TW201329092A - 鋁化合物、薄膜形成用原料及薄膜之製造方法 - Google Patents
鋁化合物、薄膜形成用原料及薄膜之製造方法 Download PDFInfo
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- TW201329092A TW201329092A TW101138137A TW101138137A TW201329092A TW 201329092 A TW201329092 A TW 201329092A TW 101138137 A TW101138137 A TW 101138137A TW 101138137 A TW101138137 A TW 101138137A TW 201329092 A TW201329092 A TW 201329092A
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- Prior art keywords
- film
- aluminum
- raw material
- aluminum compound
- compound
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- -1 Aluminum compound Chemical class 0.000 title claims abstract description 99
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 83
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title abstract description 19
- 239000007858 starting material Substances 0.000 title abstract 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 230000008016 vaporization Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 74
- 239000000758 substrate Substances 0.000 claims description 17
- 239000010408 film Substances 0.000 abstract description 124
- 238000000034 method Methods 0.000 abstract description 50
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 45
- 239000002243 precursor Substances 0.000 abstract description 45
- 230000015572 biosynthetic process Effects 0.000 abstract description 17
- 230000000704 physical effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 42
- 150000001875 compounds Chemical class 0.000 description 32
- 229910052719 titanium Inorganic materials 0.000 description 29
- 239000010936 titanium Substances 0.000 description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 28
- 238000000151 deposition Methods 0.000 description 18
- 125000000217 alkyl group Chemical group 0.000 description 15
- 230000008021 deposition Effects 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 238000000231 atomic layer deposition Methods 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- 229910052787 antimony Inorganic materials 0.000 description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 10
- 125000004432 carbon atom Chemical group C* 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 238000002309 gasification Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 229910052797 bismuth Inorganic materials 0.000 description 8
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 8
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000012434 nucleophilic reagent Substances 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 229910052762 osmium Inorganic materials 0.000 description 7
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 7
- 230000001590 oxidative effect Effects 0.000 description 7
- YRAJNWYBUCUFBD-UHFFFAOYSA-N 2,2,6,6-tetramethylheptane-3,5-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(C)(C)C YRAJNWYBUCUFBD-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 6
- 229910052741 iridium Inorganic materials 0.000 description 6
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000013110 organic ligand Substances 0.000 description 6
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 239000010419 fine particle Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 229910052735 hafnium Inorganic materials 0.000 description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 4
- 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 4
- TXGJTWACJNYNOJ-UHFFFAOYSA-N hexane-2,4-diol Chemical compound CCC(O)CC(C)O TXGJTWACJNYNOJ-UHFFFAOYSA-N 0.000 description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 150000002736 metal compounds Chemical class 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- CEGGECULKVTYMM-UHFFFAOYSA-N 2,6-dimethylheptane-3,5-dione Chemical compound CC(C)C(=O)CC(=O)C(C)C CEGGECULKVTYMM-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000005481 NMR spectroscopy Methods 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
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229940125782 compound 2 Drugs 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 150000002009 diols Chemical class 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 125000005843 halogen group Chemical group 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 3
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 2
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- 229940035437 1,3-propanediol Drugs 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
- AKPLTHZVVWBOPT-UHFFFAOYSA-N 2,2-diethylbutane-1,3-diol Chemical compound CCC(CC)(CO)C(C)O AKPLTHZVVWBOPT-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
- DSKYSDCYIODJPC-UHFFFAOYSA-N 2-butyl-2-ethylpropane-1,3-diol Chemical compound CCCCC(CC)(CO)CO DSKYSDCYIODJPC-UHFFFAOYSA-N 0.000 description 2
- XLLIQLLCWZCATF-UHFFFAOYSA-N 2-methoxyethyl acetate Chemical compound COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 2
- 125000003229 2-methylhexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
- GRWPYGBKJYICOO-UHFFFAOYSA-N 2-methylpropan-2-olate;titanium(4+) Chemical compound [Ti+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] GRWPYGBKJYICOO-UHFFFAOYSA-N 0.000 description 2
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
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- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 2
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- 239000006227 byproduct Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
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- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- ILPNRWUGFSPGAA-UHFFFAOYSA-N heptane-2,4-dione Chemical compound CCCC(=O)CC(C)=O ILPNRWUGFSPGAA-UHFFFAOYSA-N 0.000 description 2
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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 2
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- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
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- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 2
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- 229920000768 polyamine Polymers 0.000 description 2
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 2
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 2
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- 150000002910 rare earth metals Chemical group 0.000 description 2
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- BHXFKXOIODIUJO-UHFFFAOYSA-N benzene-1,4-dicarbonitrile Chemical compound N#CC1=CC=C(C#N)C=C1 BHXFKXOIODIUJO-UHFFFAOYSA-N 0.000 description 1
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- FZDXUOSYZYROKU-UHFFFAOYSA-N butoxy(dimethyl)alumane Chemical compound C[Al+]C.CCCC[O-] FZDXUOSYZYROKU-UHFFFAOYSA-N 0.000 description 1
- ZAGHKONXGGSVDV-UHFFFAOYSA-N butylcyclopentane Chemical compound CCCCC1CCCC1 ZAGHKONXGGSVDV-UHFFFAOYSA-N 0.000 description 1
- KVNRLNFWIYMESJ-UHFFFAOYSA-N butyronitrile Chemical compound CCCC#N KVNRLNFWIYMESJ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
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- 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 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
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- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000011109 contamination Methods 0.000 description 1
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- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 150000003983 crown ethers Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- MGWYSXZGBRHJNE-UHFFFAOYSA-N cyclohexane-1,4-dicarbonitrile Chemical compound N#CC1CCC(C#N)CC1 MGWYSXZGBRHJNE-UHFFFAOYSA-N 0.000 description 1
- VBWIZSYFQSOUFQ-UHFFFAOYSA-N cyclohexanecarbonitrile Chemical compound N#CC1CCCCC1 VBWIZSYFQSOUFQ-UHFFFAOYSA-N 0.000 description 1
- 229960002887 deanol Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 125000005265 dialkylamine group Chemical group 0.000 description 1
- UNTITLLXXOKDTB-UHFFFAOYSA-N dibenzo-24-crown-8 Chemical compound O1CCOCCOCCOC2=CC=CC=C2OCCOCCOCCOC2=CC=CC=C21 UNTITLLXXOKDTB-UHFFFAOYSA-N 0.000 description 1
- BBGKDYHZQOSNMU-UHFFFAOYSA-N dicyclohexano-18-crown-6 Chemical compound O1CCOCCOC2CCCCC2OCCOCCOC2CCCCC21 BBGKDYHZQOSNMU-UHFFFAOYSA-N 0.000 description 1
- QMLGNDFKJAFKGZ-UHFFFAOYSA-N dicyclohexano-24-crown-8 Chemical compound O1CCOCCOCCOC2CCCCC2OCCOCCOCCOC2CCCCC21 QMLGNDFKJAFKGZ-UHFFFAOYSA-N 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 229940043279 diisopropylamine Drugs 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- CRGGFGFWZPSXPP-UHFFFAOYSA-N dimethylazanide;titanium(3+) Chemical compound [Ti+3].C[N-]C.C[N-]C.C[N-]C CRGGFGFWZPSXPP-UHFFFAOYSA-N 0.000 description 1
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- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 description 1
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- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 239000010931 gold Substances 0.000 description 1
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 1
- NGAZZOYFWWSOGK-UHFFFAOYSA-N heptan-3-one Chemical compound CCCCC(=O)CC NGAZZOYFWWSOGK-UHFFFAOYSA-N 0.000 description 1
- SDAXRHHPNYTELL-UHFFFAOYSA-N heptanenitrile Chemical compound CCCCCCC#N SDAXRHHPNYTELL-UHFFFAOYSA-N 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- NFWSQSCIDYBUOU-UHFFFAOYSA-N methylcyclopentadiene Chemical compound CC1=CC=CC1 NFWSQSCIDYBUOU-UHFFFAOYSA-N 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- DWFKOMDBEKIATP-UHFFFAOYSA-N n'-[2-[2-(dimethylamino)ethyl-methylamino]ethyl]-n,n,n'-trimethylethane-1,2-diamine Chemical compound CN(C)CCN(C)CCN(C)CCN(C)C DWFKOMDBEKIATP-UHFFFAOYSA-N 0.000 description 1
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 1
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 description 1
- XHFGWHUWQXTGAT-UHFFFAOYSA-N n-methylpropan-2-amine Chemical compound CNC(C)C XHFGWHUWQXTGAT-UHFFFAOYSA-N 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-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
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 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
- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 description 1
- 125000004115 pentoxy group Chemical group [*]OC([H])([H])C([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 125000005005 perfluorohexyl group Chemical group FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)* 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007789 sealing Methods 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
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000004544 sputter deposition 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
- 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
- 238000000427 thin-film deposition Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 150000003613 toluenes Chemical class 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-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
- 238000007740 vapor deposition Methods 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
- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/062—Al linked exclusively to C
-
- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/066—Aluminium compounds with C-aluminium linkage compounds with Al linked to an element other than Al, C, H or halogen (this includes Al-cyanide linkage)
-
- 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
- C23C16/403—Oxides of aluminium, magnesium or beryllium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- 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
- H01L21/02178—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 aluminium, e.g. Al2O3
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- 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
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Formation Of Insulating Films (AREA)
Abstract
本發明係一種下述化學式(I)所表示之鋁化合物、含有該鋁化合物而成之薄膜形成用原料、及薄膜之製造方法,該薄膜之製造方法係將使該薄膜形成用原料氣化而獲得之含有上述鋁化合物之蒸氣導入設置有基體之成膜腔室內,使該鋁化合物分解及/或發生化學反應而於該基體表面形成含有鋁之薄膜。本發明之薄膜形成用原料由於作為前驅物之鋁化合物之物性適於CVD法、ALD法,因此尤其可用作化學氣相沈積用原料。□
Description
本發明係關於一種具有特定之有機配位基之新穎鋁化合物、含有該化合物而成之薄膜形成用原料、及使用該原料形成含有鋁之薄膜的薄膜之製造方法。
含有鋁元素之薄膜材料表現出特殊之電氣特性及光學特性,而應用於各種用途。例如,就高導電性、電遷移耐性之方面而言,鋁及鋁合金薄膜可用作LSI(Large Scale Integration,大型積體電路)之配線材料,氧化鋁系薄膜可用作機械零件或工具等之硬質塗層膜;半導體記憶體之絕緣膜、閘極絕緣膜、介電質膜;硬碟用MR(magnetoresistive,磁電阻)頭等電子零件;光通信用電路等之光學玻璃。
作為上述薄膜之製造方法,可列舉:濺鍍法、離子電鍍法、塗佈熱分解法或溶膠凝膠法等MOD(Metal Organic Deposition,金屬有機沈積)法、化學氣相沈積法等,其中包含ALD(Atomic Layer Deposition,原子層沈積)法之化學氣相沈積(以下,有時亦簡稱為CVD(Chemical Vapor Deposition))法由於具有組成控制性、階梯覆蓋性優異,適於量產化,可混合集成(Hybrid Integration)等大量優點,故而為最佳之製造製程。
作為以廉價之氯化鋁作為氧化鋁系薄膜之氣相沈積法用原料的CVD法,大量報告有切割工具等在硬度及強度得到提高之塗層中之使用,例如,專利文獻1中揭示有藉由使
用二氧化碳、鹽酸或硫化氫作為氧化性氣體之CVD法製造氧化鋁膜之方法。然而,專利文獻1中所記載之使用氯化鋁之製程係使用固體作為原料,於對薄膜沈積部位之原料供給性或微粒產生之方面存在問題,且成膜溫度亦較高,因此並非提供適於半導體元件用途之電氣特性、階梯覆蓋性、膜質等經高度控制的微細薄膜之形成者。專利文獻2中揭示有包含本發明之鋁化合物在內之通式作為觸媒組合物之原料成分,但並無關於本發明之鋁化合物之記載,亦無關於使用該成分作為薄膜形成用原料之記載。專利文獻3中揭示有包含本發明之鋁化合物在內之通式作為薄膜形成用原料,但並無關於本發明之鋁化合物之記載,作為烷氧基矽烷中最佳之薄膜形成用原料,報告有AlMe2(OiPr)。然而,AlMe2(OiPr)之熱穩定性較低,作為化學氣相沈積用原料,並非為可充分滿足之化合物。又,於專利文獻4中,作為藉由化學蒸鍍以氧化鋁塗佈基材之材料,報告有二甲基第三丁醇鋁。然而,二甲基第三丁醇鋁之熔點較高,作為化學氣相沈積用原料,並非為可充分滿足之化合物。
專利文獻1:US2002/0076284A1
專利文獻2:US5747409A
專利文獻3:US2009/0203222A1
專利文獻4:US5922405A
於使化學氣相沈積用原料等氣化而形成薄膜之情形時,適合於該原料之化合物(前驅物)所要求之性質係無自燃性(spontaneous combustibility),熔點較低,可於液體狀態下輸送;蒸氣壓較大容易氣化;及熱穩定性較高。尤其於ALD法中,為實施如下步驟,重要的是前驅物之較高之熱穩定性:於藉由加熱成為氣相之前驅物不會發生熱分解之情況下將其向基體輸送,使其不會發生熱分解地吸附於加熱至高溫之基體,並與其後所導入之反應性氣體反應,藉此形成薄膜。於先前之鋁化合物中,就該等方面而言,並非為可充分滿足之化合物。
本發明者等人進行反覆研究,結果發現使用有特定之配位基之鋁化合物可解決上述課題,從而完成本發明。
本發明係提供一種下述化學式(I)所表示之鋁化合物、含有其而成之薄膜形成用原料、及使用該原料形成含有鋁之薄膜的薄膜之製造方法。
根據本發明,可獲得一種無自燃性,常溫下為液體,表現充分之揮發性且具有較高之熱穩定性的鋁化合物。又,該化合物適合作為利用CVD法之薄膜形成用原料。
本發明之鋁化合物係上述化學式(I)所表示者,適合作為包含CVD法等氣化步驟之薄膜製造方法之前驅物,就熱穩定性較高之方面而言,尤其適合作為用於ALD法之前驅物。再者,化學式(I)中之第二丁基係具有光學活性部位之基,本發明之鋁化合物並非特別藉由R體、S體而加以區別,可為其任一者,亦可為R體與S體之任意比例之混合物。外消旋體之製造成本較為廉價。
本發明之鋁化合物並不特別受該製造方法限制,可應用周知之反應而製造。作為製造方法,例如可藉由使第二丁醇與三甲基鋁反應而獲得。
所謂本發明之薄膜形成用原料,係指將上述說明之本發明之鋁化合物作為薄膜之前驅物者,其形態根據應用該薄膜形成用原料之製造製程之不同而有所不同。例如,於製造僅含鋁作為金屬之薄膜之情形時,本發明之薄膜形成用原料不含上述鋁化合物以外之金屬化合物及半金屬化合物。另一方面,於製造包含鋁、及鋁以外之金屬及/或半金屬的薄膜之情形時,本發明之薄膜形成用原料除了含有上述鋁化合物以外,亦含有包含鋁以外之金屬之化合物及/或包含半金屬之化合物(以下,亦稱為其他前驅物)。本發明之薄膜形成用原料亦可如下所述般進而含有有機溶劑及/
或親核性試劑。
如上所說明般,本發明之薄膜形成用原料由於作為前驅物之鋁化合物之物性適於CVD法、ALD法,因此尤其可用作化學氣相沈積用原料(以下,有時亦稱為CVD用原料)。
於本發明之薄膜形成用原料為化學氣相沈積用原料之情形時,其形態可根據所使用之CVD法之輸送供給方法等方法而適當選擇。
作為上述輸送供給方法,有如下方法:氣體輸送法,其係藉由將CVD用原料於儲存該原料之容器(以下,有時亦簡稱為原料容器)中進行加熱及/或減壓,而使之氣化形成蒸氣,將該蒸氣與視需要所使用之氬氣、氮氣、氦氣等載體氣體一併導入設置有基體之成膜腔室內(以下,有時亦記載為沈積反應部);液體輸送法,其係藉由將CVD用原料於液體或溶液之狀態下輸送至氣化室並於氣化室內進行加熱及/或減壓,而使之氣化形成蒸氣,將該蒸氣導入成膜腔室內。於氣體輸送法之情形時,可以上述化學式(I)所表示之鋁化合物本身作為CVD原料。於液體輸送法之情形時,可以上述化學式(I)所表示之鋁化合物本身或將該化合物溶解於有機溶劑而成之溶液作為CVD用原料。該等CVD原料亦可進而含有其他前驅物或親核性試劑等。
又,於多成分系之CVD法中,有使CVD用原料各成分獨立地氣化而供給之方法(以下,有時亦記載為單源(single source)法),及使預先以所需組成混合多成分原料而成之混合原料氣化而供給之方法(以下,有時亦記載為混合源
法)。於混合源法之情形時,可以本發明之鋁化合物與其他前驅物之混合物、或者將該混合物溶解於有機溶劑而成之混合溶液作為CVD用原料。該混合物或混合溶液亦可進而含有親核性試劑等。
再者,於僅使用本發明之鋁化合物作為前驅物且併用R體與S體之情形時,可使包含R體之CVD用原料與包含S體之CVD用原料分別氣化,或者亦可使包含R體及S體之混合物之CVD用原料氣化。
作為上述有機溶劑,並無特別限制,可使用周知通常之有機溶劑。作為該有機溶劑,例如可列舉:甲醇、乙醇、異丙醇、正丁醇等醇類;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、乙二醇二甲醚、二乙二醇二甲醚、三乙二醇二甲醚、二丁醚、二烷等醚類;甲基丁基酮、甲基異丁基酮、乙基丁基酮、二丙基酮、二異丁基酮、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;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;吡啶、二甲基吡啶等;該等溶劑根據溶質之溶解性、使用溫度與沸點、燃點之關係等,可單獨使用或作為兩種以上之混合溶劑使用。於使用該等有機溶劑之情形時,作為將前驅物溶解於有機溶劑而成之溶液的CVD用原料中之前驅物之總
量較佳為0.01~2.0莫耳/升,尤佳為0.05~1.0莫耳/升。所謂前驅物之總量,於本發明之薄膜形成用原料不含本發明之鋁化合物以外之金屬化合物及半金屬化合物的情形時,係指本發明之鋁化合物之量,於本發明之薄膜形成用原料除了含有該鋁化合物以外,亦含有包含鋁以外之金屬之化合物及/或包含半金屬之化合物之情形時,係指本發明之鋁化合物及其他前驅物之合計量。
又,於多成分系之CVD法之情形時,作為與本發明之鋁化合物一併使用之其他前驅物,並無特別限制,可使用CVD用原料中所使用之周知通常之前驅物。
作為上述其他前驅物,可列舉選自由醇化合物、二醇化合物、β-二酮化合物、環戊二烯化合物、有機胺化合物等用作有機配位基之化合物所組成之群中之一種或兩種以上、與矽或金屬(其中鋁除外)之化合物。又,作為前驅物之金屬種類,可列舉:鎂、鈣、鍶、鋇、鈦、鋯、鉿、釩、鈮、鉭、錳、鐵、釕、鈷、銠、銥、鎳、鈀、鉑、銅、銀、金、鋅、鎵、銦、鍺、錫、鉛、銻、鉍、鈧、釔、鑭、鈰、鐠、釹、鉕、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿、鎦。
作為上述用作有機配位基之醇化合物,可列舉:甲醇、乙醇、丙醇、異丙醇、丁醇、第二丁醇、異丁醇、第三丁醇、戊醇、異戊醇、第三戊醇等烷基醇類;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;二甲基胺基乙醇、乙基甲基胺基乙醇、二乙基胺基乙醇、二甲基胺基-2-戊醇、乙基甲基胺基-2-戊醇、二甲基胺基-2-甲基-2-戊醇、乙基甲基胺基-2-甲基-2-戊醇、二乙基胺基-2-甲基-2-戊醇等二烷基胺基醇類等。
作為上述用作其他前驅物之有機配位基之二醇化合物,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。
又,作為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-3,5-二酮等經醚取代之β-二酮類等。
又,作為環戊二烯化合物,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、四甲基環戊二烯等,作為上述用作有機配位基之有機胺化合物,可列舉:甲基胺、乙基胺、丙基胺、異丙基胺、丁基胺、第二丁基胺、第三丁基胺、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。
上述其他前驅物於該技術領域中為公知者,其製造方法亦為公知。若列舉製造方法之一例,則例如於使用醇化合物作為有機配位基之情形時,可藉由使之前所述之金屬之無機鹽或其水合物與該醇化合物之鹼金屬烷氧化物反應而製造前驅物。此處,作為金屬之無機鹽或其水合物,可列舉:金屬之鹵化物、硝酸鹽等,作為鹼金屬烷氧化物,可列舉:烷醇鈉、烷醇鋰、烷醇鉀等。
上述其他前驅物於單源法之情形時,較佳為本發明之鋁化合物、以及熱及/或氧化分解之行為類似之化合物,於混合源法之情形時,較佳為熱及/或氧化分解之行為類似,並且混合時不會因化學反應發生變質者。
作為上述其他前驅物中包含鈦、鋯或鉿之前驅物,可列舉下述式(II-1)~(II-5)所表示之化合物。
於上述式(II-1)~(II-5)中,作為Ra及Rb所表示之可經鹵素原子取代,亦可於鏈中含有氧原子的碳數1~20之烷基,可列舉:甲基、乙基、丙基、異丙基、丁基、第二丁基、第三丁基、異丁基、戊基、異戊基、第二戊基、第三戊基、己基、環己基、1-甲基環己基、庚基、3-庚基、異庚基、第三庚基、正辛基、異辛基、第三辛基、2-乙基己基、三
氟甲基、全氟己基、2-甲氧基乙基、2-乙氧基乙基、2-丁氧基乙基、2-(2-甲氧基乙氧基)乙基、1-甲氧基-1,1-二甲基甲基、2-甲氧基-1,1-二甲基乙基、2-乙氧基-1,1-二甲基乙基、2-異丙氧基-1,1-二甲基乙基、2-丁氧基-1,1-二甲基乙基、2-(2-甲氧基乙氧基)-1,1-二甲基乙基等。又,作為Rc所表示之碳數1~8之烷基,可列舉:甲基、乙基、丙基、異丙基、丁基、第二丁基、第三丁基、異丁基、戊基、異戊基、第二戊基、第三戊基、己基、1-乙基戊基、環己基、1-甲基環己基、庚基、異庚基、第三庚基、正辛基、異辛基、第三辛基、2-乙基己基等。又,所謂Rd所表示之碳數2~18之可分支之伸烷基,係指由二醇提供之基,作為該二醇,例如可列舉:1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、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、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、1-甲基-2,4-戊二醇等。又,作為Re及Rf所表示之碳數1~3之烷基,可列舉:甲基、乙基、丙基、2-丙基等,作為Rg、Rh、Rj及Rk所表示之碳數1~4之烷基,可列舉:甲基、乙基、丙基、異丙基、丁基、第二丁基、第三丁基、異丁基等。
具體而言,作為含有鈦之前驅物,可列舉:四(乙氧基)鈦、四(2-丙氧基)鈦、四(丁氧基)鈦、四(第二丁氧基)鈦、四(異丁氧基)鈦、四(第三丁氧基)鈦、四(第三戊基)鈦、四(1-甲氧基-2-甲基-2-丙氧基)鈦等四烷氧基鈦類;四(戊
烷-2,4-二酮)鈦、(2,6-二甲基庚烷-3,5-二酮)鈦、四(2,2,6,6-四甲基庚烷-3,5-二酮)鈦等四(β-二酮)鈦類;雙(甲氧基)雙(戊烷-2,4-二酮)鈦、雙(乙氧基)雙(戊烷-2,4-二酮)鈦、雙(第三丁氧基)雙(戊烷-2,4-二酮)鈦、雙(甲氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦、雙(乙氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦、雙(2-丙氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦、雙(第三丁氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦、雙(第三戊氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦、雙(甲氧基)雙(2,2,6,6-四甲基庚烷-3,5-二酮)鈦、雙(乙氧基)雙(2,2,6,6-四甲基庚烷-3,5-二酮)鈦、雙(2-丙氧基)雙(2,6,6,6-四甲基庚烷-3,5-二酮)鈦、雙(第三丁氧基)雙(2,2,6,6-四甲基庚烷-3,5-二酮)鈦、雙(第三戊氧基)雙(2,2,6,6-四甲基庚烷-3,5-二酮)鈦等雙(烷氧基)雙(β-二酮)鈦類;(2-甲基戊二氧基)雙(2,2,6,6-四甲基庚烷-3,5-二酮)鈦、(2-甲基戊二氧基)雙(2,6-二甲基庚烷-3,5-二酮)鈦等二醇基雙(β-二酮)鈦類;(甲基環戊二烯基)三(二甲基胺基)鈦、(乙基環戊二烯基)三(二甲基胺基)鈦、(環戊二烯基)三(二甲基胺基)鈦、(甲基環戊二烯基)三(乙基甲基胺基)鈦、(乙基環戊二烯基)三(乙基甲基胺基)鈦、(環戊二烯基)三(乙基甲基胺基)鈦、(甲基環戊二烯基)三(二乙基胺基)鈦、(乙基環戊二烯基)三(二乙基胺基)鈦、(環戊二烯基)三(二乙基胺基)鈦等(環戊二烯基)三(二烷基胺基)鈦類;(環戊二烯基)三(甲氧基)鈦、(甲基環戊二烯基)三(甲氧基)鈦、(乙基環戊二烯基)三(甲氧基)鈦、(丙基環戊二烯基)三(甲氧
基)鈦、(異丙基環戊二烯基)三(甲氧基)鈦、(丁基環戊二烯基)三(甲氧基)鈦、(異丁基環戊二烯基)三(甲氧基)鈦、(第三丁基環戊二烯基)三(甲氧基)鈦等(環戊二烯基)三(烷氧基)鈦類等,作為含有鋯之前驅物或含有鉿之前驅物,可列舉作為上述含有鈦之前驅物所例示的化合物中之鈦經鋯或鉿取代之化合物。
作為含有稀土元素之前驅物,可列舉下述式(III-1)~(III-3)所表示之化合物。
於上述含有稀土元素之前驅物中,作為M2所表示之稀土原子,可列舉:鈧、釔、鑭、鈰、鐠、釹、鉕、釤、銪、釓、鋱、鏑、鈥、鉺、銩、鐿、鎦,作為Ra、Rb、Rc、
Re、Rf、Rg及Rj所表示之基,可列舉上述鈦前驅物中所例示之基。
又,於本發明之薄膜形成用原料中,為賦予本發明之鋁化合物及其他前驅物之穩定性,視需要亦可含有親核性試劑。作為該親核性試劑,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-6、二環己基-18-冠-6、24-冠-8、二環己基-24-冠-8、二苯并-24-冠-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、三乙氧基三乙胺等聚胺類;四氮雜環十四烷(cyclam)、四氮雜環十二烷(cyclen)等環狀聚胺類;吡啶、吡咯啶、哌啶、啉、N-甲基吡咯啶、N-甲基哌啶、N-甲基啉、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;乙醯乙酸甲酯、乙醯乙酸乙酯、乙醯乙酸-2-甲氧基乙酯等β-酮酯類或乙醯丙酮、2,4-己二酮、2,4-庚二酮、3,5-庚二酮、二(三甲基乙醯基)甲烷等β-二酮類;該等親核性試劑之使用量相對於前驅物之總量1莫耳,較佳為0.1莫耳~10莫耳之範圍,更佳為1~4莫耳。
於本發明之薄膜形成用原料中,使其儘量不含構成其之成分以外之雜質金屬元素成分、雜質氯等雜質鹵素成分、及雜質有機成分。雜質金屬元素成分較佳為每種元素為100 ppb以下,更佳為10 ppb以下,以總量計較佳為1 ppm
以下,更佳為100 ppb以下。尤其於用作LSI之閘極絕緣膜、閘極膜、阻障層之情形時,必需減少對所獲得之薄膜之電氣特性存在影響之鹼金屬元素、鹼土金屬元素、及同族元素之含量。雜質鹵素成分較佳為100 ppm以下,更佳為10 ppm以下,進而較佳為1 ppm以下。雜質有機成分以總量計較佳為500 ppm以下,更佳為50 ppm以下,進而較佳為10 ppm以下。又,水分成為化學氣相沈積用原料中之微粒產生、或薄膜形成中之微粒產生之原因,因此關於金屬化合物、有機溶劑、及親核性試劑,為降低各自之水分,較佳為於使用時儘可能預先去除水分。金屬化合物、半金屬化合物、有機溶劑及親核性試劑各自之水分量較佳為10 ppm以下,進而較佳為1 ppm以下。
又,為降低或防止所形成之薄膜之微粒污染,本發明之薄膜形成用原料較佳為儘量不含微粒。具體而言,於液相下利用光散射式液中粒子檢測器之微粒測定中,較佳為大於0.3 μm之粒子數量於液相1 ml中為100個以下,更佳為大於0.2 μm之粒子數量於液相1 ml中為1000個以下,進而較佳為大於0.2 μm之粒子數量於液相1 ml中為100個以下。
作為使用本發明之薄膜形成用原料製造薄膜的本發明之薄膜之製造方法,係如下CVD法:將使本發明之薄膜形成用原料氣化而成之蒸氣、及視需要所使用之反應性氣體導入設置有基體之成膜腔室內,繼而,使前驅物於基體上分解及/或發生化學反應而於基體表面生長、沈積含有鋁之薄膜。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,可使用周知通常之條件、方法。
作為上述視需要所使用之反應性氣體,例如,作為氧化性者,可列舉: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、伸烷基二胺等有機胺化合物、肼、氨等,該等可使用一種或兩種以上。
又,作為上述輸送供給方法,可列舉上述所記載之氣體輸送法、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:僅藉由熱使原料氣體或原料氣體與反應性氣體反應而使薄膜沈積之熱CVD;使用熱與電漿之電漿CVD;使用熱與光之光CVD;使用熱、光及電漿之光電漿CVD;及將CVD之沈積反應分為基本過程,以分子等級階段性地進行沈積之ALD。
作為上述基體之材質,例如可列舉:矽;氮化矽、氮化鈦、氮化鉭、氧化鈦、氮化鈦、氧化釕、氧化鋯、氧化鉿、氧化鑭等陶瓷;玻璃;金屬釕等金屬。作為基體形狀,可列舉:板狀、球狀、纖維狀、鱗片狀,基體表面可為平面,亦可為溝槽(trench)結構等三維結構。
又,作為上述製造條件,可列舉:反應溫度(基體溫度)、反應壓力、沈積速度等。反應溫度係使本發明之鋁化合物充分反應之溫度,較佳為100℃以上,更佳為150℃~400℃。又,反應壓力於熱CVD、光CVD之情形
時,較佳為大氣壓~10 Pa,於使用電漿之情形時,較佳為2000 Pa~10 Pa。
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、反應壓力而控制。若沈積速度較大,則有所獲得之薄膜之特性惡化之情形,若較小,則有於生產性上產生問題之情形,因此較佳為0.01~100 nm/min,更佳為1~50 nm/min。又,於ALD法之情形時,為獲得所需之膜厚,以循環次數進行控制。
作為上述製造條件,進而可列舉使薄膜形成用原料氣化而形成蒸氣時之溫度或壓力。使薄膜形成用原料氣化而形成蒸氣之步驟可於原料容器內進行,亦可於氣化室內進行。於任一情形下,本發明之薄膜形成用原料均較佳為於0~150℃下蒸發。又,於原料容器內或氣化室內使薄膜形成用原料氣化而形成蒸氣之情形時,原料容器內之壓力及氣化室內之壓力均較佳為1~10000 Pa。
本發明之薄膜之製造方法除了包含採用ALD法,藉由上述輸送供給方法,使薄膜形成用原料氣化形成蒸氣,將該蒸氣導入成膜腔室內的原料導入步驟以外,亦可包含:藉由該蒸氣中之上述鋁化合物於上述基體表面形成前驅物薄膜的前驅物薄膜成膜步驟;將未反應之鋁化合物氣體排出之排氣步驟;及使該前驅物薄膜與反應性氣體發生化學反應,於該基體表面形成上述含有鋁之薄膜的含有鋁之薄膜形成步驟。
以下,針對上述各步驟,以形成氧化鋁薄膜之情形為例
詳細地說明。於藉由ALD法形成氧化鋁薄膜之情形時,首先,進行上述所說明之原料導入步驟。使薄膜形成用原料形成蒸氣時之較佳之溫度或壓力係與上述所說明者相同。其次,藉由導入沈積反應部之鋁化合物,於基體表面使前驅物薄膜成膜(前驅物薄膜成膜步驟)。此時,可對基體進行加熱或亦可對沈積反應部進行加熱而施加熱。於該步驟中所成膜之前驅物薄膜係氧化鋁薄膜、或使鋁化合物之一部分分解及/或反應而生成之薄膜,具有與目標之氧化鋁薄膜不同之組成。本步驟進行時之基體溫度較佳為室溫~500℃,更佳為150~350℃。本步驟進行時之系統(成膜腔室內)壓力較佳為1~10000 Pa,更佳為10~1000 Pa。
繼而,自沈積反應部將未反應之鋁化合物氣體或副生成之氣體排出(排氣步驟)。較理想為未反應之鋁化合物氣體或副生成之氣體自沈積反應部完全排出,但未必需要完全排出。作為排氣方法,可列舉:藉由氮氣、氦氣、氬氣等惰性氣體沖洗(purge)系統內之方法;藉由對系統內進行減壓而排氣之方法;以及組合該等之方法等。進行減壓之情形時之減壓度較佳為0.01~300 Pa,更佳為0.01~100 Pa。
繼而,向沈積反應部導入氧化性氣體,藉由該氧化性氣體或氧化性氣體及熱之作用,由先前之前驅物薄膜成膜步驟中所獲得之前驅物薄膜形成氧化鋁薄膜(含有鋁之薄膜形成步驟)。於本步驟中發揮熱之作用之情形時之溫度較佳為室溫~500℃,更佳為150~350℃。本步驟進行時之系統(成膜腔室內)壓力較佳為1~10000 Pa,更佳為10~1000
Pa。本發明之鋁化合物與氧化性氣體之反應性良好,可獲得氧化鋁薄膜。
於本發明之薄膜之製造方法中,於如上述般採用ALD法之情形時,亦可將利用包含上述原料導入步驟、前驅物薄膜成膜步驟、排氣步驟、及含有鋁之薄膜形成步驟之一系列操作之薄膜沈積設為1次循環,將該循環重複複數次直至獲得必需之膜厚之薄膜。於此情形時,較佳為進行1次循環後,以與上述排氣步驟相同之方式自沈積反應部將未反應之鋁化合物氣體及反應性氣體(於形成氧化鋁薄膜之情形時為氧化性氣體)、進而副生成之氣體排出,然後進行下1次循環。
又,於氧化鋁薄膜之利用ALD法之形成中,亦可施加電漿、光、電壓等能量。施加該等能量之時間點並無特別限定,例如,可為原料導入步驟中之鋁化合物氣體導入時、前驅物薄膜成膜步驟或含有鋁之薄膜形成步驟中之加溫時、排氣步驟中之系統內之排氣時、含有鋁之薄膜形成步驟中之氧化性氣體導入時,亦可為上述各步驟之間。
又,於本發明之薄膜之製造方法中,亦可於薄膜沈積之後,為獲得更良好之電氣特性而於惰性環境下、氧化性環境下或還原性環境下進行退火處理,於必需階梯覆蓋性之情形時,亦可設置回焊步驟。此情形時之溫度為200~1000℃,較佳為250~500℃。
使用本發明之薄膜形成用原料製造薄膜之裝置可使用周知之化學氣相沈積法用裝置。作為具體之裝置之例,可列
舉:如圖1之非簇射頭型裝置、或如圖2之可藉由起泡供給前驅物而進行之裝置、或如圖3之包含氣化室之裝置。又,不限於如圖1、圖2、圖3之單片式裝置,亦可利用使用分批爐之可同時處理多片之裝置。上述成膜腔室於圖2中記載為「反應成膜室」,於圖3中記載為「薄膜沈積部」。
使用本發明之薄膜形成用原料製造之薄膜可藉由適當選擇其他前驅物、反應性氣體及製造條件,而形成金屬、氧化物陶瓷、氮化物陶瓷、玻璃等所需種類之薄膜。作為所製造之含有鋁之薄膜,例如可列舉鋁金屬薄膜或鋁系陶瓷薄膜等。作為上述鋁系陶瓷薄膜,可列舉以鋁氮化物薄膜、鋁氧化物薄膜、或鈦酸鋁為代表的含有鋁之複合金屬系氧化物薄膜等。該等可廣泛用於LSI之配線材料;機械零件或工具等之硬質塗層膜;半導體記憶體之絕緣膜、閘極絕緣膜、介電質膜;硬碟用MR頭等電子零件;光通信用電路等之光學玻璃;觸媒等之製造中。
以下,藉由實施例及評價例進一步詳細地說明本發明。然而,本發明並不受以下實施例等之任何限制。
於氬氣環境下,將於反應燒瓶中向經脫水處理之甲苯溶液460 g中溶解三甲基鋁52.9 g而成之溶液於冰冷浴中進行攪拌,使之冷卻至0℃附近,歷時3小時緩緩滴加經脫水處理之外消旋體之第二丁醇54.4 g。將反應中所產生之甲烷
氣體藉由氬氣之通氣而蒸餾去除。其後,恢復至室溫,反應約20小時。其後,將甲苯於浴100℃、減壓下蒸餾去除,獲得液體殘渣。將該液體於190 Pa之減壓下、浴100℃下蒸餾,獲得於塔頂溫度70℃下餾出之化合物。利用該純化獲得之回收率為79%。所獲得之化合物於室溫下為液體,進行元素分析及1H-NMR(Nuclear Magnetic Resonance,核磁共振)分析,結果確認其為作為目標物之本發明之鋁化合物。將該等分析結果表示如下。以下,亦一併表示TG-DTA(Thermo Gravimetric Differential Thermal Analysis,熱重差熱同步分析)之結果。
(分析值)
(1)元素分析(金屬分析:ICP-AES(Inductively Coupled Plasma-Atomic Emission Spectroscopy,感應耦合電漿-原子發射光譜))
鋁:19.7質量%(理論值20.73質量%),C:54.09質量%、H:12.58質量%(理論值C:55.36質量%、H:11.62質量%)
(2)1H-NMR(溶劑:氘苯)(化學位移:多重性:H數)
(-0.448 ppm:s:6)(0.666 ppm:t:3)(1.028 ppm:d:3)(1.251 ppm:m:1)(1.481 ppm:m:1)(3.628 ppm:sext:1)
(3)TG-DTA
TG-DTA(Ar 100 ml/min、10℃/min升溫、試樣量9.791 mg)50質量%減少溫度為136℃
關於本發明之鋁化合物及以下所示之比較化合物1、2及3,藉由放置於大氣中而確認有無可燃性。將結果示於表1。
根據表1之結果,可知比較化合物1於大氣中表現可燃性。就安全性之方面而言,表現可燃性之化合物不易作為化學氣相沈積用原料進行處理。可知本發明之鋁化合物以及比較化合物2及3未表現出可燃性,於大氣中亦可安全使用。
關於作為無可燃性之化合物的本發明之鋁化合物以及比較化合物2及3,使用微小熔點測定裝置對20℃下為固體者測定熔點。又,使用TG-DTA測定裝置,確認藉由Ar環境下之加熱使試樣重量減少50質量%之時間點的溫度。將結
果示於表2。
根據表2之結果,可確認本發明之鋁化合物及比較化合物2係常溫(20℃)下為液體之化合物或表現出較高之蒸氣壓之化合物。又,可知比較化合物3於常溫下為固體,熔點較高。於將熔點較高之化合物用作化學氣相沈積用原料之情形時,為於液體狀態下進行輸送而必需大量能量,因此於能量方面較為不利。
關於作為常溫下為液體之化合物的本發明之鋁化合物及比較化合物2,使用DSC(Differential Scanning Calorimetry,示差掃描熱析法)測定裝置測定產生熱分解之溫度,藉此確認各化合物之熱穩定性。將結果示於表3。
根據表3之結果,可知本發明之鋁化合物表現出400℃以
上之非常高之熱穩定性。與此相對,可知比較化合物2於200℃附近之低溫下產生熱分解。由此可知,本發明之鋁化合物係表現出尤為優異之熱穩定性之化合物。
將上述實施例1中獲得之本發明之鋁化合物作為化學氣相沈積用原料,使用圖3所示之裝置,藉由以下條件之ALD法於矽晶圓上製造氧化鋁薄膜。對所獲得之薄膜進行利用X射線反射率法之膜厚測定、利用X射線繞射法及X射線光電子分光法之薄膜結構及薄膜組成之確認,結果膜厚為6 nm,膜組成為氧化鋁,碳含量為1 atom%。
(條件)
反應溫度(基體溫度):300℃,反應性氣體:臭氧
(步驟)
將包含下述(1)~(4)之一系列步驟設為1次循環,重複進行150次循環。
(1)將於氣化室溫度:45℃、氣化室壓力:1.1 Torr(147 Pa)之條件下氣化而成之化學氣相沈積用原料之蒸氣導入成膜腔室內,於系統壓力1 Torr(133 Pa)下,在矽晶圓表面沈積10秒。
(2)藉由20秒之氬氣沖洗,去除未反應原料。
(3)導入反應性氣體,於系統壓力1 Torr(133 Pa)下反應10秒。
(4)藉由20秒之氬氣沖洗,去除未反應原料。
1‧‧‧成膜腔室
2‧‧‧壓力計
3‧‧‧MFC(質量流量控制器)
4‧‧‧沖洗氣體
5‧‧‧反應性氣體
6‧‧‧加熱器
7‧‧‧原料容器
8‧‧‧阱
9‧‧‧真空泵
10‧‧‧排氣
11‧‧‧載體氣體
12‧‧‧密封氣體
13‧‧‧反應成膜室
14‧‧‧自動壓力控制器
15‧‧‧氣化室
16‧‧‧薄膜沈積部
圖1係表示本發明之含有鋁之薄膜之製造方法中所使用的化學氣相沈積用裝置之一例之概要圖。
圖2係表示本發明之含有鋁之薄膜之製造方法中所使用的化學氣相沈積用裝置之另一例之概要圖。
圖3係表示本發明之含有鋁之薄膜之製造方法中所使用的化學氣相沈積用裝置之另一例之概要圖。
1‧‧‧成膜腔室
2‧‧‧壓力計
3‧‧‧MFC(質量流量控制器)
4‧‧‧沖洗氣體
5‧‧‧反應性氣體
6‧‧‧加熱器
7‧‧‧原料容器
8‧‧‧阱
9‧‧‧真空泵
10‧‧‧排氣
Claims (3)
- 一種鋁化合物,其係下述化學式(I)所表示者,
- 一種薄膜形成用原料,其係含有如請求項1之鋁化合物而成。
- 一種薄膜之製造方法,其係將使如請求項2之薄膜形成用原料氣化而獲得的含有上述鋁化合物之蒸氣導入設置有基體之成膜腔室內,使該鋁化合物分解及/或發生化學反應而於該基體表面形成含有鋁之薄膜。
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