TWI419896B - A metal compound, a method for producing a chemical vapor-containing raw material and a film containing a metal - Google Patents
A metal compound, a method for producing a chemical vapor-containing raw material and a film containing a metal Download PDFInfo
- Publication number
- TWI419896B TWI419896B TW097141862A TW97141862A TWI419896B TW I419896 B TWI419896 B TW I419896B TW 097141862 A TW097141862 A TW 097141862A TW 97141862 A TW97141862 A TW 97141862A TW I419896 B TWI419896 B TW I419896B
- Authority
- TW
- Taiwan
- Prior art keywords
- film
- chemical vapor
- raw material
- metal
- metal compound
- Prior art date
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- 150000002736 metal compounds Chemical class 0.000 title claims description 49
- 239000002994 raw material Substances 0.000 title claims description 46
- 239000000126 substance Substances 0.000 title claims description 41
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 229910052751 metal Inorganic materials 0.000 title claims description 26
- 239000002184 metal Substances 0.000 title claims description 26
- 239000010408 film Substances 0.000 claims description 87
- 238000000034 method Methods 0.000 claims description 59
- 239000010936 titanium Substances 0.000 claims description 24
- 238000005229 chemical vapour deposition Methods 0.000 claims description 18
- 238000001947 vapour-phase growth Methods 0.000 claims description 17
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 150000004767 nitrides Chemical class 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 229910052801 chlorine Inorganic materials 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052735 hafnium Chemical group 0.000 claims description 8
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical group [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 6
- 125000005843 halogen group Chemical group 0.000 claims description 5
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 description 27
- 239000007789 gas Substances 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 19
- 239000002131 composite material Substances 0.000 description 19
- 239000002243 precursor Substances 0.000 description 16
- -1 alcohol compound Chemical class 0.000 description 15
- 238000000231 atomic layer deposition Methods 0.000 description 14
- 238000000151 deposition Methods 0.000 description 14
- 239000000460 chlorine Substances 0.000 description 11
- 230000008021 deposition Effects 0.000 description 11
- 239000003960 organic solvent Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 9
- 238000005979 thermal decomposition reaction Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 239000013110 organic ligand Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 229910052746 lanthanum Inorganic materials 0.000 description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical class CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- 239000012434 nucleophilic reagent Substances 0.000 description 5
- 230000008016 vaporization Effects 0.000 description 5
- 238000005160 1H NMR spectroscopy Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- NEGBOTVLELAPNE-UHFFFAOYSA-N [Ti].[Ce] Chemical compound [Ti].[Ce] NEGBOTVLELAPNE-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- UHOVQNZJYSORNB-MZWXYZOWSA-N benzene-d6 Chemical compound [2H]C1=C([2H])C([2H])=C([2H])C([2H])=C1[2H] UHOVQNZJYSORNB-MZWXYZOWSA-N 0.000 description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 4
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000000921 elemental analysis Methods 0.000 description 4
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 4
- 238000002309 gasification Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
- MDAXKAUIABOHTD-UHFFFAOYSA-N 1,4,8,11-tetraazacyclotetradecane Chemical compound C1CNCCNCCCNCCNC1 MDAXKAUIABOHTD-UHFFFAOYSA-N 0.000 description 2
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 2
- NWFVDKHZNWEXAD-UHFFFAOYSA-N 1-tert-butylcyclopenta-1,3-diene Chemical compound CC(C)(C)C1=CC=CC1 NWFVDKHZNWEXAD-UHFFFAOYSA-N 0.000 description 2
- OISVCGZHLKNMSJ-UHFFFAOYSA-N 2,6-dimethylpyridine Chemical compound CC1=CC=CC(C)=N1 OISVCGZHLKNMSJ-UHFFFAOYSA-N 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 2
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 2
- MIMZQOBIADUIHQ-UHFFFAOYSA-N [Ce].[La].[Ti] Chemical compound [Ce].[La].[Ti] MIMZQOBIADUIHQ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 125000005265 dialkylamine group Chemical group 0.000 description 2
- LNKYFCABELSPAN-UHFFFAOYSA-N ethyl(methyl)azanide;titanium(4+) Chemical compound [Ti+4].CC[N-]C.CC[N-]C.CC[N-]C.CC[N-]C LNKYFCABELSPAN-UHFFFAOYSA-N 0.000 description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 2
- LIWAQLJGPBVORC-UHFFFAOYSA-N ethylmethylamine Chemical compound CCNC LIWAQLJGPBVORC-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- TXGJTWACJNYNOJ-UHFFFAOYSA-N hexane-2,4-diol Chemical compound CCC(O)CC(C)O TXGJTWACJNYNOJ-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000768 polyamine Polymers 0.000 description 2
- TVSBRLGQVHJIKT-UHFFFAOYSA-N propan-2-ylcyclopentane Chemical compound CC(C)C1CCCC1 TVSBRLGQVHJIKT-UHFFFAOYSA-N 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 150000003613 toluenes Chemical class 0.000 description 2
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- BVPKYBMUQDZTJH-UHFFFAOYSA-N 1,1,1-trifluoro-5,5-dimethylhexane-2,4-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(F)(F)F BVPKYBMUQDZTJH-UHFFFAOYSA-N 0.000 description 1
- SHXHPUAKLCCLDV-UHFFFAOYSA-N 1,1,1-trifluoropentane-2,4-dione Chemical compound CC(=O)CC(=O)C(F)(F)F SHXHPUAKLCCLDV-UHFFFAOYSA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- BGYBONWLWSMGNV-UHFFFAOYSA-N 1,4,7,10,13,16,19,22-octaoxacyclotetracosane Chemical compound C1COCCOCCOCCOCCOCCOCCOCCO1 BGYBONWLWSMGNV-UHFFFAOYSA-N 0.000 description 1
- QBPPRVHXOZRESW-UHFFFAOYSA-N 1,4,7,10-tetraazacyclododecane Chemical compound C1CNCCNCCNCCN1 QBPPRVHXOZRESW-UHFFFAOYSA-N 0.000 description 1
- SIUWDFVMEASCRP-UHFFFAOYSA-N 1-(2-methoxyethoxy)-2-methylpropan-2-ol Chemical compound COCCOCC(C)(C)O SIUWDFVMEASCRP-UHFFFAOYSA-N 0.000 description 1
- UFOXNPJWBCYEJE-UHFFFAOYSA-N 1-(2-methoxyethoxy)heptane-3,5-dione Chemical compound COCCOCCC(CC(CC)=O)=O UFOXNPJWBCYEJE-UHFFFAOYSA-N 0.000 description 1
- GHJATKVLNMETBA-UHFFFAOYSA-N 1-(2-methylpropyl)cyclopenta-1,3-diene Chemical compound CC(C)CC1=CC=CC1 GHJATKVLNMETBA-UHFFFAOYSA-N 0.000 description 1
- JCALRHVFTLBTOZ-UHFFFAOYSA-N 1-butoxy-2-methylpropan-2-ol Chemical compound CCCCOCC(C)(C)O JCALRHVFTLBTOZ-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- FTFYDDRPCCMKBT-UHFFFAOYSA-N 1-butylcyclopenta-1,3-diene Chemical compound CCCCC1=CC=CC1 FTFYDDRPCCMKBT-UHFFFAOYSA-N 0.000 description 1
- BCYNAHGOLUTMDM-UHFFFAOYSA-N 1-ethoxy-2-methylpropan-2-ol Chemical compound CCOCC(C)(C)O BCYNAHGOLUTMDM-UHFFFAOYSA-N 0.000 description 1
- IQSUNBLELDRPEY-UHFFFAOYSA-N 1-ethylcyclopenta-1,3-diene Chemical compound CCC1=CC=CC1 IQSUNBLELDRPEY-UHFFFAOYSA-N 0.000 description 1
- QNLXXWOBNIYLGO-UHFFFAOYSA-N 1-methoxy-2,2,6,6-tetramethylheptane-3,5-dione Chemical compound COCC(C)(C)C(=O)CC(=O)C(C)(C)C QNLXXWOBNIYLGO-UHFFFAOYSA-N 0.000 description 1
- MXUXZWFVAPTPAG-UHFFFAOYSA-N 1-methoxy-2-methylpropan-2-ol Chemical compound COCC(C)(C)O MXUXZWFVAPTPAG-UHFFFAOYSA-N 0.000 description 1
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 1
- AVFZOVWCLRSYKC-UHFFFAOYSA-N 1-methylpyrrolidine Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 description 1
- RZPAXISDLOEXPI-UHFFFAOYSA-N 1-propylcyclopenta-1,3-diene Chemical compound CCCC1=CC=CC1 RZPAXISDLOEXPI-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
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- GJYXGIIWJFZCLN-UHFFFAOYSA-N octane-2,4-dione Chemical compound CCCCC(=O)CC(C)=O GJYXGIIWJFZCLN-UHFFFAOYSA-N 0.000 description 1
- BTNXBLUGMAMSSH-UHFFFAOYSA-N octanedinitrile Chemical compound N#CCCCCCCC#N BTNXBLUGMAMSSH-UHFFFAOYSA-N 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- OOFGXDQWDNJDIS-UHFFFAOYSA-N oxathiolane Chemical compound C1COSC1 OOFGXDQWDNJDIS-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- WQIQNKQYEUMPBM-UHFFFAOYSA-N pentamethylcyclopentadiene Chemical compound CC1C(C)=C(C)C(C)=C1C WQIQNKQYEUMPBM-UHFFFAOYSA-N 0.000 description 1
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012048 reactive intermediate Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/308—Oxynitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Electrodes Of Semiconductors (AREA)
Description
本發明係關於一種具有特定結構之新穎金屬化合物、含有其之化學氣相成長用原料及使用該原料的含金屬之薄膜之製造方法。
含有鈦、鋯或鉿之薄膜係用作高介電體電容器、強介電體電容器、閘極膜、阻擋膜、閘極絕緣膜等電子零件之電子部件,或光學波導、光開關、光放大器等光通訊用裝置之光學部件。
作為上述薄膜之製造方法,可列舉塗布熱分解法或溶膠-凝膠法等MOD法(Metal-organic Deposition method,有機金屬分解法),CVD法(Chemical Vapor Deposition method,化學氣相沈積法)或ALD法(atomic layer deposition,原子層沈積法)等化學氣相成長法等,由於將CVD法、ALD法等之前驅物氣化而進行使用之化學氣相成長法具有成分控制性、階梯覆蓋性優異,適合量產,可進行混成積體化等多個優點,故而係最為適宜之製造製程。作為CVD法、ALD法之前驅物,係利用使用有機配位基之金屬化合物。
金屬原子為鈦、鋯或鉿之氮化金屬系薄膜係用作使切削工具等之硬度及強度提昇的塗層、半導體元件之閘極膜、阻擋膜,目前已有許多關於藉由化學氣相成長法來製造該等薄膜之技術的報告。
例如,專利文獻1中揭示有使用鈦、鋯、鉿、釩、鈮或鉭之鹵化物的氮化金屬及/或碳化金屬薄膜之製造方法,專利文獻2中揭示有採用使用四氯化鈦及氨氣之CVD法的氮化鈦薄膜之製造方法。
專利文獻2~5中揭示有使用以有機胺作為配位基之二烷基胺基金屬化合物作為鈦、鋯或鉿之前驅物的含第4族金屬之薄膜之製造方法,並且揭示有使用乙基甲基胺作為有機胺配位基之金屬化合物。
但是,使用以四氯化鈦為代表之氯化物的方法,於形成薄膜時需要至少500℃左右之溫度,不適合用於製造閘極膜等半導體元件。又,以有機胺作為配位基之有機醯胺系金屬化合物,雖可於低溫下製造氮化金屬薄膜,但使用其而獲得之薄膜之殘留碳成分較多,故而難以實現所期待之電氣特性,尤其是難以應用於要求導電性之閘極膜、阻擋膜、電極膜。
專利文獻6中揭示有採用使用Ti(N(CH3
)2
)3
X、Ti(N(CH3
)2
)2
X2
、Ti(N(C2
H5
)2
)3
X、Ti(N(C2
H5
)2
)2
X2
(X為鹵素原子)之CVD法的氮化鈦薄膜之製造方法。關於該等鈦化合物,揭示有其熱分解性較高,可較好地用作閘極薄膜材料。但是,於專利文獻6中代表性地使用的Ti(N(CH3
)2
)3
Cl、Ti(N(CH3
)2
)2
Cl2
係固體,於用作CVD材料時,需要保持在熔點以上之溫度下。該等雖然熱分解性良好,但另一方面熱穩定性差,若為了長時間保持液體狀態而進行加熱,則有發生分解之虞。又,若直接使用固體,則會在揮發量不足、經時變化等原料氣體供給性或原料在生產線上之輸送方面存在問題,亦存在微粒汚染之問題。又,於利用使用將固體前驅物溶解於有機溶劑中而成之溶液的溶液CVD法等之溶液的製程中,氣化裝置中之溫度變化或溶劑之部分揮發、濃度變化會引起固體析出,而無法完全解決配管堵塞等所引起的供給量之經時變化、或微粒汚染之問題。
專利文獻1:日本專利特開2003-64475號公報
專利文獻2:日本專利特開平7-201779號公報
專利文獻3:韓國專利156980號公報
專利文獻4:日本專利特開2006-45083號公報
專利文獻5:日本專利特開2006-182709號公報
專利文獻6:日本專利特開2000-36473號公報
本發明所欲解決之課題在於提供一種金屬化合物,其可提供殘留碳較少之良好的含金屬之薄膜,且可提供於成膜速度或薄膜成分控制方面穩定的製程。再者,本發明之所謂化學氣相成長用原料,只要未特別予以區分,則表示CVD用原料或者ALD用原料之兩者。
本發明者等經過反覆研究,結果發現具有特定結構之金屬化合物可解決上述課題,從而完成了本發明。
本發明係提供下述通式(1)所表示之金屬化合物:
[化1]
(式中,M表示鈦、鋯或鉿,X表示鹵素原子;m表示1或2)。
又,本發明係提供含有上述金屬化合物之化學氣相成長用原料。
又,本發明係提供採用使用上述化學氣相成長用原料之化學氣相成長法的含金屬之薄膜之製造方法。
以下,基於較好的實施形態對本發明進行詳細說明。
本發明之金屬化合物係上述通式(1)所表示之新穎化合物。
上述通式(1)中,作為X所表示之鹵素原子,可列舉氟、氯、溴、碘。該等鹵素原子中,氯由於原料價格低廉且揮發性較高,故而較好。
又,m為1之金屬化合物之揮發性大於m為2之金屬化合物,m為2之金屬化合物之熱分解溫度低於m為1之金屬化合物。於用作化學氣相成長用原料時,由於揮發溫度(蒸氣溫度)與薄膜沈積溫度(反應溫度)之差值較大者可取得較廣之製程範圍,故而容易使用。因此,對於m,選擇製程範圍較大者即可。例如,M為鈦原子時,m為1之金屬化合物可取得較大之製程範圍,故而較好。
X為氯且M為鈦時,類似化合物即Cln
Ti(N(CH3
)2
)4-n
(n為1或2)係熔點在70~95℃之範圍內的固體,由於本發明之金屬化合物為液體,故而尤其適合用作化學氣相成長用原料。
作為本發明之金屬化合物的具體例,可列舉下述化合物No. 1~24:
[化2]
[化3]
[化4]
本發明之金屬化合物並不根據其製造方法而受到特別之制限,可應用眾所周知之反應來製造。作為其製造方法,例如可列舉:使MX4
(M、X與上述通式(1)相同)與達到所期望之m所需要之量的乙基甲基胺進行反應的方法;使MX4
與達到所期望之m所需要之量的M(NEtMe)4
進行反應的方法。於前一方法之情形時,較好的是使用烷基鋰作為反應劑,經由作為反應性中間物之乙基甲基胺基鋰,使其與MX4
進行反應的方法。於後一方法之情形時,較好的是將MX4
與M(NEtMe)4
混合,並於反應所需要之溫度下進行攪拌的方法。又,本發明之金屬化合物之製造,係於儘可能地將水分、氧、二氧化碳等反應活性種自體系中除去的環境下進行。
本發明之所謂化學氣相成長用原料,係以上述通式(1)所表示之金屬化合物作為薄膜之前驅物者,其形態可根據所使用之化學氣相成長法的輸送供給方法等方法進行適當選擇。
作為上述輸送供給方法,有如下方法:藉由將化學氣相成長用原料於原料容器中進行加熱及/或減壓而使其氣化,再與視需要而使用之氬氣、氮氣、氦氣等載體氣體一併導入至沈積反應部的氣體輸送法;藉由以液體或溶液狀態將化學氣相成長用原料輸送至氣化室內,並於氣化室內進行加熱及/或減壓而使其氣化,再導入至沈積反應部的液體輸送法。於採用氣體輸送法之情形時,係以上述通式(1)所表示之金屬化合物本身作為化學氣相成長用原料;於採用液體輸送法之情形時,係以上述通式(1)所表示之金屬化合物本身或將該金屬化合物溶解於有機溶劑而成之溶液作為化學氣相成長用原料。
又,關於製造多成分系薄膜時所採用之多成分系化學氣相成長法,有如下方法:使化學氣相成長用原料之各成分獨立氣化,並進行供給的方法(以下有時稱為單源(single source)法);及使預先以所期望之成分將多成分原料混合而成之混合原料氣化,並進行供給的方法(以下有時稱為混合源(cocktail source)法)。於採用混合源法之情形時,化學氣相成長用原料為:僅包含上述通式(1)所表示之金屬化合物的混合物或者於該等混合物中添加有機溶劑而成的混合溶液、上述通式(1)所表示之金屬化合物與其他前驅物之混合物或者於該等混合物中添加有機溶劑而成的混合溶液。
作為上述化學氣相成長用原料所使用之有機溶劑,並無特別限制,可使用不與本發明之金屬化合物發生反應的眾所周知之一般有機溶劑。作為該有機溶劑,例如可列舉:乙酸乙酯、乙酸丁酯、乙酸甲氧基乙酯等乙酸酯類;四氫呋喃、四氫吡喃、嗎啉、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、丁醚、二烷等醚類;甲基丁基酮、甲基異丁基酮、乙基丁基酮、丙酮、異丁酮、甲基戊基酮、環己酮、甲基環己酮等酮類;己烷、環己烷、甲基環己烷、二甲基環己烷、乙基環己烷、庚烷、辛烷、甲苯、二甲苯等烴類;乙腈、1-氰基丙烷、1-氰基丁烷、1-氰基己烷、氰基環己烷、氰基苯、1,3-二氰基丙烷、1,4-二氰基丁烷、1,6-二氰基己烷、1,4-二氰基環己烷、1,4-二氰基苯等具有氰基之烴類;吡吡、二甲基吡啶,該等可根據溶質之溶解性、使用溫度與沸點及引火點之關係等而單獨使用,或製成二種類以上之混合溶媒來使用。於使用該等有機溶劑之情形時,較好的是使該有機溶劑中之本發明之金屬化合物成分的總量達到0.01~2.0莫耳/升,尤其好的是達到0.05~1.0莫耳/升。
又,於使用單源法或混合源法之多成分系化學氣相成長法中,作為可與本發明之上述通式(1)所表示之金屬化合物一併使用的其他前驅物,並無特別限制,可使用眾所周知之一般前驅物。
作為上述其他前驅物,可列舉:選自由可用作醇化合物、二醇化合物、β-二酮化合物、環戊二烯化合物及有機胺化合物等之有機配位基的化合物所組成群中的一種或二種以上,與矽、硼、磷或金屬之化合物。作為金屬種,可列舉:鋰、鈉、鉀、銣、銫等第1族元素,鈹、鎂、鈣、鍶、鋇等第2族元素,鈧、釔、鑭系元素(鑭、鈰、鐠、釹、鉕、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿、鑥)、錒系元素等第3族元素,鈦、鋯、鉿等第4族元素,釩、鈮、鉭之第5族元素,鉻、鉬、鎢之第6族元素,錳、鎝、錸之第7族元素,鉄、釕、鋨之第8族元素,鈷、銠、銥之第9族元素,鎳、鈀、鉑之第10族元素,銅、銀、金之第11族元素,鋅、鎘、汞之第12族元素,鋁、鎵、銦、鉈之第13族元素,鍺、錫、鉛之第14族元素,砷、銻、鉍之第15族元素,釙之第16族元素。
作為可用作有機配位基之上述醇化合物,可列舉:甲醇、乙醇、丙醇、異丙醇、丁醇、2-丁醇、異丁醇、第三丁醇、戊醇、異戊醇、第三戊醇等烷醇類;2-甲氧基乙醇、2-乙氧基乙醇、2-丁氧基乙醇、2-(2-甲氧基乙氧基)乙醇、2-甲氧基-1-甲基乙醇、2-甲氧基-1,1-二甲基乙醇、2-乙氧基-1,1-二甲基乙醇、2-異丙氧基-1,1-二甲基乙醇、2-丁氧基-1,1-二甲基乙醇、2-(2-甲氧基乙氧基)-1,1-二甲基乙醇、2-丙氧基-1,1-二乙基乙醇、2-第二丁氧基-1,1-二乙基乙醇、3-甲氧基-1,1-二甲基丙醇等醚醇類;二烷基胺基醇等。
作為可用作有機配位基之上述二醇化合物,可列舉:1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、2,4-己二醇、2,2-二甲基-1,3-丙二醇、2,2-二乙基-1,3-丙二醇、1,3-丁二醇、2,4-丁二醇、2,2-二乙基-1,3-丁二醇、2-乙基-2-丁基-1,3-丙二醇、2,4-戊二醇、2-甲基-1,3-丙二醇、2-甲基-2,4-戊二醇、2,4-己二醇、2,4-二甲基-2,4-戊二醇等。
作為可用作有機配位基之上述β-二酮化合物,可列舉:乙醯丙酮、己烷-2,4-二酮、5-甲基己烷-2,4-二酮、庚烷-2,4-二酮、2-甲基庚烷-3,5-二酮、5-甲基庚烷-2,4-二酮、6-甲基庚烷-2,4-二酮、2,2-二甲基庚烷-3,5-二酮、2,6-二甲基庚烷-3,5-二酮、2,2,6-三甲基庚烷-3,5-二酮、2,2,6,6-四甲基庚烷-3,5-二酮、辛烷-2,4-二酮、2,2,6-三甲基辛烷-3,5-二酮、2,6-二甲基辛烷-3,5-二酮、2,9-二甲基壬烷-4,6-二酮2-甲基-6-乙基癸烷-3,5-二酮、2,2-二甲基-6-乙基癸烷-3,5-二酮等經烷基取代之β-二酮類;1,1,1-三氟戊烷-2,4-二酮、1,1,1-三氟-5,5-二甲基己烷-2,4-二酮、1,1,1,5,5,5-六氟戊烷-2,4-二酮、1,3-二全氟己基丙烷-1,3-二酮等經氟取代之烷基β-二酮類;1,1,5,5-四甲基-1-甲氧基己烷-2,4-二酮、2,2,6,6-四甲基-1-甲氧基庚烷-3,5-二酮、2,2,6,6-四甲基-1-(2-甲氧基乙氧基)庚烷-3,5-二酮等經醚基取代之β-二酮類等。
作為可用作有機配位基之上述環戊二烯化合物,可列舉:環戊二烯、甲基環戊二烯、乙基環戊二烯、丙基環戊二烯、異丙基環戊二烯、丁基環戊二烯、第二丁基環戊二烯、異丁基環戊二烯、第三丁基環戊二烯、二甲基環戊二烯、四甲基環戊二烯、五甲基環戊二烯等。
作為可用作有機配位基之上述有機胺化合物,可列舉:甲胺、乙胺、丙胺、異丙胺、丁胺、第三丁胺、第二丁基胺、異丁基胺、二甲基胺、二乙基胺、二丙基胺、二異丙基胺、乙基甲基胺、丙基甲基胺、異丙基甲基胺等。
作為多成分系化學氣相成長法中之上述其他前驅物,於採用單源法之情形時,較好的是與本發明之金屬化合物變化為薄膜成分時之反應或分解舉動類似的化合物。又,於採用ALD法之情形時,較好的是與所形成之分子級的層(本發明之金屬化合物層或其經過反應而成之中間物層)具有反應活性之化合物。於採用混合源法之情形時,較好的是變化為薄膜成分之舉動類似,並且混合時不會發生由化學反應所引起之變質的化合物。
又,本發明之化學氣相成長用原料中,可視需要而含有親核性試劑,以使本發明之金屬化合物及其他前驅物具有穩定性。作為該親核試劑,可列舉:乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、四乙二醇二甲醚等乙二醇醚類,18-冠醚-6、二環己基-18-冠醚-6、24-冠醚-8、二環己基-24-冠醚-8、二苯并-24-冠醚-8等冠醚類,乙二胺、N,N'-四甲基乙二胺、二乙三胺、三乙四胺、四乙五胺、五乙六胺、1,1,4,7,7-五甲基二乙三胺、1,1,4,7,10,10-六甲基三乙四胺、三乙氧基三乙四胺等多胺類,1,4,8,11-四氮雜環十四烷(Cyclam)、1,4,7,10-四氮雜環十二烷(cyclen)等環狀多胺類,吡啶、吡咯啶、哌啶、嗎啉、N-甲基吡咯啶、N-甲基哌啶、N-甲基嗎啉、四氫呋喃、四氫吡喃、1,4-二烷、唑、噻唑、氧硫雜環戊烷等雜環化合物類,作為穩定劑之該等親核性試劑的使用量,相對於本發明之金屬化合物1莫耳,較好的是在0.05莫耳~10莫耳之範圍內使用,更好的是在0.1~5莫耳之範圍內使用。
關於本發明之化學氣相成長用原料,係儘力使其不含有除構成成分以外之雜質金屬元素成分、氯成分等雜質鹵素、及雜質有機成分。雜質金屬元素成分較好的是每種元素為100ppb以下,更好的是10ppb以下。總量較好的是1ppm以下,更好的是100ppb以下。尤其是將金屬氧化物、與矽之複合金屬氧化物、氮化物、與矽之氮氧化物等用於LSI之閘極絕緣膜、閘極膜、阻擋層之情形時,需要降低會對所獲得之薄膜的電氣特性產生影響之鹼金屬元素、鹼土類金屬元素及同族元素(鈦、鋯或鉿)的含量。雜質鹵素成分較好的是100ppm以下,更好的是10ppm以下,更好的是1ppm以下。雜質有機成分,以總量計,較好的是500ppm以下,更好的是50ppm以下,更好的是10ppm以下。又,由於水分係導致CVD原料中產生微粒或藉由化學氣相成長法時產生微粒之原因,故而為了減少金屬化合物、有機溶劑及親核性試劑之水分,較好的是於使用時預先儘可能地除去水分。金屬化合物、有機溶劑及親核性試劑之各自水分量較好的是10ppm以下,更好的是1ppm以下。
又,對於本發明之化學氣相成長用原料,為了降低或防止所製造之薄膜的微粒汚染,於液相中利用光散射式液體中粒子檢測器進行微粒測定時,較好的是大於0.3μm之粒子數在1ml液相中為100個以下,更好的是大於0.2μm之粒子數在1ml液相中為1000個以下,更好的是大於0.2μm之粒子數在1ml液相中為100個以下。
本發明之所謂薄膜之製造方法,係基於化學氣相成長用法之製造方法,該化學氣相成長用法係將本發明之金屬化合物、及使視需要而使用之其他前驅物氣化而成之蒸氣、以及視需要而使用之反應性氣體導入至基板上,繼而使前驅物於基板上進行分解及/或反應,而使薄膜於基板上成長、沈積的方法。關於原料之輸送供給方法、沈積方法、製造條件、製造裝置等,並無特別限制,可採用眾所周知之一般條件、方法。
作為上述視需要而使用之反應性氣體,例如:作為製造氧化物者,可列舉作為氧化性氣體之氧氣、臭氧、二氧化氮、一氧化氮、水蒸氣、過氧化氫、甲酸、乙酸、乙酸酐等;作為還原性者,可列舉氫氣;又,作為製造氮化物者,可列舉單烷基胺、二烷基胺、三烷基胺、烷二胺等有機胺化合物,肼、氨氣、氮氣等。
又,作為上述輸送供給方法,可列舉:上述氣體輸送法、液體輸送法、單源法、混合源法等。
又,作為上述沈積方法,可列舉:僅利用熱使原料氣體、或原料氣體及反應性氣體反應而沈積薄膜的熱CVD;使用熱及電漿之電漿CVD;使用熱及光之光CVD;使用熱、光及電漿之光電漿CVD;將CVD之沈積反應劃分為基元步驟,並以分子級階段性地進行沈積之ALD(Atomic Layer Deposition,原子層沈積法)。
又,作為上述製造條件,可列舉:反應溫度(基板溫度)、反應壓力、沈積速度等。關於反應溫度,較好的是本發明之金屬化合物可充分反應之溫度即150℃以上,更好的是250℃~450℃。又,關於反應壓力,於採用熱CVD或光CVD之情形時,較好的是大氣壓~10Pa,於使用電漿之情形時,較好的是10Pa~2000Pa。又,沈積速度可藉由原料之供給條件(氣化溫度、氣化壓力)、反應溫度、反應壓力來進行控制。由於沈積速度過大所獲得之薄膜的特性會變差,過小會在生產性方面產生問題,故而沈積速度較好的是0.5~5000nm/min,更好的是1~1000nm/min。又,於採用ALD之情形時,可控制循環次數,以獲得所期望之膜厚。再者,利用本發明之化學氣相成長用原料所形成之薄膜的厚度,可根據用途來適當選擇,較好的是自0.1~1000nm之範圍內進行選擇。
由於本發明之金屬化合物可提供殘留碳等雜質之含量較小的金屬氮化物,故而可較好地用於製造氮化金屬系薄膜。又,使用本發明之化學氣相成長用原料來製造氮化金屬系薄膜之較好的方法為ALD。ALD係交替向沈積部供給原料與視需要而使用之反應性氣體、視需要而使用之其他前驅物,以此作為1個循環,從而階段性地使所期望之薄膜之分子層沈積的方法。又,於各循環中,亦可任意導入如下步驟:於供給原料氣體及/或反應性氣體後,利用惰性氣體進行沖洗及/或藉由減壓進行排氣,來除去未反應之原料氣體及/或反應性氣體的步驟。ALD與其他CVD法相比,具有可獲得厚度較薄且均勻之良好薄膜的特徵。又,由其成膜機構可將薄膜沈積溫度控制在較低之溫度,可不受基體之耐熱性、元素於基體上之擴散性等的影響而進行廣泛應用。又,ALD亦可與熱、光、電漿併用。
又,於本發明之薄膜之製造方法中,薄膜沈積後為了獲得良好之電氣特性,可於惰性氣體環境下、氧化性氣體環境下或還原性氣體環境下進行退火處理,於需要階梯覆蓋之情形時,亦可設置回焊步驟。退火、回焊之溫度在用途上係於容許之溫度內。通常為300~1200℃,較好的是400~600℃。
藉由使用本發明之化學氣相成長法用原料的本發明之薄膜之製造方法所製造的薄膜,藉由適當選擇其他成分之前驅物、反應性氣體及製造條件,可製成金屬氧化物系薄膜、金屬氮化物系薄膜、玻璃等所期望之種類的薄膜。作為所製造之薄膜的成分,例如:作為金屬氧化物系薄膜,可列舉氧化鈦、氧化鋯、氧化鉿、鉍-鈦複合氧化物、鉍-稀土類元素-鈦複合氧化物、矽-鈦複合氧化物、矽-鋯複合氧化物、矽-鉿複合氧化物、鉿-鋁複合氧化物、鉿-稀土類元素複合氧化物、矽-鉍-鈦複合氧化物、矽-鉿-鋁複合氧化物、矽-鉿-稀土類元素複合氧化物、鈦-鋯-鉛複合氧化物、鈦-鉛複合氧化物、鍶-鈦複合氧化物、鋇-鈦複合氧化物、鋇-鍶-鈦複合氧化物等;作為金屬氮化物系薄膜,可列舉氮化鈦、氮化鋯、氮化鉿、鈦-鋁複合氮化膜、矽-鉿複合氧化氮化物(HfSiON)、鈦複合氧化氮化物。作為該等薄膜之用途,可列舉:高介電膜電容器、閘極絕緣膜、閘極膜、電極膜、阻擋膜、強介電膜電容器、電容膜等電子零件部件,光纖、光學波導、光放大器、光開關等光學玻璃部件。
以下,根據實施例、評價例及比較例對本發明進行更詳細地說明。然而,本發明並不受以下實施例等之任何制限。
在乾燥氬氣環境下,向反應燒瓶中裝入43.0g之四氯化鈦(TiCl4
)、500ml之脫水己烷,冷卻至-10℃。以反應體系不超過-5℃之方式,向其中滴加191g之四(乙基甲基胺基)鈦(Ti[N(CH3
)(C2
H5
)]4
)與500ml之脫水己烷之混合溶液。滴加完畢後,於室溫下攪拌8小時後,於減壓下將己烷蒸餾除去。對殘渣進行減壓蒸餾,自壓力100Pa、餾出溫度82℃之餾份中,以90%之產率獲得目標化合物No. 2。所獲得之化合物No. 2之鑑定係藉由元素分析及1
H-NMR來進行。其結果如下所示。
(1)元素分析(金屬分析:原子吸光,氯分析:硝酸銀滴定法)
Ti:18.5質量%(理論值18.59質量%)
氯:13.4質量%(理論值13.76質量%)
(2)1
H-NMR(溶媒:氘代苯)(化學位移:多重度:H數比)
(3.096:s:3)(3.429:q:2)(1.003:t:3)
在乾燥氬氣環境下,向反應燒瓶中裝入55.7g之四氯化鈦(TiCl4
)、300ml之脫水甲苯,冷卻至-10℃。以反應體系不超過-5℃之方式,向其中滴加82.3g之四(乙基甲基胺基)鈦(Ti[N(CH3
)(C2
H5
)]4
)與300ml之脫水甲苯之混合溶液。滴加完畢後,於室溫下攪拌8小時後,於減壓下將甲苯蒸餾除去。對殘渣進行減壓蒸餾,自壓力100Pa、餾出溫度85℃之餾份中,以90%之產率獲得目標化合物No. 6。所獲得之化合物No. 6之鑑定係藉由元素分析及1
H-NMR來進行。其結果如下所示。
(1)元素分析(金屬分析:原子吸光,氯分析:硝酸銀滴定法)
Ti:20.3質量%(理論值20.38質量%)
氯:30.1質量%(理論值30.17質量%)
(2)1
H-NMR(溶媒:氘代苯)(化學位移:多重度:H數比)
(3.021:s:3)(3.470:q:2)(1.003:t:3)
針對上述實施例1及2所獲得之化合物No. 2、6,表1、2所示之比較化合物,進行於20℃下之狀態(若為固體則為熔點:藉由DTA測定而測得的熔點之吸熱開始溫度)及熱分解性的評價。將該等之結果示於表1或表2。熱分解性,係確認到將化合物密閉於不鏽鋼容器中並加熱1小時後於減壓下(10torr)進行TG-DTA測定而獲得的結果超過0.5質量%的分解物時之加熱溫度。關於加熱溫度,TiCl4
以外係於80℃~200℃之範圍內,以10℃為間隔進行選擇,而TiCl4
係於250。C~300℃之範圍內進行選擇。例如,於130℃下加熱1小時後於減壓下進行TG-DTA測定而獲得的結果為幾乎全部揮發,而於140℃下加熱1小時後於減壓下進行TG-DTA測定而獲得的結果為並未全部揮發,且質量減少完畢時產生超過0.5質量%之殘渣時,則將熱分解性評價為140℃。
由上述評價例可知,由於本發明之金屬化合物即化合物No. 2與類似化合物即TiCl[N(CH3
)2
]3
不同,於室溫下為液體,故而適用於化學氣相成長用原料。又,本發明之金屬化合物的熱分解性亦優於TiCl4
、Ti[N(CH3
)(C2
H5
)]4
。此情況提示:可於更低之溫度下製造薄膜,並且以本發明之金屬化合物作為前驅物而獲得之薄膜的膜質良好。尤其是由於薄膜中之殘留碳對電氣特性之影響較小,故而適用於以氮化鈦為代表之LSI之閘極膜、阻擋膜、電極膜的用途。
由上述評價例可知,由於本發明之金屬化合物即化合物No. 6與類似化合物即TiCl2
[N(CH3
)2
]2
不同,於室溫下為液體,故而適用於化學氣相成長用原料。又,熱分解性相同。若對化合物No. 2與化合物No. 6進行比較,則可確認化合物No. 6會於低溫下發生分解,於分解溫度為100℃時,與揮發溫度之製程範圍較小。考慮到氣化步驟之溫度及成膜溫度的範圍,化合物No. 6比化合物No. 2更加適合用於化學氣相成長法。
以上述實施例1所獲得之金屬化合物No. 2作為化學氣相成長用原料,使用圖1所示之裝置,藉由以下條件之ALD法,於矽晶圓上製造氮化鈦膜。針對所獲得之薄膜,藉由螢光X射線測定膜厚,並確認薄膜成分,結果膜厚為60nm,膜成分為氮化鈦,碳含量為1.3atom%。
反應溫度(基板溫度):300℃,反應性氣體:NH3
以包括下述(1)~(4)之一系列步驟作為1個循環,重複進行300個循環。
(1)於氣化室溫度為120℃、氣化室壓力為250Pa之條件下導入被氣化之CVD原料之蒸氣,於250Pa之系統壓力下使之沈積3秒鐘。
(2)藉由3秒鐘之氬氣沖洗來除去未反應原料。
(3)導入反應性氣體,於250Pa之系統壓力下使之反應3秒鐘。
(4)藉由2秒鐘之氬氣沖洗來除去未反應原料。
以Ti[N(CH3
)(C2
H5
)]4
作為化學氣相成長用原料,藉由與上述實施例2相同條件之ALD法,於矽晶圓上製造氮化鈦膜。針對所獲得之薄膜,藉由螢光X射線測定膜厚,並確認薄膜成分,結果膜厚為50nm,膜成分為氮化鈦,碳含量為7.0atom%。
根據本發明,可提供一種具有適合含金屬之薄膜、尤其是氮化金屬系薄膜之製造所使用之化學氣相成長用原料之物性的金屬化合物。
圖1係表示用於本發明之薄膜之製造方法的CVD裝置之一例的概略圖。
(無元件符號說明)
Claims (8)
- 一種金屬化合物,其以下述通式(1)表示:[化1]
- 如請求項1之金屬化合物,其中於上述通式(1)中,M為鈦原子。
- 如請求項1之金屬化合物,其中於上述通式(1)中,X為氯原子。
- 如請求項1之金屬化合物,其中於上述通式(1)中,m為1。
- 一種化學氣相成長用原料,其係含有如請求項1之金屬化合物。
- 如請求項5之化學氣相成長用原料,其係於基體上藉由化學氣相成長法形成氮化金屬系薄膜之原料者。
- 一種含金屬之薄膜之製造方法,其採用使用如請求項5之化學氣相成長用原料之化學氣相成長法。
- 一種氮化金屬系薄膜之製造方法,其採用使用如請求項6之化學氣相成長用原料之化學氣相成長法。
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