低k介電層,這樣可以獲得更好的剖面控制。
為解決現有技術中在晶圓清洗過程中的清洗液無法同時滿足有效去除刻蝕殘留物以及同時保護低k介電材料、非金屬材料和金屬材料的技術問題,本發明提供一種等離子體刻蝕殘留物清洗液,包括氧化劑、pH調節劑、穩定劑、有機酸銨鹽、金屬緩蝕劑、以及水。
在一些實施例中,所述氧化劑的質量百分濃度為0.1wt%-30wt%。
在一些實施例中,所述氧化劑為H2
O2
、N-甲基嗎啉氧化物(NMMO或NMO)、過氧化苯甲醯、過氧單硫酸四丁銨、臭氧、高錳酸、高氯酸、碘酸、高碘酸、過硫酸、過氧二硫酸銨、過乙酸(CH3
(CO)OOH)、過氧化脲((CO(NH2
)2
)H2
O2
)、硝酸、次氯酸銨、氯酸銨、碘酸銨、高氯酸銨、高碘酸銨、亞氯酸四甲銨、氯酸四甲銨、碘酸四甲銨、過硼酸四甲銨、高氯酸四甲銨、高碘酸四甲銨、過硫酸四甲銨、過氧乙酸、過氧苯甲酸、四氧嘧啶中的一種或多種。所述氧化劑優選為H2
O2
。
在一些實施例中,所述有機酸銨鹽的質量百分濃度為0.01wt%-50wt%。
在一些實施例中,所述有機酸銨鹽為甲酸銨、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、乙二胺四乙酸四銨(EDTA四銨)、乙二胺四乙酸三銨(EDTA三銨)、乙二胺四乙酸二銨(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。優選地,所述有機酸銨鹽為螯合能力強的有機酸銨鹽。
在一些實施例中,所述pH調節劑的質量百分濃度為0.1wt%-20wt%。
在一些實施例中,所述pH調節劑為鹼性調節劑。
在一些實施例中,所述pH調節劑為季胺氫氧化物、有機胺、有機醇胺中的一種或多種。
在一些實施例中,所述季胺氫氧化物為四甲基氫氧化銨(TMAH)、四乙基氫氧化銨(TEAH)、三甲基苯基氫氧化銨、苄基三甲基氫氧化銨(BTMAH)、苄基三乙基氫氧化銨(BTEAH)、四丁基氫氧化銨、四丁基氫氧化磷(TBPH)、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。
在一些實施例中,所述有機胺為單乙胺、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。
在一些實施例中,所述有機醇胺為單乙醇胺(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pH調節劑為金屬離子含量少的鹼性pH調節劑。優選地,為金屬離子含量<50ppb的鹼性pH調節劑。
在一些實施例中,所述穩定劑的質量百分濃度為0.05-1000 ppm。所述穩定劑的質量百分濃度優選為0.1-100ppm。
在一些實施例中,所述穩定劑為甘氨酸、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)、羥基乙叉二膦酸(HEDP)、亞氨基二乙酸(IDA)、氨三乙酸、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、磺胺、丙二胺四乙酸中的一種或多種。
在一些實施例中,所述金屬緩蝕劑的質量百分濃度為0.02wt%-29wt%。
在一些實施例中,所述金屬緩蝕劑為多元醇與包含至少一個氮元素的雜環化合物的混合物。優選地,所述多元醇為含羥基數較多的多元醇。
在一些實施例中,所述包含至少一個氮元素的雜環化合物為苯並三氮唑(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、羥苯並三唑、1-氨基-1,2,3-苯並三唑、噻唑中的一種或多種。所述包含至少一個氮元素的雜環化合物優選為苯並三氮唑(BTA)。
在一些實施例中,所述多元醇的結構通式為Cn
H2n+2
Om
(n≥2,m≥2)。
在一些實施例中,所述多元醇為甘油、季戊四醇、木糖醇、三羥甲基乙烷(TME)、三羥甲基丙烷(TMP)、乙二醇(EG)、丙二醇、1,2-丙二醇(1,2-PG)、1,4-丁二醇(BDO)、一縮二丙二醇、新戊二醇(NPG)、二縮二乙二醇、1,6-己二醇、葡萄塘、葡萄糖醇、果糖、核糖、丁四醇、戊五醇、己六醇、聚乙二醇400(PEG-400)、聚乙二醇600(PEG-600)、聚丙二醇400(PPG-400)、甘露醇、山梨醇中的一種或多種。
在一些實施例中,所述水的質量百分濃度為28.4wt%-96.9wt%。
在一些實施例中,所述的等離子體刻蝕殘留物清洗液的pH為7-12。
本發明中的所有試劑均市售可得。
本發明中的ppm是指用溶質質量占全部溶液質量的百萬分比來表示的質量濃度,稱百萬分比濃度;本發明的wt% 為質量百分比濃度。
與現有技術相比較,本發明的優勢在於:本發明提供了一種等離子體刻蝕殘留物清洗液,可有效去除晶圓清洗過程中的等離子體刻蝕殘留物,例如,多元醇能夠進一步降低BTA及其衍生物在銅表面的吸附,並且,在金屬孔道中的殘留物少;對氮化鈦的刻蝕具有高選擇性,能夠高效去除氮化鈦硬遮罩;並且在高轉速單片機清洗中對金屬材料(如Cu和Co等)和非金屬材料以及Low-k介質材料(如SiON、TEOS、BDII(低介電常數氧化矽)等)均有較小的腐蝕速率,例如,通過BTA及其衍生物與多元醇的協同效應,能夠很好地控制金屬銅和鈷的腐蝕;操作視窗較大,清洗溫度範圍廣,可在20℃-80℃條件下使用;本申請的清洗液中不含氟,即使是小於14nm的晶圓也不會影響其電性能。本申請的等離子體刻蝕殘留物清洗液在半導體晶圓清洗等微電子領域具有良好的應用前景。
以下通過實施例以及測試結果來詳細闡明根據本發明所述的清洗液組合物,但不限於這些實施例和以及各測試顯示的結果。本發明的清洗液組合物可體現為多種特定配方,其中所述的組合物具體組分以質量百分比來論述所有此類清洗液組合物。
實施例
製備方法:按照下述表1中各個實施例和對比例的配方(特定組分及其對應的特定含量)將各個組分進行簡單混合。
表1. 不同實施例及對比例的配方和清洗溫度
實施例 | 氧化劑wt% | 穩定劑 ppm | pH 調節劑wt% | 金屬緩蝕劑wt% | 有機酸銨鹽wt% | 水wt% | 溫度℃ |
實施例1 | H2 O2 :3.1 | 甘氨酸:0.5 | TMAH:0.4 | BTA:0.5 甘油:0.5 | 甲酸銨:0.5 | 95.0 | 50℃ |
實施例2 | H2 O2 :6.2 | EDTA:1 | TEAH:1.0 | 1,2,4-三氮唑:1.0 季戊四醇:5 | 草酸銨:0.2 | 86.6 | 50℃ |
實施例3 | H2 O2 :9.3 | CDTA:100 | TBPH:1.0 | TTA:1.0 木糖醇:0.5 | 乳酸銨:2.0 | 86.2 | 50℃ |
實施例4 | H2 O2 :12.4 | 尿酸:0.05 | BTMAH:0.5 | 羥基苯並三唑:1.0 TME:5 | 酒石酸銨:1.0 | 80.1 | 50℃ |
實施例5 | H2 O2 :15.5 | 吡啶甲酸:1 | BTEAH:10 | 吡唑:1.0 木糖醇:0.5 | 檸檬酸銨:1.0 | 72.0 | 50℃ |
實施例6 | H2 O2 :18.6 | IDA:10 | 異丙醇胺:1 | BTA:0.5 1,6-己二醇:0.5 | 乳酸銨:1 | 78.4 | 50℃ |
實施例7 | H2 O2 :21.7 | EDDS:8 | DTAH:1.0 | 四氮唑:5 山梨醇:0.5 | 氨基甲酸銨:1.0 | 70.8 | 50℃ |
實施例8 | H2 O2 :24.8 | 谷氨酸:80 | CTOH:1.0 | 苯並噻唑:0.5 核糖:0.5 | 碳酸銨:0.5 | 72.7 | 50℃ |
實施例9 | H2 O2 :27.9 | DTPA:8 | 單乙胺:10 | 2-氨基苯並噻唑:0.01 丙二醇:0.01 | 苯甲酸銨:1.0 | 61.08 | 50℃ |
實施例10 | 氯酸銨:0.1 | HEDTA:8 | 二乙胺:1.0 | 2-巰基苯並噻唑:0.5 甘露醇:0.5 | EDTA四銨:1.0 | 96.9 | 20℃ |
實施例11 | 過氧乙酸:30 | HEDP:0.1 | 三乙胺:1.0 | TTL:0.5 1,4-丁二醇:1.0 | EDTA三銨:1.0 | 66.5 | 30℃ |
實施例12 | 過氧苯甲酸:5.3 | IDA:8 | 環己胺:1.0 | 甲基四唑:0.5 葡萄糖醇:0.1 | EDTA二銨:1.0 | 92.1 | 40℃ |
實施例13 | 高氯酸:5 | 氨三乙酸:5 | 單乙醇胺:0.1 | 1-氨基-1,2,4三唑:3.5 TMP:0.5 | 琥鉑酸銨:0.8 | 90.1 | 50℃ |
實施例14 | 高碘酸:10 | 煙酸:10 | 二乙醇胺:0.5 | 羥苯並三唑:5 乙二醇:0.5 | 1-H-吡唑-3-甲酸銨:3.5 | 80.5 | 50℃ |
實施例15 | 過硫酸銨:1 | 酒石酸:20 | 三乙醇胺:1 | 噻唑:0.5 丙二醇:0.5 | 丙二酸銨:2.5 | 94.5 | 50℃ |
實施例16 | 高氯酸銨:5 | 檸檬酸:30 | 二甘醇胺:2 | 3-巰基-1,2,4-三唑:0.05 1,2-丙二醇:0.01 | 己二酸銨:10 | 82.94 | 20℃ |
實施例17 | 四氧嘧啶:8 | DOTA:40 | 異丙醇胺:4 | 5-硝基-苯並三唑:0.5 1,4-丁二醇:0.5 | 亞氨基二乙酸銨:2.4 | 84.6 | 30℃ |
實施例18 | H2 O2 :18.6 | DTPA:8 | 單乙醇胺:2 | BTA:0.25 木糖醇:0.25 | 苯甲酸銨:1 | 77.9 | 50℃ |
實施例19 | 硝酸:5 | HDDHA:60 | 二乙醇胺:8 | 巰基苯並咪唑:0.5 一縮二丙二醇:0.1 | 苯甲酸銨:0.01 | 86.39 | 40℃ |
實施例20 | NMO:5.5 | CDTA:70 | TMAH:10 | 3,5-二甲基吡唑:3.5 一縮二丙二醇:15 | 乙酸銨:1 | 65.0 | 60℃ |
實施例21 | 碘酸銨:7.5 | EDTA:80 | 1,2-丙二胺:12 | 四氮唑:5 新戊二醇:20 | 檸檬酸銨:5 | 50.5 | 70℃ |
實施例22 | H2 O2 :18.6 | DTPA:90 | 三乙醇胺:15 | BTA:0.5 二縮二乙二醇:10 | 酒石酸銨:10 | 45.9 | 80℃ |
實施例23 | H2 O2 :18.6 | CDTA:5 | TMAH:1 | BTA:0.5 山梨醇:0.5 | 乙酸銨:1.0 | 78.4 | 50℃ |
實施例24 | H2 O2 :18.6 | EDDS:200 | N-甲基乙醇胺:20 | BTA:9 葡萄糖:20 | 草酸銨:2 | 30.4 | 50℃ |
實施例25 | H2 O2 :18.6 | 氨三乙酸:0.05 | 二甘醇胺:5 | BTA:0.5 葡萄糖醇:5 | 甲酸銨:30 | 40.9 | 50℃ |
實施例26 | H2 O2 :18.6 | HEDP:0.5 | TEAH:1.0 | BTA:0.5 甘露醇:0.1 | 酒石酸銨:40 | 39.8 | 50℃ |
實施例27 | H2 O2 :18.6 | 谷氨酸:1 | TBPH:1.0 | BTA:0.5 核糖:0.5 | 檸檬酸銨:5 | 74.4 | 50℃ |
實施例28 | H2 O2 :18.6 | EDTA:1 | 二甘醇胺:0.5 | BTA:0.5 丙三醇:0.5 | 酒石酸銨:0.5 | 78.4 | 50℃ |
實施例29 | H2 O2 :18.6 | CDTA:3 | 二乙胺:1.0 | BTA:0.5 果糖:0.5 | 苯甲酸銨:0.5 | 78.9 | 60℃ |
實施例30 | H2 O2 :18.6 | NTA:4 | 三乙胺:1.0 | BTA:0.5 丁四醇:1.0 | 琥鉑酸銨:5 | 73.9 | 60℃ |
實施例31 | H2 O2 :18.6 | EDTA:5 | 二乙胺:1 | BTA:0.5 聚乙二醇:1.0 | EDTA二銨:8 | 70.9 | 50℃ |
實施例32 | H2 O2 :18.6 | DTPA:6 | TMAH:1 | BTA:0.5 聚丙二醇:1.0 | 酒石酸銨:2 | 76.9 | 50℃ |
實施例33 | H2 O2 :18.6 | EDTA:100 | 三乙醇胺:1 | BTA:1 木糖醇:1 | 苯甲酸銨:50 | 28.4 | 50℃ |
實施例34 | H2 O2 :18.6 | NTA:1000 | DGA:2 | BTA:0.3 山梨醇:0.5 | 乙酸銨:2 | 76.6 | 50℃ |
對比例1 | H2 O2 :18.6 | DTPA:8 | 單乙醇胺:2 | BTA:/ 木糖醇:/ | 苯甲酸銨:1.0 | 78.4 | 50℃ |
對比例2 | H2 O2 :18.6 | DTPA:8 | 單乙醇胺:2 | BTA:/ 木糖醇:0.5 | 苯甲酸銨:1.0 | 77.9 | 50℃ |
對比例3 | H2 O2 :18.6 | DTPA:8 | 單乙醇胺:2 | BTA:0.5 木糖醇:/ | 苯甲酸銨:1.0 | 77.9 | 50℃ |
對比例4 | H2 O2 :18.6 | DTPA:8 | 單乙醇胺:2 | BTA:0.25 木糖醇:0.25 | 苯甲酸銨:/ | 78.9 | 50℃ |
效果實施例
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—Shanghai Huali Microelectronics Corporation.(上海華力微電子有限公司)
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,高純氮氣吹乾,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(Etch Rate)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,高純氮氣吹乾,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。
將按照表1的實施例與對比例製備得到的不同清洗液,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,並利用X射線光電子能譜分析XPS測試金屬緩蝕劑在銅晶圓表面的吸附情況,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,氮氣吹乾。使用的介質為:TiN—氮化鈦;Cu—銅;Co—鈷;SiON—氮氧化矽;TEOS—低介質材料;BDII—低介質材料。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. 不同實施例與對比例的蝕刻速率、表面吸附結果、及清洗效果
清洗液 | 氮化鈦蝕刻速率 | 金屬蝕刻速率 | 非金屬蝕刻速率 | 表面吸附結果 | 晶圓清洗結果 | |||
TiN ER (Å/min) | Cu ER (Å/min) | Co ER (Å/min) | SiON ER (Å/min) | TEOS ER (Å/min) | BDII ER (Å/min) | XPS | 大馬士革工藝金屬孔道 | |
實施例6 | 298.72 | 0.71 | 0.31 | -0.07 | 0.16 | -0.17 | ◎ | ◎ |
實施例12 | 245.39 | 1.43 | 0.65 | 0.42 | -0.15 | 0.33 | ○ | ○ |
實施例18 | 261.35 | 0.42 | 0.26 | -0.14 | 0.16 | -0.13 | ◎ | ◎ |
實施例24 | 273.19 | 0.41 | 0.11 | -0.02 | 0.12 | -0.07 | ◎ | ◎ |
實施例30 | 269.33 | 0.62 | 0.23 | 0.26 | -0.14 | 0.13 | ◎ | ◎ |
對比例1 | 253.91 | 12.51 | 3.72 | 0.31 | -0.08 | 0.28 | ◎ | × |
對比例2 | 269.77 | 6.79 | 2.61 | 0.31 | 0.27 | 0.33 | ◎ | ◎ |
對比例3 | 251.66 | 1.03 | 0.73 | 0.39 | 0.26 | 0.21 | △ | △ |
對比例4 | 131.24 | 0.74 | 0.29 | 0.29 | 0.25 | 0.21 | ○ | / |
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:本發明的清洗液對半導體製程中所用的金屬(如Cu和Co)和非金屬(SiON、TEOS、BDII)基本不會侵蝕,其腐蝕情況在高轉速條件下均滿足半導體業界通常在單片高速旋轉清洗下的要求(<1Ǻ/min),而對氮化鈦的蝕刻有較高的選擇性,蝕刻速率較高。對比例1與實施例18對照表明:在對比例1中,不添加BTA和多元醇的清洗液,金屬Cu和Co腐蝕嚴重,且金屬孔道中有大量殘留物。對比例2與對比例1相比,對比例2中單獨添加多元醇,對Cu和Co的腐蝕有一定的控制作用,但對比例2與實施例18相比,對比例2的清洗液對Cu和Co的腐蝕速率仍然較大,還是難以滿足要求,但是,金屬孔道被基本清洗乾淨,基本無殘留。相對於對比例1、對比例2,對比例3中單獨添加BTA能夠有效抑制金屬Cu和Co的腐蝕,其抑制效果比對比例2中的單獨添加多元醇效果好,但是,單獨添加BTA的對比例3的清洗液對銅表面吸附物的去除能力差,即銅表面會有較多的BTA吸附。對比例3與實施例18相比,其Cu和Co的腐蝕的腐蝕速率還有進一步降低的空間。綜合對比實施例18以及對比例1-3可以說明,多元醇和BTA對金屬的腐蝕有協同控制作用。相對於未添加多元醇的對比例3,此外,添加多元醇的清洗液(如對比例2和實施例18),BTA在銅表面吸附相對較少,說明多元醇的加入能夠促進BTA從銅表面脫附,降低銅表面的殘留,有利於提高半導體器件的良率。對比例4與實施例18相比,不添加有機酸銨鹽的清洗液,氮化鈦的蝕刻速率降低很多,說明有機酸銨鹽能夠促進氮化鈦硬遮罩的去除。
綜上,本發明的積極進步效果在於:本發明開發的一種等離子體刻蝕殘留物清洗液,通過BTA及其衍生物與多元醇的協同效應,能夠很好地控制金屬銅和鈷的腐蝕,並且多元醇能夠進一步降低BTA及其衍生物在銅表面的吸附。該清洗液能夠高效地去除TiN硬遮罩,並且在高轉速單片機清洗中對非金屬材料包括Low-k介質材料(如SiON、TEOS、BDII等)均有較小的腐蝕速率,操作視窗較大,在半導體晶片清洗等微電子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。
Claims (24)
- 一種等離子體刻蝕殘留物清洗液,其中,包括氧化劑、pH調節劑、穩定劑、有機酸銨鹽、金屬緩蝕劑、以及水。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述氧化劑的質量百分濃度為0.1 wt%-30 wt%。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述氧化劑為H2O2、N-甲基嗎啉氧化物、過氧化苯甲醯、過氧單硫酸四丁銨、臭氧、高錳酸、高氯酸、碘酸、高碘酸、過硫酸、過氧二硫酸銨、過乙酸、過氧化脲、硝酸、次氯酸銨、氯酸銨、碘酸銨、高氯酸銨、高碘酸銨、亞氯酸四甲銨、氯酸四甲銨、碘酸四甲銨、過硼酸四甲銨、高氯酸四甲銨、高碘酸四甲銨、過硫酸四甲銨、過氧乙酸、過氧苯甲酸、四氧嘧啶中的一種或多種。
- 如請求項3所述的等離子體刻蝕殘留物清洗液,其中,所述氧化劑為H2 O2 。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述有機酸銨鹽的質量百分濃度為0.01 wt%-50 wt%。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述有機酸銨鹽為甲酸銨、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、乙二胺四乙酸四銨、乙二胺四乙酸三銨、乙二胺四乙酸二銨、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1所述的等離子體刻蝕殘留物清洗液,其中,所述pH調節劑的質量百分濃度為0.1 wt%-20 wt%。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述pH調節劑為鹼性調節劑。
- 如請求項8所述的等離子體刻蝕殘留物清洗液,其中,所述pH調節劑為季胺氫氧化物、有機胺、有機醇胺中的一種或多種。
- 如請求項9所述的等離子體刻蝕殘留物清洗液,其中,所述季胺氫氧化物為四甲基氫氧化銨、四乙基氫氧化銨、三甲基苯基氫氧化銨、苄基三甲基氫氧化銨、苄基三乙基氫氧化銨、四丁基氫氧化銨、四丁基氫氧化磷、膽鹼氫氧化物、氫氧化銨、十二烷基三甲基氫氧化銨、十六烷基三甲基氫氧化銨中的一種或多種。
- 如請求項9所述的等離子體刻蝕殘留物清洗液,其中,所述有機胺為單乙胺、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。
- 如請求項9所述的等離子體刻蝕殘留物清洗液,其中,所述有機醇胺為單乙醇胺、二乙醇胺、三乙醇胺、二甘醇胺、異丙醇胺、N-甲基乙醇胺中的一種或多種。
- 如請求項9所述的等離子體刻蝕殘留物清洗液,其中,所述pH調節劑為金屬離子含量小於50ppb的鹼性pH調節劑。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述穩定劑的質量濃度為0.05-1000ppm。
- 如請求項14所述的等離子體刻蝕殘留物清洗液,其中,所述穩定劑的質量濃度為0.1-100ppm。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述穩定劑為甘氨酸、乙二胺四乙酸、反式-1,2環己二胺四乙酸、尿酸、吡啶甲酸、次氮基三乙酸、乙二胺-N,N’-二琥鉑酸、谷氨酸、二乙烯三胺五乙酸、羥乙基乙二胺三乙酸、羥基乙叉二膦酸、亞氨基二乙酸、氨三乙酸、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、乙二醇四乙酸、1,2-雙(鄰氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、磺胺、丙二胺四乙酸中的一種或多種。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述金屬緩蝕劑的質量百分濃度為0.02wt%-29wt%。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述金屬緩蝕劑為多元醇與包含至少一個氮元素的雜環化合物的混合物。
- 如請求項18所述的等離子體刻蝕殘留物清洗液,其中,所述包含至少一個氮元素的雜環化合物為苯並三氮唑、1,2,4-三氮唑、5-甲基苯並三氮唑、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、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、羥苯並三唑、1-氨基-1,2,3-苯並三唑、噻唑中的一種或多種。
- 如請求項19所述的等離子體刻蝕殘留物清洗液,其中,所述包含至少一個氮元素的雜環化合物為苯並三氮唑。
- 如請求項18所述的等離子體刻蝕殘留物清洗液,其中,所述多元醇的結構通式為Cn H2n+2 Om (n≥2,m≥2)。
- 如請求項21所述的等離子體刻蝕殘留物清洗液,其中,所述多元醇為甘油、季戊四醇、木糖醇、三羥甲基乙烷、三羥甲基丙烷、乙二醇、丙二醇、1,2-丙二醇、1,4-丁二醇、一縮二丙二醇、新戊二醇、二縮二乙二醇、1,6-己二醇、葡萄塘、葡萄糖醇、果糖、核糖、丁四醇、戊五醇、己六醇、聚乙二醇400、聚乙二醇600、聚丙二醇400、甘露醇、山梨醇中的一種或多種。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述水的質量百分濃度為28.4wt%-96.9wt%。
- 如請求項1所述的等離子體刻蝕殘留物清洗液,其中,所述等離子體刻蝕殘留物清洗液的pH為7-12。
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US8361237B2 (en) * | 2008-12-17 | 2013-01-29 | Air Products And Chemicals, Inc. | Wet clean compositions for CoWP and porous dielectrics |
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US9546321B2 (en) * | 2011-12-28 | 2017-01-17 | Advanced Technology Materials, Inc. | Compositions and methods for selectively etching titanium nitride |
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US9976111B2 (en) * | 2015-05-01 | 2018-05-22 | Versum Materials Us, Llc | TiN hard mask and etch residual removal |
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