TW202307272A - 記憶體元件用半導體基板之製造方法 - Google Patents
記憶體元件用半導體基板之製造方法 Download PDFInfo
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- TW202307272A TW202307272A TW111109966A TW111109966A TW202307272A TW 202307272 A TW202307272 A TW 202307272A TW 111109966 A TW111109966 A TW 111109966A TW 111109966 A TW111109966 A TW 111109966A TW 202307272 A TW202307272 A TW 202307272A
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- titanium
- semiconductor substrate
- acid
- film
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- 239000000758 substrate Substances 0.000 title claims abstract description 122
- 239000004065 semiconductor Substances 0.000 title claims abstract description 90
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 44
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 130
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 130
- 239000010937 tungsten Substances 0.000 claims abstract description 130
- 229910052751 metal Inorganic materials 0.000 claims abstract description 119
- 239000002184 metal Substances 0.000 claims abstract description 117
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 97
- 239000010936 titanium Substances 0.000 claims abstract description 80
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 78
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 70
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 51
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000002253 acid Substances 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- -1 hexafluorosilicic acid Chemical compound 0.000 claims description 80
- 125000000217 alkyl group Chemical group 0.000 claims description 55
- 125000004432 carbon atom Chemical group C* 0.000 claims description 35
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- 125000003118 aryl group Chemical group 0.000 claims description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 22
- 150000003839 salts Chemical class 0.000 claims description 21
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 19
- 239000007800 oxidant agent Substances 0.000 claims description 18
- 150000002222 fluorine compounds Chemical class 0.000 claims description 17
- 125000001072 heteroaryl group Chemical group 0.000 claims description 17
- 125000004474 heteroalkylene group Chemical group 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 229910000042 hydrogen bromide Inorganic materials 0.000 claims description 9
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 9
- 229910052736 halogen Inorganic materials 0.000 claims description 8
- 150000002367 halogens Chemical class 0.000 claims description 8
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 8
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 8
- 150000004965 peroxy acids Chemical class 0.000 claims description 8
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 6
- 125000002947 alkylene group Chemical group 0.000 claims description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 125000000592 heterocycloalkyl group Chemical group 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical group [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 claims description 4
- DXIGZHYPWYIZLM-UHFFFAOYSA-J tetrafluorozirconium;dihydrofluoride Chemical compound F.F.F[Zr](F)(F)F DXIGZHYPWYIZLM-UHFFFAOYSA-J 0.000 claims description 4
- 150000001721 carbon Chemical class 0.000 claims description 3
- YOYLLRBMGQRFTN-SMCOLXIQSA-N norbuprenorphine Chemical compound C([C@@H](NCC1)[C@]23CC[C@]4([C@H](C3)C(C)(O)C(C)(C)C)OC)C3=CC=C(O)C5=C3[C@@]21[C@H]4O5 YOYLLRBMGQRFTN-SMCOLXIQSA-N 0.000 claims description 3
- 238000005530 etching Methods 0.000 abstract description 106
- 150000007513 acids Chemical class 0.000 abstract 1
- 239000010408 film Substances 0.000 description 231
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 54
- 238000011282 treatment Methods 0.000 description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 33
- 238000005260 corrosion Methods 0.000 description 33
- 230000007797 corrosion Effects 0.000 description 32
- 229910052814 silicon oxide Inorganic materials 0.000 description 27
- 230000004888 barrier function Effects 0.000 description 20
- 125000001424 substituent group Chemical group 0.000 description 19
- 238000005259 measurement Methods 0.000 description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 14
- 239000002904 solvent Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000007598 dipping method Methods 0.000 description 13
- 230000003647 oxidation Effects 0.000 description 13
- 238000007254 oxidation reaction Methods 0.000 description 13
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- 229910017855 NH 4 F Inorganic materials 0.000 description 10
- 230000006870 function Effects 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 10
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- 125000002704 decyl 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])* 0.000 description 8
- 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 8
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 8
- 125000001421 myristyl group Chemical group [H]C([*])([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])C([H])([H])[H] 0.000 description 8
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- 125000000913 palmityl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 8
- 125000004079 stearyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 7
- 125000003545 alkoxy group Chemical group 0.000 description 7
- 238000007654 immersion Methods 0.000 description 7
- 239000011630 iodine Substances 0.000 description 7
- 229910052740 iodine Inorganic materials 0.000 description 7
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 7
- GKQHIYSTBXDYNQ-UHFFFAOYSA-M 1-dodecylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+]1=CC=CC=C1 GKQHIYSTBXDYNQ-UHFFFAOYSA-M 0.000 description 6
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 6
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
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- 239000002585 base Substances 0.000 description 6
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- 238000010790 dilution Methods 0.000 description 6
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- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 6
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- HTZVLLVRJHAJJF-UHFFFAOYSA-M 1-decyl-3-methylimidazolium chloride Chemical compound [Cl-].CCCCCCCCCCN1C=C[N+](C)=C1 HTZVLLVRJHAJJF-UHFFFAOYSA-M 0.000 description 5
- OXFBEEDAZHXDHB-UHFFFAOYSA-M 3-methyl-1-octylimidazolium chloride Chemical compound [Cl-].CCCCCCCCN1C=C[N+](C)=C1 OXFBEEDAZHXDHB-UHFFFAOYSA-M 0.000 description 5
- UIHCLUNTQKBZGK-UHFFFAOYSA-N 3-methyl-2-pentanone Chemical compound CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 5
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 5
- UARILQSOMYIQCM-UHFFFAOYSA-N benzyl-decyl-dimethylazanium Chemical class CCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 UARILQSOMYIQCM-UHFFFAOYSA-N 0.000 description 5
- QDYLMAYUEZBUFO-UHFFFAOYSA-N cetalkonium chloride Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 QDYLMAYUEZBUFO-UHFFFAOYSA-N 0.000 description 5
- QFWPJPIVLCBXFJ-UHFFFAOYSA-N glymidine Chemical compound N1=CC(OCCOC)=CN=C1NS(=O)(=O)C1=CC=CC=C1 QFWPJPIVLCBXFJ-UHFFFAOYSA-N 0.000 description 5
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 125000001624 naphthyl group Chemical group 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten(VI) oxide Inorganic materials O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 5
- 235000012431 wafers Nutrition 0.000 description 5
- OPXNHKQUEXEWAM-UHFFFAOYSA-M 1-dodecyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCN1C=C[N+](C)=C1 OPXNHKQUEXEWAM-UHFFFAOYSA-M 0.000 description 4
- ZCPPLZJPPBIWRU-UHFFFAOYSA-M 1-hexadecyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCN1C=C[N+](C)=C1 ZCPPLZJPPBIWRU-UHFFFAOYSA-M 0.000 description 4
- LCXGSWXECDJESI-UHFFFAOYSA-M 1-methyl-3-octadecylimidazol-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCN1C=C[N+](C)=C1 LCXGSWXECDJESI-UHFFFAOYSA-M 0.000 description 4
- SDXDXENAFAXVMX-UHFFFAOYSA-M 1-methyl-3-tetradecylimidazol-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCN1C=C[N+](C)=C1 SDXDXENAFAXVMX-UHFFFAOYSA-M 0.000 description 4
- HXVNBWAKAOHACI-UHFFFAOYSA-N 2,4-dimethyl-3-pentanone Chemical compound CC(C)C(=O)C(C)C HXVNBWAKAOHACI-UHFFFAOYSA-N 0.000 description 4
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 235000019270 ammonium chloride Nutrition 0.000 description 4
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical compound [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 description 4
- FWLORMQUOWCQPO-UHFFFAOYSA-N benzyl-dimethyl-octadecylazanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 FWLORMQUOWCQPO-UHFFFAOYSA-N 0.000 description 4
- WNBGYVXHFTYOBY-UHFFFAOYSA-N benzyl-dimethyl-tetradecylazanium Chemical class CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 WNBGYVXHFTYOBY-UHFFFAOYSA-N 0.000 description 4
- 229940006460 bromide ion Drugs 0.000 description 4
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- 239000000203 mixture Substances 0.000 description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 125000001400 nonyl group Chemical group [H]C([*])([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])[H] 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 125000005702 oxyalkylene group Chemical group 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
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- 238000005240 physical vapour deposition Methods 0.000 description 4
- 125000004076 pyridyl group Chemical group 0.000 description 4
- 239000002516 radical scavenger Substances 0.000 description 4
- CPRMKOQKXYSDML-UHFFFAOYSA-M rubidium hydroxide Chemical compound [OH-].[Rb+] CPRMKOQKXYSDML-UHFFFAOYSA-M 0.000 description 4
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- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 4
- PFCHFHIRKBAQGU-UHFFFAOYSA-N 3-hexanone Chemical compound CCCC(=O)CC PFCHFHIRKBAQGU-UHFFFAOYSA-N 0.000 description 3
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 125000001204 arachidyl group Chemical group [H]C([*])([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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- CYDRXTMLKJDRQH-UHFFFAOYSA-N benzododecinium Chemical class CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 CYDRXTMLKJDRQH-UHFFFAOYSA-N 0.000 description 3
- SHFLYPPECXRCFO-UHFFFAOYSA-N benzyl-dimethyl-octylazanium Chemical class CCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SHFLYPPECXRCFO-UHFFFAOYSA-N 0.000 description 3
- 238000011088 calibration curve Methods 0.000 description 3
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- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
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- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
- CENIAFYRIODGSU-UHFFFAOYSA-N triethyl(octadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCC[N+](CC)(CC)CC CENIAFYRIODGSU-UHFFFAOYSA-N 0.000 description 2
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- GLFDLEXFOHUASB-UHFFFAOYSA-N trimethyl(tetradecyl)azanium Chemical class CCCCCCCCCCCCCC[N+](C)(C)C GLFDLEXFOHUASB-UHFFFAOYSA-N 0.000 description 2
- BOCQFIMDCVFJEF-UHFFFAOYSA-M trimethyl-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethyl]azanium;chloride Chemical compound [Cl-].CC(C)(C)CC(C)(C)C1=CC=C(OCCOCC[N+](C)(C)C)C=C1 BOCQFIMDCVFJEF-UHFFFAOYSA-M 0.000 description 2
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- 125000002948 undecyl group Chemical group [H]C([*])([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])[H] 0.000 description 2
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- IOXAUPNPMJKSKQ-UHFFFAOYSA-N 1-benzyl-2,3-dimethylbenzene Chemical group CC1=CC=CC(CC=2C=CC=CC=2)=C1C IOXAUPNPMJKSKQ-UHFFFAOYSA-N 0.000 description 1
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- HJUPHPDWOUZDKH-UHFFFAOYSA-M 1-decylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCC[N+]1=CC=CC=C1 HJUPHPDWOUZDKH-UHFFFAOYSA-M 0.000 description 1
- QWLSTCVUGYAKLE-UHFFFAOYSA-M 1-dodecyl-3-methylimidazol-3-ium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+]=1C=CN(C)C=1 QWLSTCVUGYAKLE-UHFFFAOYSA-M 0.000 description 1
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- HXWGXXDEYMNGCT-UHFFFAOYSA-M decyl(trimethyl)azanium;chloride Chemical group [Cl-].CCCCCCCCCC[N+](C)(C)C HXWGXXDEYMNGCT-UHFFFAOYSA-M 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- VUFOSBDICLTFMS-UHFFFAOYSA-M ethyl-hexadecyl-dimethylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CC VUFOSBDICLTFMS-UHFFFAOYSA-M 0.000 description 1
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- LXPCOISGJFXEJE-UHFFFAOYSA-N oxifentorex Chemical compound C=1C=CC=CC=1C[N+](C)([O-])C(C)CC1=CC=CC=C1 LXPCOISGJFXEJE-UHFFFAOYSA-N 0.000 description 1
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- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- 125000003386 piperidinyl group Chemical group 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- OSFBJERFMQCEQY-UHFFFAOYSA-N propylidene Chemical group [CH]CC OSFBJERFMQCEQY-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 1
- 125000003226 pyrazolyl group Chemical group 0.000 description 1
- 125000000719 pyrrolidinyl group Chemical group 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 159000000005 rubidium salts Chemical class 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 description 1
- 159000000008 strontium salts Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 description 1
- YQIVQBMEBZGFBY-UHFFFAOYSA-M tetraheptylazanium;bromide Chemical compound [Br-].CCCCCCC[N+](CCCCCCC)(CCCCCCC)CCCCCCC YQIVQBMEBZGFBY-UHFFFAOYSA-M 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- 125000001412 tetrahydropyranyl group Chemical group 0.000 description 1
- 125000003507 tetrahydrothiofenyl group Chemical group 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 125000000335 thiazolyl group Chemical group 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- SBHRWOBHKASWGU-UHFFFAOYSA-M tridodecyl(methyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(CCCCCCCCCCCC)CCCCCCCCCCCC SBHRWOBHKASWGU-UHFFFAOYSA-M 0.000 description 1
- JXCCIZBMTUFJKN-UHFFFAOYSA-N triethyl(tetradecyl)azanium Chemical class CCCCCCCCCCCCCC[N+](CC)(CC)CC JXCCIZBMTUFJKN-UHFFFAOYSA-N 0.000 description 1
- FNNFSPDSZSISPX-UHFFFAOYSA-N trimethyl(1-phenylnonadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCCC([N+](C)(C)C)C1=CC=CC=C1 FNNFSPDSZSISPX-UHFFFAOYSA-N 0.000 description 1
- PDSVZUAJOIQXRK-UHFFFAOYSA-N trimethyl(octadecyl)azanium Chemical class CCCCCCCCCCCCCCCCCC[N+](C)(C)C PDSVZUAJOIQXRK-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02186—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing titanium, e.g. TiO2
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C23F1/14—Aqueous compositions
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- C23F1/26—Acidic compositions for etching refractory metals
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C23F1/14—Aqueous compositions
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- C23F1/30—Acidic compositions for etching other metallic material
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
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- C23F1/32—Alkaline compositions
- C23F1/38—Alkaline compositions for etching refractory metals
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
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- C23F1/40—Alkaline compositions for etching other metallic material
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/141—Amines; Quaternary ammonium compounds
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
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- C23F11/164—Sulfur-containing compounds containing a -SO2-N group
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
- H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
- H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer
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- H—ELECTRICITY
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
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- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/308—Chemical or electrical treatment, e.g. electrolytic etching using masks
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Abstract
本發明提供以高生產效率製造高功能之記憶體元件用半導體基板的方法。一種記憶體元件用半導體基板之製造方法,包括下列步驟:步驟(1),使具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜的半導體基板與前處理劑接觸,而去除前述氧化鎢膜的至少一部分;以及步驟(2),使經步驟(1)後的半導體基板與蝕刻劑接觸,而去除前述含鈦膜的至少一部分;前述前處理劑含有選自於由酸、氨、及銨鹽構成之群組中之至少一者之氧化鎢蝕刻劑。
Description
本發明關於記憶體元件用半導體基板之製造方法。
近年來,愈發要求記憶體元件的進一步小型化、高功能化,半導體基板之微細化、三維積體化等之技術開發正在推進。
可實現如上述記憶體元件的小型化、高功能化的半導體基板中,就其材料而言,可理想地使用金屬鎢。金屬鎢能夠以CVD(化學氣相沉積)成膜,並有不易發生電遷移、電阻低、耐熱性高等特徵。因此,金屬鎢在DRAM等記憶體元件中被使用於埋入字元線等。
已知前述埋入字元線例如可藉由下列方法製造。亦即,在具有藉由蝕刻而形成之凹部的矽基板上,按順序將氧化矽膜、含有鈦、鈦合金之含鈦膜(阻隔膜)、金屬鎢膜進行製膜。然後,利用CMP(化學機械研磨)予以平坦化,再藉由乾蝕刻等對於含鈦膜及金屬鎢膜、或金屬鎢膜選擇性地蝕刻(亦可省略CMP)。然後,對於含鈦膜選擇性地蝕刻,藉此製造記憶體元件的埋入字元線(非專利文獻1)。
如上述,記憶體元件用半導體基板之製造方法中,包括不對金屬鎢造成損傷而將鈦、鈦合金予以選擇性地去除的步驟(鈦、鈦合金之選擇性蝕刻步驟)。因此,在使用金屬鎢製造小型且高功能之記憶體元件時,需要有不蝕刻金屬鎢而蝕刻鈦、鈦合金(Ti/W蝕刻選擇比高)的蝕刻劑。
[先前技術文獻]
[非專利文獻]
[非專利文獻1]SPCC 2019 Technical Program, "Wet Etchant for DRAM Word-line Titanium Nitride Recess with Selectivity to Tungsten", Wilson et al., [https://www.linx-consulting.com/wp-content/uploads/2019/04/03-15-W_Yeh-Dupont-Wet_Etchant_for_DRAM_Word_line_TiN_Recess_with_Selectivity_to_W.pdf]
[發明所欲解決之課題]
但是,已得知即便欲使用習知的蝕刻劑來製造使用金屬鎢作為材料之記憶體元件用半導體基板,有時仍會有無法獲得所期望之性能之記憶體元件的情形。其原因之一據認為是在記憶體元件用半導體基板之製造步驟中因金屬鎢膜表面的氧化而形成之氧化鎢膜所致之影響。例如,在埋入字元線中,氧化鎢膜以覆蓋含鈦膜之至少一部分之表面的形式存在的話,有時會有蝕刻劑無法和鈦、鈦合金接觸、無法蝕刻鈦、鈦合金的情形。
於是,據認為會在利用蝕刻劑所為之氮化鈦之選擇性蝕刻步驟前,利用前處理劑來去除氧化鎢。此時,前處理劑的氧化鎢膜之去除速度慢的話,使用了前處理劑的前處理所需之時間變長,從而記憶體元件用半導體基板的生產效率(處理量)降低。於是,宜使用氧化鎢之去除速度大的前處理劑。可使用如此之前處理劑來迅速地去除氧化鎢膜,然後進行利用蝕刻劑所為之鈦、鈦合金的選擇性蝕刻步驟,藉此能夠以高生產效率製造高功能之記憶體元件用半導體基板。
亦即,本發明提供以高生產效率製造高功能之記憶體元件用半導體基板的方法。
[解決課題之手段]
本案發明人等為了解決上述課題而努力研究。結果發現藉由在利用蝕刻劑所為之鈦、鈦合金的選擇性蝕刻步驟前,使用預定之前處理劑來去除氧化鎢膜,可解決上述課題,乃完成本發明。亦即,本發明例如如下所述。
[1]一種記憶體元件用半導體基板之製造方法,包括下列步驟:
步驟(1),使具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜的半導體基板與前處理劑接觸,而去除前述氧化鎢膜的至少一部分;以及
步驟(2),使經步驟(1)後的半導體基板與蝕刻劑接觸,而去除前述含鈦膜的至少一部分;
前述前處理劑含有選自於由酸、氨、及銨鹽構成之群組中之至少一者之氧化鎢蝕刻劑。
[2]如上述[1]之記憶體元件用半導體基板之製造方法,其中,前述前處理劑之pH為0.1~13。
[3]如上述[1]或[2]之記憶體元件用半導體基板之製造方法,其中,前述氧化鎢蝕刻劑含有選自於由氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸、及磷酸構成之群組中之至少一者。
[4]如上述[1]至[3]中任一項之記憶體元件用半導體基板之製造方法,其中,
前述半導體基板更含有氧化鈦膜,且
前述步驟(1)更包含將前述氧化鈦膜的至少一部分去除之步驟。
[5]如上述[1]至[4]中任一項之記憶體元件用半導體基板之製造方法,其中,
前述蝕刻劑含有(A)氧化劑、(B)氟化合物、及(C)金屬鎢抗蝕劑,
前述(A)氧化劑的添加比率,相對於前述蝕刻劑之全部質量為0.0001~10質量%,
前述(B)氟化合物的添加比率,相對於前述蝕刻劑之全部質量為0.005~10質量%,
前述(C)金屬鎢抗蝕劑的添加比率,相對於前述蝕刻劑之全部質量為0.0001~5質量%。
[6]如上述[5]之記憶體元件用半導體基板之製造方法,其中,前述(A)氧化劑含有選自於由過氧酸、鹵素含氧酸、及該等的鹽構成之群組中之至少一者。
[7]如上述[5]或[6]之記憶體元件用半導體基板之製造方法,其中,前述(B)氟化合物含有選自於由氟化氫(HF)、四氟硼酸(HBF
4)、六氟矽酸(H
2SiF
6)、六氟鋯酸(H
2ZrF
6)、六氟鈦酸(H
2TiF
6)、六氟磷酸(HPF
6)、六氟鋁酸(H
2AlF
6)、六氟鍺酸(H
2GeF
6)、及該等的鹽構成之群組中之至少一者。
[8]如上述[5]至[7]中任一項之記憶體元件用半導體基板之製造方法,其中,前述(C)金屬鎢抗蝕劑含有選自於由下列式(1)表示之銨鹽及具有碳數5~30之烷基之雜芳基鹽構成之群組中之至少一者;
[化1]
上述式(1)中,
R
1為碳數5~30之烷基、有取代或無取代之烷基(聚)雜伸烷基、有取代或無取代之芳基(聚)雜伸烷基、下列式(2)表示之基,
[化2]
上述式中,
Cy為有取代或無取代之碳數3~10之環烷基、有取代或無取代之碳數2~10之雜環烷基、有取代或無取代之碳數6~15之芳基、有取代或無取代之碳數2~15之雜芳基,
A各自獨立而為碳數1~5之伸烷基,
r為0或1,
Z為下列式中之任一者;
[化3]
R
2各自獨立而為有取代或無取代之碳數1~18之烷基、有取代或無取代之碳數6~20之芳基,
X為鹵化物離子、氫氧化物離子、有機磺酸離子、四氟硼酸根、六氟磷酸根。
[發明之效果]
依照本發明,提供以高生產效率製造高功能之記憶體元件用半導體基板的方法。
以下,針對用以實施本發明之形態詳細說明。
<記憶體元件用半導體基板之製造方法>
本發明之記憶體元件用半導體基板之製造方法包括下列步驟:步驟(1),使具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜的半導體基板與前處理劑接觸,而去除前述氧化鎢膜的至少一部分;以及步驟(2),使經步驟(1)後的半導體基板與蝕刻劑接觸,而去除前述含鈦膜的至少一部分。此時,前述前處理劑含有選自於由酸、氨、及銨鹽構成之群組中之至少一者之氧化鎢蝕刻劑。
前述前處理劑對於在半導體基板所具有之含金屬鎢之材料之表面形成之氧化鎢的蝕刻速度大,可理想地去除氧化鎢,所以處理量不會降低。又,前處理時之金屬鎢之蝕刻速度十分緩慢,所以能夠以高生產效率製造高功能之記憶體元件用半導體基板。
此外,就前述鈦合金而言,只要是對於鈦加入1種以上之除鈦以外之金屬元素或非金屬元素而成且具有金屬性質,便不特別限制,可列舉鈦與選自於由鋁、氮、碳、鉬、釩、鈮、鐵、鉻、鎳、錫、鉿 、鋯、鈀、釕、及鉑構成之群組中之至少1種元素的合金。該等之中,宜為氮化鈦。此外,本說明書中,「鈦合金」意指鈦元素之含有率相對於鈦合金之總原子量為20原子量%以上者。此外,鈦合金中之鈦元素之含有率,相對於鈦合金之總原子量宜為20原子量%以上,較佳為30原子量%,更佳為35原子量%,特佳為40~99.9原子量%。
又,本說明書中,「氧化鎢」係指因金屬鎢氧化而形成者,通常意指氧化鎢(VI)(WO
3)。
以下,邊參照圖式邊說明本發明。此外,圖式有時會有為了說明而誇飾記載的情形,有時會與實際尺寸不同。
圖1係本發明之步驟(1)的示意圖。半導體基板(步驟(1)前)10具有:具有凹部之矽基板11、由氧化矽構成之絕緣膜12、由氮化鈦構成之阻隔膜13、及金屬鎢膜14。如此之半導體基板(步驟(1)前)10,可藉由在具有凹部之矽基板上,按順序將由氧化矽構成之絕緣膜、由氮化鈦構成之阻隔膜、金屬鎢膜予以製膜,並進行利用CMP(化學機械研磨)所為之平坦化、利用乾蝕刻等所為之阻隔膜及金屬鎢膜之選擇性蝕刻來製造(亦可省略CMP)。此處,半導體基板(清洗前)10於阻隔膜13及金屬鎢膜14上具有因金屬鎢之氧化而形成的氧化鎢膜15。氧化鎢膜15係以覆蓋阻隔膜13之表面的形式存在,所以即便欲選擇性地蝕刻由氮化鈦構成之阻隔膜13,有時仍會有蝕刻劑無法理想地和阻隔膜13接觸、無法蝕刻阻隔膜13的情形。此處,參照圖1中的放大圖的話,在由氮化鈦構成之阻隔膜13表面形成有氧化鈦膜16。前述氧化鈦膜16有可能由於氧化鎢膜15之膜密度疏鬆從而通過了氧化鎢膜15的氧於阻隔膜13之表面使氮化鈦氧化而形成。此外,前述氧化鈦膜16有可能由於在記憶體元件用半導體基板之製造步驟中因非必須實施的灰化步驟導致氮化鈦氧化而形成。
可藉由對於具有如此之構成之半導體基板(清洗前)10使用前處理劑以去除氧化鎢膜15。此時,前述前處理劑對氧化鎢之蝕刻速度大,所以處理量不會降低,可實現高生產效率。又,可防止或抑制前處理時之金屬鎢之蝕刻。其結果,經前處理後獲得之半導體基板(步驟(1)後)20會具有如下疊層而成的構成:具有凹部之矽基板21、由氧化矽構成之絕緣膜22、由氮化鈦構成之阻隔膜23、及金屬鎢膜24。因此,於步驟(2)使用蝕刻劑的話,蝕刻劑能夠理想地和阻隔膜23接觸。其結果,可選擇性地蝕刻氮化鈦,獲得之半導體基板(步驟(2)後)30具有如下疊層而成的構成:具有凹部之矽基板31、絕緣膜32、經蝕刻後之阻隔膜33、及金屬鎢膜34。
此外,在較佳之一實施形態中,前處理劑不會引起或幾乎不會引起伽凡尼腐蝕(異種金屬接觸腐蝕;galvanic corrosion)。在鈦、鈦合金及金屬鎢接觸的情況下,取決於處理環境,有時會容易於和鈦、鈦合金相比自然電位相對較低的金屬鎢發生伽凡尼腐蝕。但是,本發明之較佳之一實施形態中,藉由使用合適的前處理劑,可防止或抑制伽凡尼腐蝕。
又,在較佳之一實施形態中,前處理劑可將氧化鈦膜16的至少一部分和氧化鎢膜15一起去除。藉此,蝕刻劑能夠更有效地和鈦、鈦合金接觸。其結果,可進一步選擇性地蝕刻鈦、鈦合金,可製造高功能之半導體基板。
以下,針對各步驟詳細說明。
[步驟(1)]
步驟(1)係使具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜的半導體基板與前處理劑接觸,而去除前述氧化鎢膜的至少一部分的步驟。
(半導體基板)
半導體基板具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜。半導體基板的構成不特別限制,可適當採用公知的構成。
例如,當使用於記憶體元件之埋入字元線時,半導體基板可具有在具有凹部之矽基板上按順序疊層絕緣膜、由鈦及/或鈦合金構成之阻隔膜、金屬鎢膜而得之結構。此時,通常會將阻隔膜與金屬鎢膜予以相鄰配置。
前述半導體基板更含有因金屬鎢膜表面之金屬鎢氧化而生成的氧化鎢膜。前述氧化鎢膜之形狀不特別限制。例如,可形成厚度均勻的膜,也可形成厚度不均勻的膜。又,可為連續的1個膜,也可存在有多個不連續的膜。此外,氧化鎢的體積會隨著金屬鎢之氧化而增大,所以氧化鎢膜也可存在於阻隔膜等金屬鎢膜之相鄰膜的表面。此外,於步驟(1)中,藉由前處理劑而理想地去除前述氧化鎢膜。
前述半導體基板也可更含有因含鈦膜表面之鈦、鈦合金氧化而生成的氧化鈦膜。該氧化鈦膜有可能因含鈦膜表面之鈦、鈦合金的自然氧化而形成。此時,即便含鈦膜表面被氧化鎢膜覆蓋,若該氧化鎢膜的膜密度疏鬆的話,氧仍可通過氧化鎢膜,所以有可能發生含鈦膜表面的自然氧化。又,氧化鈦膜也會因為在記憶體元件用半導體基板之製造步驟中因非必要實施的灰化步驟導致鈦、鈦合金氧化等而形成。前述氧化鈦膜之形狀不特別限制。例如,可形成厚度均勻的膜,也可形成厚度不均勻的膜。又,可為連續的1個膜,也可存在有多個不連續的膜。宜於步驟(1)中藉由前處理劑而理想地去除前述氧化鈦膜。亦即,較佳之一實施形態宜為:半導體基板更含有氧化鈦膜,且步驟(1)更包含將前述氧化鈦膜的至少一部分去除之步驟。此外,本說明書中,「氧化鈦」係指因氮化鈦氧化而形成者,通常意指氧化鈦(IV)(TiO
2)、氧氮化鈦(TiO
xN
y)(此處,x為0.01~2,y為0~1)、及它們的組合。
(前處理劑)
前處理劑含有氧化鎢蝕刻劑。可藉由使用前述前處理劑來去除前述氧化鎢膜的至少一部分。所以,前述前處理劑可以說是氧化鎢膜去除用處理劑。
氧化鎢蝕刻劑
氧化鎢蝕刻劑含有選自於由酸、氨、及銨鹽構成之群組中之至少一者。
前述酸不特別限制,可列舉:氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸、磷酸等無機酸;乙酸、甲烷磺酸、三氟甲烷磺酸、苯磺酸、對甲苯磺酸、10-樟腦磺酸等有機酸。
前述銨鹽不特別限制,可列舉:氟化銨(NH
4F);氟化氫銨(NH
4F・HF);四乙基氫氧化銨(TEAH)、四甲基氫氧化銨(TMAH)、乙基三甲基氫氧化銨、二乙基二甲基氫氧化銨、三乙基甲基氫氧化銨、四丙基氫氧化銨、四丁基氫氧化銨等四烷基氫氧化銨;苄基三甲基氫氧化銨、苄基三乙基氫氧化銨等含芳基之氫氧化銨;三甲基(2-羥基乙基)氫氧化銨、三乙基(2-羥基乙基)氫氧化銨、三丙基(2-羥基乙基)氫氧化銨、三甲基(1-羥基丙基)氫氧化銨等含羥基之氫氧化銨等。
上述之中,氧化鎢蝕刻劑,就可防止或抑制伽凡尼腐蝕的觀點,宜為酸、氟化銨、氟化氫銨,較佳為無機酸,更佳為氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸、磷酸,特佳為氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸,且就可理想地去除氧化鈦的觀點,最佳為氟化氫。
上述氧化鎢蝕刻劑可單獨使用,也可將2種以上組合使用。亦即,在一實施形態中,氧化鎢蝕刻劑,就可防止或抑制伽凡尼腐蝕的觀點,宜含有選自於由酸、氟化銨、及氟化氫銨構成之群組中之至少一者,較佳為含有無機酸中之至少一者,更佳為含有選自於由氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸、及磷酸構成之群組中之至少一者,特佳為含有選自於由氟化氫、氯化氫、溴化氫、碘化氫、硫酸、及硝酸構成之群組中之至少一者,且就可理想地去除氧化鈦的觀點,最佳為含有氟化氫。
氧化鎢蝕刻劑之含有率,相對於前處理劑之全部質量宜為0.001~50質量%,較佳為0.01~10質量%,更佳為0.03~3質量%,特佳為0.05~1質量%。氧化鎢蝕刻劑之含有率為0.001質量%以上的話,氧化鎢之蝕刻速度變大,故較理想。另一方面,氧化鎢蝕刻劑之含有率為50質量%以下的話,可於步驟(1)中防止或抑制金屬鎢之蝕刻,故較理想。
溶劑
前處理劑宜含有溶劑。前述溶劑具有使前處理劑中含有的各成分均勻分散的功能、稀釋的功能等。
作為前述溶劑,可列舉水、有機溶劑。
前述水不特別限制,宜為藉由蒸餾、離子交換處理、過濾處理、各種吸附處理等將金屬離子、有機雜質、微粒粒子等予以去除後所獲得之水,更宜為純水,尤其宜為超純水。
前述有機溶劑不特別限制,可列舉:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、第三丁醇等醇;乙二醇、丙二醇、新戊二醇、1,2-己二醇、1,6-己二醇、2-乙基己烷-1,3-二醇、甘油等多元醇;二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇單丁醚、丙二醇單甲醚、丙二醇單乙醚、二丙二醇單甲醚、三丙二醇單甲醚、二丙二醇二甲醚、二丙二醇單乙醚、丙二醇正丙醚、二丙二醇正丙醚、三丙二醇正丙醚、丙二醇正丁醚、二丙二醇正丁醚、三丙二醇正丁醚、丙二醇苯醚等二醇醚等。
上述之中,溶劑較佳為水。此外,前述溶劑可單獨使用,也可將2種以上組合使用。
就溶劑尤其水之添加比率而言,相對於前處理劑之全部質量宜為50質量%以上,較佳為80質量%以上,更佳為90質量%以上,特佳為95質量%以上。
添加劑
前處理劑也可更含有添加劑。該添加劑不特別限制,可列舉氫氧化鋰、氫氧化鈉、氫氧化鉀、氫氧化銣、氫氧化銫、氫氧化鈹、氫氧化鎂、氫氧化鈣、氫氧化鍶、氫氧化鋇等pH調整劑。此等添加劑可單獨使用,也可將2種以上組合使用。
前處理劑之物性
前處理劑之pH宜為0.1~13,就可防止或抑制伽凡尼腐蝕的觀點,較佳為0.5~10,更佳為0.5~5,特佳為0.4~2.5。
前處理劑的氧化鎢之蝕刻速度宜為15Å/min以上,較佳為20~500Å/min,更佳為20~100Å/min,特佳為20~50Å/min。前處理劑的氧化鎢之蝕刻速度為15Å/min以上的話,處理量不會降低,並可防止前處理時之金屬鎢之蝕刻,故較理想。此外,前處理劑的氧化鎢之蝕刻速度意指藉由實施例之方法測得之值。
前處理劑的金屬鎢之蝕刻速度宜為10Å/min以下,較佳為7.5Å/min以下,更佳為5.0Å/min以下,特佳為3.0Å/min以下,最佳為0.1~2.8Å/min。前處理劑的金屬鎢之蝕刻速度為10Å/min以下的話,可防止於步驟(1)(前處理時)之金屬鎢之蝕刻,故較理想。此外,前處理劑的金屬鎢之蝕刻速度意指藉由實施例之方法測得之值。
前處理劑的鈦、鈦合金之蝕刻速度宜為10Å/min以下,較佳為6Å/min以下,更佳為2Å/min以下。前處理劑的鈦、鈦合金之蝕刻速度為10Å/min以下的話,可理想地進行後述步驟(2)之蝕刻,故較理想。此外,前處理劑的鈦、鈦合金之蝕刻速度意指藉由實施例之方法測得之值。
前處理劑的絕緣層材料之蝕刻速度宜為3.0Å/min以下,較佳為1.0Å/min以下,更佳為0.3Å/min以下,特佳為0.2Å/min以下,最佳為0.1Å/min以下。前處理劑的絕緣層材料之蝕刻速度為3.0Å/min以下的話,半導體基板的形狀得到維持且就半導體元件而言的性能提高,故較理想。此外,前述絕緣層材料不特別限制,可列舉氧化矽(例如,th-Ox)等。又,前處理劑的絕緣層材料之蝕刻速度意指藉由實施例之方法測得之值。
前處理劑的WO
3/W蝕刻選擇比宜為5以上,較佳為10~100,更佳為15~100,特佳為30~100,最佳為50~90。WO
3/W蝕刻選擇比為5以上的話,可製造高功能之記憶體元件用半導體基板,故較理想。此外,本說明書中,「WO
3/W蝕刻選擇比」意指氧化鎢與金屬鎢的蝕刻選擇比,具體而言意指氧化鎢之蝕刻速度與金屬鎢之蝕刻速度的比(氧化鎢之蝕刻速度/金屬鎢之蝕刻速度)。
前處理劑的金屬鎢(W)之腐蝕電位宜為-1000~-50mV,較佳為-500~-50mV,更佳為-300~-50mV,特佳為-150~-60mV,最佳為-115~-70mV。此外,前處理劑的金屬鎢(W)之腐蝕電位意指藉由實施例之方法測得之值。
前處理劑的鈦、鈦合金之腐蝕電位宜為-500~-20mV,較佳為-350~-20mV,更佳為-200~-20mV,特佳為-130~-30mV,最佳為-100~-40mV。此外,前處理劑的鈦、鈦合金之腐蝕電位意指藉由實施例之方法測得之值。
前處理劑的金屬鎢(W)與鈦、鈦合金之腐蝕電位差(金屬鎢(W)之腐蝕電位-鈦、鈦合金之腐蝕電位)不特別限制,宜為-50~300mV,較佳為-50~200mV,更佳為-30~100mV,特佳為-30~50mV,最佳為-10~40mV。腐蝕電位差為上述範圍的話,可防止或抑制金屬鎢(W)的伽凡尼腐蝕發生,故較理想。
(接觸)
就半導體基板與前處理劑的接觸方法而言,不特別限制,可適當採用公知的技術。具體而言,可將半導體基板浸漬於前處理劑中,也可用前處理劑對半導體基板進行噴霧,也可進行滴加(單片旋轉處理等)。此時,亦可將前述浸漬重複2次以上,亦可將噴霧重複2次以上,亦可將滴加重複2次以上,亦可將浸漬、噴霧、及滴加予以組合。
接觸溫度不特別限制,宜為0~90℃,較佳為15~80℃,更佳為20~70℃。
接觸時間不特別限制,宜為0秒~3小時,較佳為10秒~1小時,更佳為10秒~45分鐘,特佳為20秒~5分鐘。
可藉由使半導體基板與前處理劑接觸來去除氧化鎢膜的至少一部分。
[步驟(2)]
步驟(2)係使經步驟(1)後的半導體基板與蝕刻劑接觸而去除前述含鈦膜的至少一部分的步驟。
(經步驟(1)後的半導體基板)
經步驟(1)後的半導體基板具有含鈦膜及金屬鎢膜。氧化鎢膜宜於步驟(1)中被完全去除,但也可有一部分殘留。又,當在步驟(1)前之半導體基板含有氧化鈦膜時,該氧化鈦膜宜於步驟(1)中被完全去除,但也可有一部分或全部殘留。經步驟(1)後的半導體基板中,因進行了步驟(1)從而氧化鎢膜的至少一部分已被去除,所以在步驟(2)中含鈦膜可理想地和蝕刻劑接觸,可理想地進行鈦、鈦合金的選擇性蝕刻。
(蝕刻劑)
就蝕刻劑而言,只要是對金屬鎢的蝕刻慢且會蝕刻鈦、鈦合金(Ti/W蝕刻選擇比高)者,便不特別限制,可使用公知的蝕刻劑。其中,蝕刻劑宜含有(A)氧化劑、(B)氟化合物、及(C)金屬鎢抗蝕劑。此時,前述(A)氧化劑的添加比率,相對於前述蝕刻劑之全部質量宜為0.0001~10質量%。又,前述(B)氟化合物的添加比率,相對於前述蝕刻劑之全部質量宜為0.005~10質量%。而且,前述(C)金屬鎢抗蝕劑的添加比率,相對於前述蝕刻劑之全部質量宜為0.0001~5質量%。以下,針對該較佳之蝕刻劑詳細說明。此外,本說明書中,「Ti/W蝕刻選擇比」意指鈦、鈦合金與金屬鎢的蝕刻選擇比,具體而言,意指鈦、鈦合金之蝕刻速度與金屬鎢之蝕刻速度的比(鈦、鈦合金之蝕刻速度/金屬鎢之蝕刻速度)。
(A)氧化劑
(A)氧化劑具有使鈦、鈦合金中的鈦的氧化數變化為4價並使其溶解於蝕刻劑的功能等。
(A)氧化劑不特別限制,可列舉過氧酸、鹵素含氧酸、及該等的鹽。
前述過氧酸可列舉:過氧化氫、過硫酸、過碳酸、過磷酸、過乙酸、過苯甲酸、間氯過苯甲酸等。
前述鹵素含氧酸可列舉:次氯酸、亞氯酸、氯酸、過氯酸等氯的含氧酸;次溴酸、亞溴酸、溴酸、過溴酸等溴的含氧酸;次碘酸、亞碘酸、碘酸、過碘酸等碘的含氧酸等。
前述鹽可列舉:上述過氧酸或鹵素含氧酸的鋰鹽、鈉鹽、鉀鹽、銣鹽、銫鹽等鹼金屬鹽;上述過氧酸或鹵素含氧酸的鈹鹽、鎂鹽、鈣鹽、鍶鹽、鋇鹽等鹼土族金屬鹽;上述過氧酸或鹵素含氧酸的鋁鹽、銅鹽、鋅鹽、銀鹽等金屬鹽;上述過氧酸或鹵素含氧酸的銨鹽等。
上述(A)氧化劑宜為過氧化氫、碘的含氧酸,較佳為過氧化氫、碘酸、過碘酸,考量提高Ti/W蝕刻選擇比的觀點,更佳為過氧化氫、過碘酸,特佳為過碘酸。
上述(A)氧化劑可單獨使用,也可將2種以上組合使用。亦即,在一實施形態中,(A)氧化劑宜含有選自於由過氧酸、鹵素含氧酸、及該等的鹽構成之群組中之至少一者,較佳為含有選自於由過氧化氫、碘的含氧酸構成之群組中之至少一者,更佳為含有選自於由過氧化氫、碘酸、過碘酸構成之群組中之至少一者,特佳為含有選自於由過氧化氫、過碘酸構成之群組中之至少一者,最佳為含有過碘酸。
(A)氧化劑的添加比率,相對於前述蝕刻劑之全部質量宜為0.0001~10質量%,較佳為0.001~5質量%,更佳為0.003~3質量%,特佳為0.01~2質量%。
(B)氟化合物
(B)氟化合物具有促進鈦、鈦合金之蝕刻的功能等。
前述(B)氟化合物不特別限制,可列舉氟化氫(HF)、四氟硼酸(HBF
4)、六氟矽酸(H
2SiF
6)、六氟鋯酸(H
2ZrF
6)、六氟鈦酸(H
2TiF
6)、六氟磷酸(HPF
6)、六氟鋁酸(H
2AlF
6)、六氟鍺酸(H
2GeF
6)、及該等的鹽。
此時,作為前述鹽,可列舉氟化銨(NH
4F)、氟化氫銨(NH
4F・HF)、四氟硼酸銨(NH
4BF
4)、六氟矽酸銨((NH
4)
2SiF
6)、四氟硼酸四甲基銨(N(CH
3)
4BF
4)等銨鹽。
上述之中,(B)氟化合物宜為氟化氫(HF)、四氟硼酸(HBF
4)、六氟矽酸(H
2SiF
6)、及該等的鹽,較佳為氟化氫(HF)、氟化銨(NH
4F)、氟化氫銨(NH
4F・HF)、六氟矽酸(H
2SiF
6),考量鈦、鈦合金之蝕刻速度大的觀點,更佳為氟化氫(HF)、氟化氫銨(NH
4F・HF),特佳為氟化氫銨(NH
4F・HF)。
此外,上述(B)氟化合物可單獨使用,也可將2種以上組合使用。亦即,在較佳之一實施形態中,(B)氟化合物宜含有選自於由氟化氫(HF)、四氟硼酸(HBF
4)、六氟矽酸(H
2SiF
6)、六氟鋯酸(H
2ZrF
6)、六氟鈦酸(H
2TiF
6)、六氟磷酸(HPF
6)、六氟鋁酸(H
2AlF
6)、六氟鍺酸(H
2GeF
6)、及該等的鹽構成之群組中之至少一者,較佳為含有選自於由氟化氫(HF)、四氟硼酸(HBF
4)、六氟矽酸(H
2SiF
6)、及該等的鹽構成之群組中之至少一者,更佳為含有選自於由氟化氫(HF)、氟化銨(NH
4F)、氟化氫銨(NH
4F・HF)、及六氟矽酸(H
2SiF
6)構成之群組中之至少一者,特佳為含有選自於由氟化氫(HF)及氟化氫銨(NH
4F・HF)構成之群組中之至少一者,最佳為含有氟化氫銨(NH
4F・HF)。
(B)氟化合物的添加比率,相對於蝕刻劑之全部質量宜為0.005~10質量%,較佳為0.01~5質量%,更佳為0.01~3質量%,特佳為0.03~1質量%。
(C)金屬鎢抗蝕劑
(C)金屬鎢抗蝕劑具有吸附於金屬鎢而形成保護膜並且防止或抑制蝕刻劑所為之蝕刻的功能等。
前述(C)金屬鎢抗蝕劑不特別限制,可列舉下列式(1)表示之銨鹽及具有碳數5~30之烷基之雜芳基鹽等。
上述式中,R
1為碳數5~30之烷基、有取代或無取代之烷基(聚)雜伸烷基、有取代或無取代之芳基(聚)雜伸烷基、下列式(2)表示之基。
此處,式(2)中,Cy為有取代或無取代之(雜)環烷基、有取代或無取代之(雜)芳基,A各自獨立而為碳數1~5之伸烷基,r為0或1,Z為下列式中之任一者。
此時,*表示與式(1)之氮(N)原子鍵結的位置。藉此,容易吸附於金屬鎢,並使金屬鎢之抗蝕功能提高。
碳數5~30之烷基不特別限制,可列舉戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基等。
烷基(聚)雜伸烷基係以-(C
nH
2n-Z-)
m-R
3表示。此時,n各自獨立而為1~5,宜為1~3,較佳為1~2。m為1~5,宜為1~2。Z各自獨立而為氧原子(O)、硫原子(S)、磷原子(P),宜為氧原子(O)。R
3為碳數1~30之烷基,可列舉甲基、乙基、丙基、異丙基、丁基、戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基等。
烷基(聚)雜伸烷基也可具有取代基。該取代基通常會對R
3的氫原子進行取代。烷基(聚)雜伸烷基具有取代基時的取代基不特別限制,可列舉:苯基、萘基等碳數6~20之芳基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;羥基;氰基;硝基等。此外,取代基可為1個,也可有2個以上。
芳基(聚)雜伸烷基係以-(C
nH
2n-Z-)
m-Ar表示。此時,n各自獨立而為1~5,宜為1~3,較佳為1~2。m為1~5,宜為1~2。Z各自獨立而為氧原子(O)、硫原子(S)、磷原子(P),宜為氧原子(O)。Ar為碳數6~18之芳基,可列舉苯基、萘基、蒽基等。
芳基(聚)雜伸烷基也可具有取代基。該取代基通常會對Ar的氫原子進行取代。芳基(聚)雜伸烷基具有取代基時的取代基不特別限制,可列舉:甲基、乙基、丙基、異丙基、丁基、1,1-二甲基丁基、2,2-二甲基丁基、1,1,3,3-四甲基丁基等碳數1~10之烷基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;羥基;氰基;硝基等。此外,取代基可為1個,也可有2個以上。
式(2)中,Cy為有取代或無取代之碳數3~10之環烷基、有取代或無取代之碳數2~10之雜環烷基、有取代或無取代之碳數6~15之芳基、有取代或無取代之碳數2~15之雜芳基,前述碳數3~10之環烷基不特別限制,可列舉環丙基、環丁基、環戊基、環己基等。前述碳數2~10之雜環烷基不特別限制,可列舉吡咯啶基、哌啶基、四氫呋喃基、四氫吡喃基、四氫噻吩基等。前述碳數6~15之芳基不特別限制,可列舉苯基等。前述碳數2~15之雜芳基不特別限制,可列舉吡咯基、咪唑基、吡唑基、㗁唑基、異㗁唑基(isoxazolyl)、噻唑基、異噻唑基、吡啶基、吡𠯤基、嗒𠯤基、嘧啶基、喹啉基、異喹啉基等。
前述碳數3~10之環烷基、碳數2~10之雜環烷基、碳數6~15之芳基、碳數2~15之雜芳基具有取代基時的取代基不特別限制,可列舉:甲基、乙基、丙基、異丙基、丁基等碳數1~10之烷基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;乙烯基氧基、丁-1-烯氧基、-OC(CF
3)=C{ CF(CF
3)
2}
2表示之基等烯基氧基;苯基、甲苯基等碳數6~10之芳基;吡咯基、吡啶基、咪唑基、㗁唑基、異㗁唑基、嘧啶基、4-胺基-2-側氧基-1,2-二氫嘧啶-1-基等碳數3~10之雜芳基;羥基;氰基;硝基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基等。此外,取代基可為1個,也可有2個以上。
A各自獨立而為碳數1~5之伸烷基。前述碳數1~5之伸烷基不特別限制,可列舉亞甲基(-CH
2-)、伸乙基(-C
2H
4-)、伸丙基(-C
3H
6-)、伸異丙基(-CH(CH
3)CH
2-)等。
又,r為0或1。
而且,Z為下列式中之任一者。
此時,來自單磷酸或二磷酸之結構所具有的羥基中,亦可有1個或2個成為陰離子之形態。具體而言,亦可具有下列結構。
此時,式(1)中,會於R
1中存在銨陽離子的相對離子,所以有時會有不具有銨鹽X
-的情形。
此等之中,R
1宜為碳數6~20之烷基、有取代或無取代之芳基(聚)氧基伸烷基,較佳為碳數8~18之烷基、有取代或無取代之苯基(聚)氧基伸烷基,更佳為辛基、癸基、十二烷基、十四烷基、十六烷基、十八烷基、苯基氧基乙基(Ph-O-C
2H
4-)、苯基二(氧基伸乙基)(Ph-(O-C
2H
4)
2-)、對(1,1,3,3-四甲基丁基)苯基二(氧基伸乙基)(p-CH
3C(CH
3)
2CH
2C(CH
3)
2-Ph-(O-C
2H
4)
2-)。
前述R
2各自獨立而為有取代或無取代之碳數1~18之烷基、有取代或無取代之碳數6~20之芳基。
碳數1~18之烷基不特別限定,可列舉甲基、乙基、丙基、異丙基、丁基、異丁基、第二丁基、第三丁基、戊基、己基、庚基、辛基、壬基、癸基、十二烷基、十四烷基、十六烷基、十八烷基等。
作為碳數1~18之烷基具有取代基時的取代基,可列舉:苯基、萘基等碳數6~20之芳基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;羥基;氰基;硝基等。
碳數6~20之芳基不特別限制,可列舉苯基、萘基、聯苯基等。
作為碳數6~20之芳基具有取代基時的取代基,可列舉:甲基、乙基、丙基、異丙基等碳數1~10之烷基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;羥基;氰基;硝基等。
此等之中,R
2宜為有取代或無取代之碳數1~18之烷基,較佳為甲基、乙基、丙基、異丙基、己基、辛基、癸基、十二烷基、十四烷基、十六烷基、十八烷基、苄基、羥基甲基、2-羥基乙基,更佳為甲基、乙基、苄基、2-羥基乙基,特佳為甲基、苄基,最佳為甲基。又,在另一實施形態中,R
2宜為經碳數6~20之芳基取代的碳數1~10之烷基,較佳為經苯基取代的碳數1~5之烷基,更佳為苄基、苯基乙基,特佳為苄基。
前述X為鹵化物離子(氟化物離子、氯化物離子、溴化物離子、碘化物離子等)、氫氧化物離子、有機磺酸離子(甲烷磺酸離子、對甲苯磺酸離子等)、四氟硼酸根、六氟磷酸根。此等之中,X宜為鹵化物離子,較佳為氯化物離子、溴化物離子。
具有碳數5~30之烷基之銨鹽的具體例,可列舉:己基三甲基溴化銨等具有己基之銨鹽;四庚基溴化銨等具有庚基之銨鹽;辛基三甲基氯化銨、辛基二甲基苄基氯化銨等具有辛基之銨鹽;癸基三甲基氯化銨、癸基二甲基苄基氯化銨等具有癸基之銨鹽;十二烷基三甲基氯化銨、十二烷基三甲基溴化銨、十二烷基乙基二甲基氯化銨、十二烷基乙基二甲基溴化銨、苄基十二烷基二甲基氯化銨、苄基十二烷基二甲基溴化銨、三(十二烷基)甲基氯化銨、三(十二烷基)甲基溴化銨等具有十二烷基之銨鹽;十四烷基三甲基溴化銨、苄基二甲基十四烷基氯化銨等具有十四烷基之銨鹽;十六烷基三甲基氯化銨、十六烷基三甲基溴化銨、對甲苯磺酸十六烷基三甲基銨、十六烷基三甲基氫氧化銨、乙基十六烷基二甲基氯化銨、乙基十六烷基二甲基溴化銨、苄基二甲基十六烷基氯化銨等具有十六烷基之銨鹽;三甲基十八烷基氯化銨、三甲基十八烷基溴化銨、二甲基二(十八烷基)氯化銨、二甲基二(十八烷基)溴化銨、苄基二甲基十八烷基氯化銨等具有十八烷基之銨鹽。
具有有取代或無取代之烷基(聚)雜伸烷基之銨鹽的具體例,可列舉三甲基丙基二(氧基伸乙基)氯化銨、三甲基丙基氧基伸乙基硫基伸乙基氯化銨等。
具有有取代或無取代之芳基(聚)雜伸烷基之銨鹽的具體例,可列舉苄基二甲基-2-{2-[4-(1,1,3,3-四甲基丁基)苯氧基]乙氧基}乙基氯化銨(氯化苯索寧;benzethonium chloride)、苄基二甲基苯基二(氧基伸乙基)氯化銨等。
具有式(2)表示之基之銨鹽的具體例,可列舉下列結構表示之化合物。
具有碳數5~30之烷基之雜芳基鹽不特別限制,可列舉有取代或無取代之含氮原子之雜芳基環所具有之氮原子之至少1個與碳數5~30之烷基鍵結而成之雜芳基陽離子的鹽。
前述含氮原子之雜芳基環不特別限制,可列舉咪唑、吡唑、㗁唑、異㗁唑(isoxazole)、噻唑、異噻唑、吡啶、吡𠯤、嗒𠯤、嘧啶、喹啉、異喹啉等之環。
作為含氮原子之雜芳基環具有取代基時的取代基,可列舉:甲基、乙基、丙基、異丙基等碳數1~4之烷基;苯基、萘基等碳數6~20之芳基;甲氧基、乙氧基、丙氧基等碳數1~6之烷氧基;羥基;氰基;硝基等。
碳數5~30之烷基不特別限制,可列舉戊基、己基、庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基等。
此等之中,碳數5~30之烷基宜為碳數6~20之烷基,較佳為碳數8~18之烷基,更佳為辛基、癸基、十二烷基、十四烷基、十六烷基、十八烷基。
具有碳數5~30之烷基之雜芳基陽離子的相對陰離子不特別限制,可列舉:氟化物離子、氯化物離子、溴化物離子、碘化物離子等鹵化物離子;氫氧化物離子;甲烷磺酸離子、對甲苯磺酸離子等有機磺酸離子;四氟硼酸根;六氟磷酸根等。此等之中,前述相對陰離子宜為鹵化物離子,較佳為氯化物離子、溴化物離子。
具有碳數5~30之烷基之雜芳基鹽的具體例,可列舉:氯化1-甲基-3-己基咪唑鎓、氯化1-辛基-3-甲基咪唑鎓、溴化1-辛基-3-甲基咪唑鎓、四氟硼酸1-辛基-3-甲基咪唑鎓、氯化1-癸基-3-甲基咪唑鎓、溴化1-癸基-3-甲基咪唑鎓、四氟硼酸1-癸基-3-甲基咪唑鎓、氯化1-十二烷基-3-甲基咪唑鎓、溴化1-十二烷基-3-甲基咪唑鎓、氯化1-十四烷基-3-甲基咪唑鎓、溴化1-十四烷基-3-甲基咪唑鎓、氯化1-十六烷基-3-甲基咪唑鎓、溴化1-十六烷基-3-甲基咪唑鎓、氯化1-十八烷基3-甲基咪唑鎓、溴化1-十八烷基-3-甲基咪唑鎓等咪唑鎓鹽;氯化3-十二烷基㗁唑鎓、溴化3-十二烷基㗁唑鎓、氯化3-十四烷基㗁唑鎓、氯化3-十六烷基㗁唑鎓等㗁唑鎓鹽;氯化3-十二烷基噻唑鎓、溴化3-十二烷基噻唑鎓、氯化3-十二烷基-4-甲基噻唑鎓、氯化3-十四烷基噻唑鎓、氯化3-十六烷基噻唑鎓等噻唑鎓鹽;氯化1-己基吡啶鎓、氯化1-辛基吡啶鎓、氯化1-癸基吡啶鎓、氯化1-十二烷基吡啶鎓、溴化1-十二烷基吡啶鎓、氯化1-十四烷基吡啶鎓、溴化1-十四烷基吡啶鎓、氯化1-十六烷基吡啶鎓、溴化1-十六烷基吡啶鎓、氯化1-十八烷基吡啶鎓、溴化1-十八烷基吡啶鎓等吡啶鎓鹽;氯化1-己基嘧啶鎓、六氟磷酸1-己基嘧啶鎓、氯化1-辛基嘧啶鎓、氯化1-癸基嘧啶鎓、氯化1-十二烷基嘧啶鎓、氯化1-十四烷基嘧啶鎓、氯化1-十六烷基嘧啶鎓等嘧啶鎓鹽;氯化十二烷基喹啉鎓、溴化十二烷基喹啉鎓、氯化十四烷基喹啉鎓、氯化十六烷基喹啉鎓等喹啉鎓鹽;氯化十二烷基異喹啉鎓、溴化十二烷基異喹啉鎓、氯化十四烷基異喹啉鎓、氯化十六烷基異喹啉鎓等異喹啉鎓鹽等。此外,該等也可以以水合物的形式使用。
此等之中,(C)金屬鎢抗蝕劑,就Ti/W蝕刻選擇比高的觀點,宜為式(1)表示之銨鹽(此處,R
1為碳數6~20之烷基,R
2為碳數1~10之烷基、經碳數6~20之芳基取代的碳數1~10之烷基)、具有有取代或無取代之芳基(聚)雜伸烷基的銨鹽、具有碳數5~30之烷基之雜芳基鹽,較佳為式(1)表示之銨鹽(此處,R
1為碳數8~20之烷基,R
2為碳數1~5之烷基、經苯基取代的碳數1~5之烷基)、具有有取代或無取代之苯基(聚)氧基伸烷基的銨鹽、具有碳數8~20之烷基之咪唑鎓鹽,更佳為辛基三甲基銨鹽、辛基二甲基苄基銨鹽、癸基三甲基銨鹽、癸基二甲基苄基銨鹽、十二烷基三甲基銨鹽、十二烷基二甲基苄基銨鹽、十四烷基三甲基銨鹽、十四烷基二甲基苄基銨鹽、十六烷基三甲基銨鹽、十六烷基二甲基苄基銨鹽、十八烷基三甲基銨鹽、十八烷基二甲基苄基銨鹽、辛基三乙基銨鹽、辛基二乙基苄基銨鹽、癸基三乙基銨鹽、癸基二乙基苄基銨鹽、十二烷基三乙基銨鹽、十二烷基二乙基苄基銨鹽、十四烷基三乙基銨鹽、十四烷基二乙基苄基銨鹽、十六烷基三乙基苄基銨鹽、十六烷基二乙基苄基銨鹽、十八烷基三乙基銨鹽、十八烷基二乙基苄基銨鹽、辛基乙基甲基苄基銨鹽、癸基乙基甲基苄基銨鹽、十二烷基乙基甲基苄基銨鹽、十四烷基乙基甲基苄基銨鹽、十六烷基乙基甲基苄基銨鹽、十八烷基乙基甲基苄基銨鹽、三甲基-2-{2-[4-(1,1,3,3-四甲基丁基)苯氧基]乙氧基}乙基氯化銨、苄基二甲基-2-{2-[4-(1,1,3,3-四甲基丁基)苯氧基]乙氧基}乙基氯化銨(氯化苯索寧)、氯化1-辛基咪唑鎓、氯化1-癸基咪唑鎓、氯化1-十二烷基咪唑鎓、氯化1-十四烷基咪唑鎓、氯化1-十六烷基咪唑鎓、氯化1-十八烷基咪唑鎓、氯化1-辛基-3-甲基咪唑鎓、氯化1-癸基-3-甲基咪唑鎓、氯化1-十二烷基-3-甲基咪唑鎓、氯化1-十四烷基-3-甲基咪唑鎓、氯化1-十六烷基-3-甲基咪唑鎓、氯化1-十八烷基-3-甲基咪唑鎓,特佳為辛基二甲基苄基銨鹽、癸基二甲基苄基銨鹽、十二烷基二甲基苄基銨鹽、十四烷基二甲基苄基銨鹽、十六烷基二甲基苄基銨鹽、十八烷基二甲基苄基銨鹽、氯化1-辛基-3-甲基咪唑鎓、氯化1-癸基-3-甲基咪唑鎓、氯化1-十二烷基-3-甲基咪唑鎓、氯化1-十四烷基-3-甲基咪唑鎓、氯化1-十六烷基-3-甲基咪唑鎓、氯化1-十八烷基-3-甲基咪唑鎓。
此外,上述(C)金屬鎢抗蝕劑可單獨使用,也可將2種以上組合使用。亦即,在較佳之一實施形態中,(C)金屬鎢抗蝕劑宜含有選自於由具有碳數5~30之烷基之銨鹽、具有有取代或無取代之芳基(聚)雜伸烷基的銨鹽、及具有碳數5~30之烷基之雜芳基鹽構成之群組中之至少一者,就Ti/W蝕刻選擇比高的觀點,較佳為含有選自於由式(1)表示之銨鹽(此處,R
1為碳數6~20之烷基,R
2為碳數1~10之烷基、經碳數6~20之芳基取代的碳數1~10之烷基)、具有有取代或無取代之苯基(聚)氧基伸烷基的銨鹽、及具有碳數5~30之烷基之雜芳基鹽構成之群組中之至少一者,更佳為含有選自於由式(1)表示之銨鹽(此處,R
1為碳數8~20之烷基,R
2為碳數1~10之烷基、經苯基取代的碳數1~5之烷基)及具有碳數8~20之烷基之咪唑鎓鹽構成之群組中之至少一者,特佳為含有選自於由辛基三甲基銨鹽、辛基二甲基苄基銨鹽、癸基三甲基銨鹽、癸基二甲基苄基銨鹽、十二烷基三甲基銨鹽、十二烷基二甲基苄基銨鹽、十四烷基三甲基銨鹽、十四烷基二甲基苄基銨鹽、十六烷基三甲基銨鹽、十六烷基二甲基苄基銨鹽、十八烷基三甲基銨鹽、十八烷基二甲基苄基銨鹽、辛基三乙基銨鹽、辛基二乙基苄基銨鹽、癸基三乙基銨鹽、癸基二乙基苄基銨鹽、十二烷基三乙基銨鹽、十二烷基二乙基苄基銨鹽、十四烷基三乙基銨鹽、十四烷基二乙基苄基銨鹽、十六烷基三乙基銨鹽、十六烷基二乙基苄基銨鹽、十八烷基三乙基銨鹽、十八烷基二乙基苄基銨鹽、辛基乙基甲基苄基銨鹽、癸基乙基甲基苄基銨鹽、十二烷基乙基甲基苄基銨鹽、十四烷基乙基甲基苄基銨鹽、十六烷基乙基甲基苄基銨鹽、十八烷基乙基甲基苄基銨鹽、三甲基-2-{2-[4-(1,1,3,3-四甲基丁基)苯氧基]乙氧基}乙基氯化銨、苄基二甲基-2-{2-[4-(1,1,3,3-四甲基丁基)苯氧基]乙氧基}乙基氯化銨(氯化苯索寧)、氯化1-辛基咪唑鎓、氯化1-癸基咪唑鎓、氯化1-十二烷基咪唑鎓、氯化1-十四烷基咪唑鎓、氯化1-十六烷基咪唑鎓、氯化1-十八烷基咪唑鎓、氯化1-辛基-3-甲基咪唑鎓、氯化1-癸基-3-甲基咪唑鎓、氯化1-十二烷基-3-甲基咪唑鎓、氯化1-十四烷基-3-甲基咪唑鎓、氯化1-十六烷基-3-甲基咪唑鎓、及氯化1-十八烷基-3-甲基咪唑鎓構成之群組中之至少一者,最佳為含有選自於由辛基二甲基苄基銨鹽、癸基二甲基苄基銨鹽、十二烷基二甲基苄基銨鹽、十四烷基二甲基苄基銨鹽、十六烷基二甲基苄基銨鹽、十八烷基二甲基苄基銨鹽、氯化1-辛基-3-甲基咪唑鎓、氯化1-癸基-3-甲基咪唑鎓、氯化1-十二烷基-3-甲基咪唑鎓、氯化1-十四烷基-3-甲基咪唑鎓、氯化1-十六烷基-3-甲基咪唑鎓、及氯化1-十八烷基-3-甲基咪唑鎓構成之群組中之至少一者。
(C)金屬鎢抗蝕劑的添加比率,相對於前述蝕刻劑之全部質量宜為0.0001~5質量%,較佳為0.001~1質量%,更佳為0.003~0.5質量%,特佳為0.004~0.08質量%。
pH調整劑
蝕刻劑也可視需要含有pH調整劑。作為前述pH調整劑,例如可使用除(A)氧化劑、(B)氟化合物以外的酸、鹼。
作為前述酸,可列舉氯化氫、溴化氫、碘化氫、硫酸、硝酸、甲烷磺酸、三氟甲烷磺酸、苯磺酸、對甲苯磺酸、10-樟腦磺酸、及該等的鹽。此時,作為前述鹽,可列舉:氯化銨、溴化銨、碘化銨、硫酸銨、硝酸銨等銨鹽;甲基胺鹽酸鹽、二甲基胺鹽酸鹽、二甲基胺氫溴酸鹽、甲基胺硫酸鹽等烷基銨鹽等。
作為前述鹼,可列舉氫氧化鋰、氫氧化鈉、氫氧化鉀、氫氧化銣、氫氧化銫、氫氧化鈹、氫氧化鎂、氫氧化鈣、氫氧化鍶、氫氧化鋇、氨、三乙胺等。
上述之中,pH調整劑宜為氯化氫、溴化氫、碘化氫、硫酸、硝酸、甲烷磺酸、氨,較佳為硫酸、硝酸、氨,更佳為硫酸、硝酸。
溶劑
蝕刻劑宜含有溶劑。前述溶劑具有使蝕刻劑中含有的各成分均勻分散的功能、稀釋的功能等。
作為前述溶劑,可列舉水、有機溶劑。
前述水不特別限制,宜為藉由蒸餾、離子交換處理、過濾處理、各種吸附處理等將金屬離子、有機雜質、微粒粒子等予以去除後所獲得之水,更宜為純水,尤其宜為超純水。
前述有機溶劑不特別限制,可列舉:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、第三丁醇等醇;乙二醇、丙二醇、新戊二醇、1,2-己二醇、1,6-己二醇、2-乙基己烷-1,3-二醇、甘油等多元醇;二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇單丁醚、丙二醇單甲醚、丙二醇單乙醚、二丙二醇單甲醚、三丙二醇單甲醚、二丙二醇二甲醚、二丙二醇單乙醚、丙二醇正丙醚、二丙二醇正丙醚、三丙二醇正丙醚、丙二醇正丁醚、二丙二醇正丁醚、三丙二醇正丁醚、丙二醇苯醚等二醇醚等。
上述之中,溶劑較佳為水。此外,前述溶劑可單獨使用,也可將2種以上組合使用。
就溶劑尤其水的添加比率而言,相對於蝕刻劑之全部質量宜為50質量%以上,較佳為80質量%以上,更佳為90質量%以上,特佳為90~99.5質量%。
碘捕捉劑
在上述(A)氧化劑含有碘的含氧酸時,蝕刻劑宜更含有碘捕捉劑。
碘捕捉劑不特別限制,可列舉:丙酮、丁酮、2-甲基-2-丁酮、3,3-二甲基-2-丁酮、4-羥基-2-丁酮、2-戊酮、3-戊酮、3-甲基-2-戊酮、4-甲基-2-戊酮、2-甲基-3-戊酮、5-甲基-3-戊酮、2,4-二甲基-3-戊酮、5-羥基-2-戊酮、4-羥基-4-甲基-2-戊酮、2-己酮、3-己酮、2-庚酮、3-庚酮、4-庚酮、5-甲基-2-庚酮、5-甲基-3-庚酮、2,6-二甲基-4-庚酮、2-辛酮、3-辛酮、4-辛酮、環己酮、2,6-二甲基環己酮、2-乙醯基環己酮、薄荷酮、環戊酮、二環己基酮等脂肪族酮;2,5-己二酮、2,4-戊二酮、乙醯基丙酮等脂肪族二酮;苯乙酮、1-苯基乙酮、二苯基酮等芳香族酮等。此等之中,碘捕捉劑宜為脂肪族酮,較佳為4-甲基-2-戊酮、5-甲基-3-戊酮、2,4-二甲基-3-戊酮、環己酮,更佳為4-甲基-2-戊酮。此外,此等碘捕捉劑可單獨使用,也可將2種以上組合使用。
低介電常數鈍化劑
蝕刻劑也可更含有低介電常數鈍化劑。低介電常數鈍化劑具有防止或抑制蝕刻低介電常數膜例如絕緣膜之功能。
低介電常數鈍化劑不特別限制,可列舉:硼酸;五硼酸銨、四硼酸鈉等硼酸鹽;3-羥基-2-萘甲酸、丙二酸、亞胺基二乙酸等羧酸。
此等低介電常數鈍化劑可單獨使用,也可將2種以上組合使用。
低介電常數鈍化劑的添加比率,相對於前述蝕刻劑之全部質量宜為0.01~2質量%,較佳為0.02~1質量%,更佳為0.03~0.5質量%。
添加劑
蝕刻劑也可更含有添加劑。作為該添加劑,可列舉界面活性劑、螯合劑、消泡劑、含矽化合物等。
蝕刻劑之物性
蝕刻劑之pH宜為0.5~5.0,較佳為1.0~4.0,更佳為1.0~3.0。
蝕刻劑的金屬鎢之蝕刻速度宜為5.0Å/min以下,較佳為3.0Å/min以下,更佳為2.0Å/min以下,特佳為1.5Å/min以下,最佳為0.1~1.0Å/min。金屬鎢之蝕刻速度為5.0Å/min以下的話,Ti/W蝕刻選擇比會提高,故較理想。此外,蝕刻劑的金屬鎢之蝕刻速度意指藉由實施例之方法測得之值。
蝕刻劑的鈦、鈦合金之蝕刻速度宜為10Å/min以上,較佳為30Å/min以上,更佳為50Å/min以上,又更佳為60Å/min,特佳為80Å/min以上。鈦、鈦合金之蝕刻速度為10Å/min以上的話,Ti/W蝕刻選擇比會提高,故較理想。此外,蝕刻劑的鈦、鈦合金之蝕刻速度意指藉由實施例之方法測得之值。
蝕刻劑的絕緣層材料之蝕刻速度宜為5.0Å/min以下,較佳為3.0Å/min以下,更佳為2.0Å/min以下,特佳為1.5Å/min以下,最佳為1.0Å/min以下。絕緣層材料之蝕刻速度為5.0Å/min以下的話,半導體基板的形狀得到維持且就半導體元件而言的性能提高,故較理想。此外,蝕刻劑的絕緣層材料之蝕刻速度意指藉由實施例之方法測得之值。
蝕刻劑的Ti/W蝕刻選擇比(鈦、鈦合金之蝕刻速度/金屬鎢之蝕刻速度)宜為10以上,較佳為30以上,更佳為35以上,特佳為70以上,最佳為100以上。Ti/W蝕刻選擇比為10以上的話,可製造高性能的記憶體元件用半導體基板,故較理想。
(接觸)
就經步驟(1)後的半導體基板與蝕刻劑的接觸方法而言,不特別限制,可適當採用公知的技術。具體而言,可將半導體基板浸漬於蝕刻劑中,也可用蝕刻劑對半導體基板進行噴霧,也可進行滴加(單片旋轉處理等)。此時,亦可將前述浸漬重複2次以上,亦可將噴霧重複2次以上,亦可將滴加重複2次以上,亦可將浸漬、噴霧、及滴加予以組合。
接觸溫度不特別限制,宜為0~90℃,較佳為15~70℃,更佳為20~60℃。
接觸時間不特別限制,宜為10秒~3小時,較佳為30秒~1小時,更佳為1~45分鐘,特佳為1~5分鐘。
可藉由使經步驟(1)後的半導體基板與蝕刻劑接觸來進行鈦、鈦合金的選擇性蝕刻。此時,由於已在步驟(1)去除了氧化鎢膜的至少一部分,所以利用蝕刻劑所為之鈦、鈦合金的選擇性蝕刻會更理想地進行。
(記憶體元件用半導體基板)
藉由步驟(2)而獲得之記憶體元件用半導體基板可使用於DRAM等記憶體元件。藉由步驟(2)而獲得之記憶體元件可實現小型化、高功能化。
<套組>
依照本發明之一形態,提供一種套組。前述套組含有上述前處理劑及上述蝕刻劑。亦即,前述套組可用於記憶體元件用半導體基板之製造用途。將前處理劑及蝕刻劑製成套組的話,在對於具有氧化鎢膜之半導體基板進行鈦、鈦合金的選擇性蝕刻時,會有助於實施上述步驟(1)及步驟(2)。
[實施例]
以下,舉實施例來具體地說明本發明,但本發明不限於此等。
[實施例1]
(步驟(1))
準備具有氧化鎢(WO
3)膜之基板、具有金屬鎢(W)膜之基板、具有氮化鈦(TiN)膜之基板、及具有氧化矽(th-Ox)膜之基板,針對各基板實施步驟(1),並測定前處理劑對各膜之蝕刻速度。
製備前處理劑。具體而言,將作為WO
3蝕刻劑之氟化氫(HF)添加至純水中並攪拌,藉此製得前處理劑。此時,前述氟化氫的添加比率,相對於前處理劑之全部質量為0.1質量%。此外,前處理劑之pH為2.2。pH係使用堀場製作所(股)公司製桌上型pH計(F-71)及pH電極(9615S-10D)測定在23℃下的前處理劑的pH而得。
(1-A)對於具有氧化鎢(WO
3)膜之基板的處理
於矽晶圓上利用物理氣相沉積法將氧化鎢(WO
3)製膜至厚度達3000Å,並予以裁切成1cm×1cm(浸漬處理面積:1cm
2)的大小,藉此製得氧化鎢製膜樣品。
在已製備好的前處理劑10g中,將氧化鎢製膜樣品於預定之處理溫度下進行5分鐘浸漬處理。使用1質量%之硝酸水溶液將浸漬處理後之前處理劑稀釋至10~20倍而製得測定樣品。使用ICP發射光譜分析裝置(ICP-OES)即Avio200(PerkinElmer製)測得測定樣品中的鎢濃度。
此時,檢量線製作用樣品以下列方法製備。亦即,將鎢標準液(鎢濃度:1000ppm,富士軟片和光(股)公司製)以1質量%之硝酸水溶液進行稀釋,藉此製得鎢之濃度為25ppb、12.5ppb、及2.5ppb之檢量線製作用樣品。
從使用檢量線製作用樣品而算出之測定樣品之鎢濃度計算稀釋前的鎢濃度,並將稀釋前的鎢濃度與測定所使用之前處理劑之量(測定樣品之稀釋前之量) 代入下列式中,以算出氧化鎢膜之蝕刻量。
此外,上述式中,231.84(g/mol)為氧化鎢(WO
3)的分子量,7.16(g/cm
3)為氧化鎢的密度,1cm
2為氧化鎢製膜樣品的浸漬處理面積,183.84(g/mol)為金屬鎢(W)的分子量。
將算出之氧化鎢膜之蝕刻量除以使用前處理劑進行浸漬處理的時間,以算出氧化鎢膜之蝕刻速度(E.R.)。其結果,前處理劑對氧化鎢膜之蝕刻速度(E.R.)為31Å/min。
(1-B)對於具有金屬鎢(W)膜之基板的處理
於矽晶圓上利用物理氣相沉積法將鎢(W)製膜至厚度達1000Å,並予以裁切成1cm×1cm(浸漬處理面積:1cm
2)的大小,藉此製得金屬鎢製膜樣品。
除了使用金屬鎢製膜樣品、浸漬處理時間為2分鐘以外,以和氧化鎢膜之蝕刻速度之測定法同樣的方法來製備測定樣品並對測定樣品中的鎢濃度進行測定。
從使用檢量線製作用樣品而算出之測定樣品之鎢濃度計算稀釋前的鎢濃度,並將稀釋前的鎢濃度與測定所使用之前處理劑之量(測定樣品之稀釋前之量)代入下列式中,以算出金屬鎢膜之蝕刻量。
此外,上述式中19.25(g/cm
3)為金屬鎢的密度,1cm
2為鎢製膜樣品的浸漬處理面積。
將算出之金屬鎢膜之蝕刻量除以使用前處理劑進行浸漬處理的時間,以算出金屬鎢膜之蝕刻速度(E.R.)。其結果,前處理劑對金屬鎢膜之蝕刻速度(E.R.)為2.5Å/min。
(1-C)對於具有氮化鈦(TiN)膜之基板的處理
於矽晶圓上利用物理氣相沉積法將氮化鈦(TiN)製膜至厚度達1000Å,並予以裁切成2cm×2cm(浸漬處理面積:4cm
2)的大小,藉此製得氮化鈦製膜樣品。
使用螢光X射線裝置EA1200VX(Hitachi high-tech製)來測定氮化鈦製膜樣品之膜厚。
在已製備好的前處理劑10g中,將氮化鈦製膜樣品於預定之處理溫度下進行5分鐘浸漬處理。
以和上述同樣的方法測定經前處理劑浸漬處理後之氮化鈦製膜樣品之膜厚。
算出前處理劑浸漬處理前後之氮化鈦製膜樣品的膜厚差,並將其除以使用前處理劑進行浸漬處理的時間,以算出氮化鈦膜之蝕刻速度(E.R.)。其結果,前處理劑對氮化鈦膜之蝕刻速度(E.R.)為5Å/min。
(1-D)對於具有氧化矽(th-Ox)膜之基板的處理
藉由矽晶圓之熱氧化而將氧化矽製膜至厚度達1000Å,並予以裁切成1cm×1cm(浸漬處理面積:1cm
2)的大小,藉此製得氧化矽製膜樣品。
使用光學式膜厚計n&k1280(n&k科技公司製)來測定氧化矽製膜樣品之膜厚。
在已製備好的前處理劑10g中,將氧化矽製膜樣品於預定之處理溫度下進行30分鐘浸漬處理。
以和上述同樣的方法測定經浸漬處理後之氧化矽製膜樣品之膜厚。
算出處理前後之氧化矽製膜樣品的膜厚差,並將其除以使用前處理劑進行浸漬處理的時間,以算出氧化矽膜之蝕刻速度(E.R.)。其結果,前處理劑對氧化矽膜之蝕刻速度(E.R.)為2.8Å/min。
(1-E)算出WO
3/W蝕刻選擇比
將前處理劑對氧化鎢膜之蝕刻速度(E.R.)除以前處理劑對金屬鎢膜之蝕刻速度(E.R.),以算出WO
3/W蝕刻選擇比。其結果,WO
3/W蝕刻選擇比為12。
(步驟(2))
針對具有金屬鎢(W)膜之基板、具有氮化鈦(TiN)膜之基板、及具有氧化矽(th-Ox)膜之基板實施步驟(2),並測定蝕刻劑對各膜之蝕刻速度。此外,針對具有氮化鈦(TiN)膜之基板,係使用了經步驟(1)後的氮化鈦製膜樣品。又,針對具有金屬鎢(W)膜之基板及具有氧化矽(th-Ox)膜之基板,係使用了以和步驟(1)同樣的方法另外新製成的金屬鎢製膜樣品及氧化矽製膜樣品。
製備蝕刻劑。具體而言,將作為氧化劑之碘酸(HIO
3)、作為氟化合物之氟化氫(HF)、及作為金屬鎢抗蝕劑之氯化1-十二烷基吡啶鎓(DPC)添加至純水中並攪拌,而製得蝕刻劑。此時,碘酸、氟化氫、及氯化1-十二烷基吡啶鎓(DPC)的添加比率,相對於蝕刻劑之全部質量分別為0.018質量%、0.05質量%、及0.005質量%。又,蝕刻劑之pH為2.4。
(2-A)對於具有金屬鎢(W)膜之基板的處理
在已製備好的蝕刻劑10g中,將金屬鎢製膜樣品於預定之處理溫度下進行2分鐘浸漬處理。然後,以和上述(1-B)同樣的方法算出金屬鎢膜之蝕刻速度(E.R.)。其結果,蝕刻劑對金屬鎢膜之蝕刻速度(E.R.)為2.1Å/min。
(2-B)對於經步驟(1)後的具有氮化鈦(TiN)膜之基板的處理
在已製備好的蝕刻劑10g中,將經步驟(1)後的氮化鈦製膜樣品於預定之處理溫度下進行2分鐘浸漬處理。然後,以和上述(1-C)同樣的方法算出氮化鈦膜之蝕刻速度(E.R.)。其結果,蝕刻劑對氮化鈦膜之蝕刻速度(E.R.)為85Å/min。
(2-C)對於具有氧化矽(th-Ox)膜之基板的處理
在已製備好的蝕刻劑10g中,將氧化矽製膜樣品於預定之處理溫度下進行30分鐘浸漬處理。然後,以和上述(1-D)同樣的方法算出氧化矽膜之蝕刻速度(E.R.)。其結果,蝕刻劑對氧化矽膜之蝕刻速度(E.R.)為0.8Å/min。
(2-D)TiN/W蝕刻選擇比
將蝕刻劑對氮化鈦膜之蝕刻速度(E.R.)除以蝕刻劑對金屬鎢膜之蝕刻速度(E.R.),以算出TiN/W蝕刻選擇比。其結果,TiN/W蝕刻選擇比為40。
[評價]
針對前處理劑,評價金屬鎢(W)與氮化鈦(TiN)之腐蝕電位差及氧化鈦去除能力。
(金屬鎢(W)與氮化鈦(TiN)之腐蝕電位差)
金屬鎢(W)之腐蝕電位以下列方法測得。亦即,使用北斗電工製HZ7000,實施線性掃描伏安法(linear sweep voltammetry)測定。具體而言,使用了作為工作電極之在0.5質量%氨水中於23℃浸漬了1分鐘之金屬鎢膜、作為相對電極之鉑、作為參考電極之銀/氯化銀(3.3M氯化鉀水溶液)、鹽橋(含0.5M氯化鉀之洋菜膠)來進行測定。從比起腐蝕電位低30mV~200mV的電位以2mV/秒之速度對於金屬鎢施加電位,並將在各電位下之電流值作圖(塔菲爾圖;Tafel plot)。將電流值成為最低時的電位定義為金屬鎢之腐蝕電位。其結果,金屬鎢(W)之腐蝕電位為-109mV。
又,氮化鈦(TiN)之腐蝕電位以下列方法測得。亦即,使用北斗電工製HZ7000,實施線性掃描伏安法測定。具體而言,使用了作為工作電極之在1質量%氟化氫水溶液中於23℃浸漬了1分鐘之氮化鈦膜、作為相對電極之鉑、作為參考電極之銀/氯化銀(3.3M氯化鉀水溶液)、鹽橋(含0.5M氯化鉀之洋菜膠)來進行測定。從比起腐蝕電位低30mV~200mV的電位以2mV/秒之速度對於氮化鈦施加電位,並將在各電位下的電流值作圖(塔菲爾圖)。將電流值成為最低時的電位定義為氮化鈦之腐蝕電位。其結果,氮化鈦(TiN)之腐蝕電位為-73mV。
然後,算出金屬鎢(W)與氮化鈦(TiN)之腐蝕電位差(W之腐蝕電位-TiN之腐蝕電位),結果為36mV。
(氧化鈦去除能力)
於矽晶圓上利用物理氣相沉積法將氮化鈦(TiN)製膜至厚度達1000Å,並予以裁切成2cm×2cm(浸漬處理面積:4cm
2)的大小。然後,將其於20℃下在大氣中曝露30天,藉此使經製膜而得之氮化鈦膜之表面氧化而製得氧化鈦去除能力測定樣品。
將氧化鈦去除能力測定樣品,在已於步驟(1)製備好的前處理劑(0.1質量%HF水溶液)10g中於30℃下進行5分鐘浸漬處理,藉此得到前處理後樣品。然後,使用已於步驟(2)製備好的蝕刻劑,並以和(2-B)同樣的方法算出氮化鈦膜之蝕刻速度(E.R.),結果為85Å/min。此外,氮化鈦膜之蝕刻速度(E.R.)越高,則可以說越能夠在步驟(1)中藉由前處理劑來去除氧化鈦膜。
[實施例1-2~1-10]
按照下列表1所示來變更所添加之成分等,並製得前處理劑。將前處理劑之組成等和實施例1之組成等一併示於下列表1。
又,以和實施例1同樣方式來實施步驟(1)。將氧化鎢(W)膜、金屬鎢(W)膜、氮化鈦(TiN)膜、及氧化矽膜之蝕刻速度(E.R.);WO
3/W蝕刻選擇比;金屬鎢(W)之腐蝕電位、氮化鈦(TiN)之腐蝕電位、及金屬鎢(W)與氮化鈦(TiN)之腐蝕電位差;以及氧化鈦去除能力的測定結果和實施例1之結果一併示於下列表2。此外,就氧化鈦去除能力之測定中使用之蝕刻劑而言,係使用了和實施例1中所使用者相同的蝕刻劑。
由表2之結果可知,實施例1及實施例1-2~1-10皆係WO
3之蝕刻速度(E.R.)大。所以,實施例1及實施例1-2~1-10係處理量不降低且能夠防止前處理時之金屬鎢之蝕刻。因此,使用藉由步驟(1)而獲得之半導體基板來實施步驟(2)的話,能夠以高生產效率製造高功能之記憶體元件用半導體基板。
[實施例2-2~2-10]
按照下列表3所示來變更所添加之成分等,並製得蝕刻劑。將蝕刻劑之組成等和實施例1之蝕刻劑之組成等一併示於下列表3。
此外,實施例中使用之DPC、CPC、DMIC、CTAB、OMIC、及BZC具有下列結構。
和實施例1同樣地針對具有金屬鎢(W)膜之基板、具有氮化鈦(TiN)膜之基板、及具有氧化矽(th-Ox)膜之基板實施步驟(2)。此外,針對具有氮化鈦(TiN)膜之基板,係使用了經步驟(1)後的氮化鈦製膜樣品。又,針對具有金屬鎢(W)膜之基板及具有氧化矽(th-Ox)膜之基板,係使用了以和步驟(1)同樣的方法另外新製成的金屬鎢製膜樣品及氧化矽製膜樣品。將金屬鎢(W)膜、氮化鈦(TiN)膜、及氧化矽膜之蝕刻速度(E.R.);以及TiN/W蝕刻選擇比的測定結果和實施例1之結果一併示於下列表4。
由表4之結果可知,實施例1及實施例2-2~2-10係已於步驟(1)中有效率地去除了氧化鎢,所以能夠於步驟(2)中選擇性地蝕刻氮化鈦,能夠以高生產效率製造高功能之記憶體元件用半導體基板。
10:半導體基板(步驟(1)前)
11:具有凹部之矽基板
12:絕緣膜
13:阻隔膜
14:金屬鎢膜
15:氧化鎢膜
16:氧化鈦膜
20:半導體基板(步驟(1)後)
21:具有凹部之矽基板
22:絕緣膜
23:阻隔膜
24:金屬鎢膜
30:半導體基板(步驟(2)後)
31:具有凹部之矽基板
32:絕緣膜
33:經蝕刻後之阻隔膜
34:金屬鎢膜
[圖1]係本發明之步驟(1)的示意圖。
Claims (8)
- 一種記憶體元件用半導體基板之製造方法,包括下列步驟: 步驟(1),使具有含有鈦及鈦合金中之至少一者的含鈦膜、金屬鎢膜、及氧化鎢膜的半導體基板與前處理劑接觸,而去除該氧化鎢膜的至少一部分;以及 步驟(2),使經步驟(1)後的半導體基板與蝕刻劑接觸,而去除該含鈦膜的至少一部分; 該前處理劑含有選自於由酸、氨、及銨鹽構成之群組中之至少一者之氧化鎢蝕刻劑。
- 如請求項1之記憶體元件用半導體基板之製造方法,其中,該前處理劑之pH為0.1~13。
- 如請求項1或2之記憶體元件用半導體基板之製造方法,其中,該氧化鎢蝕刻劑含有選自於由氟化氫、氯化氫、溴化氫、碘化氫、硫酸、硝酸、及磷酸構成之群組中之至少一者。
- 如請求項1至3中任一項之記憶體元件用半導體基板之製造方法,其中, 該半導體基板更含有氧化鈦膜,且 該步驟(1)更包含將該氧化鈦膜的至少一部分去除之步驟。
- 如請求項1至4中任一項之記憶體元件用半導體基板之製造方法,其中, 該蝕刻劑含有(A)氧化劑、(B)氟化合物、及(C)金屬鎢抗蝕劑, 該(A)氧化劑的添加比率,相對於該蝕刻劑之全部質量為0.0001~10質量%, 該(B)氟化合物的添加比率,相對於該蝕刻劑之全部質量為0.005~10質量%, 該(C)金屬鎢抗蝕劑的添加比率,相對於該蝕刻劑之全部質量為0.0001~5質量%。
- 如請求項5之記憶體元件用半導體基板之製造方法,其中,該(A)氧化劑含有選自於由過氧酸、鹵素含氧酸、及該等的鹽構成之群組中之至少一者。
- 如請求項5或6之記憶體元件用半導體基板之製造方法,其中,該(B)氟化合物含有選自於由氟化氫(HF)、四氟硼酸(HBF 4)、六氟矽酸(H 2SiF 6)、六氟鋯酸(H 2ZrF 6)、六氟鈦酸(H 2TiF 6)、六氟磷酸(HPF 6)、六氟鋁酸(H 2AlF 6)、六氟鍺酸(H 2GeF 6)、及該等的鹽構成之群組中之至少一者。
- 如請求項5至7中任一項之記憶體元件用半導體基板之製造方法,其中,該(C)金屬鎢抗蝕劑含有選自於由下列式(1)表示之銨鹽及具有碳數5~30之烷基之雜芳基鹽構成之群組中之至少一者; 上述式(1)中, R 1為碳數5~30之烷基、有取代或無取代之烷基(聚)雜伸烷基、有取代或無取代之芳基(聚)雜伸烷基、下列式(2)表示之基, 上述式中, Cy為有取代或無取代之碳數3~10之環烷基、有取代或無取代之碳數2~10之雜環烷基、有取代或無取代之碳數6~15之芳基、有取代或無取代之碳數2~15之雜芳基, A各自獨立而為碳數1~5之伸烷基, r為0或1, Z為下列式中之任一者; R 2各自獨立而為有取代或無取代之碳數1~18之烷基、有取代或無取代之碳數6~20之芳基, X為鹵化物離子、氫氧化物離子、有機磺酸離子、四氟硼酸根、六氟磷酸根。
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JP (1) | JPWO2022202646A1 (zh) |
KR (1) | KR20230159521A (zh) |
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US6534415B2 (en) * | 1999-12-03 | 2003-03-18 | United Microelectronics Corp. | Method of removing polymer residues after tungsten etch back |
JP2014093407A (ja) * | 2012-11-02 | 2014-05-19 | Fujifilm Corp | エッチング液、これを用いたエッチング方法及び半導体素子の製造方法 |
TWI642763B (zh) * | 2014-01-27 | 2018-12-01 | 三菱瓦斯化學股份有限公司 | 氮化鈦除去用液體組成物、利用該液體組成物之半導體元件之洗滌方法、及半導體元件之製造方法 |
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US20240170278A1 (en) | 2024-05-23 |
KR20230159521A (ko) | 2023-11-21 |
CN117015849A (zh) | 2023-11-07 |
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