TW201223957A - Magnesium bis(dialkyl amide) compound and method of producing magnesium-containing thin film using same - Google Patents
Magnesium bis(dialkyl amide) compound and method of producing magnesium-containing thin film using same Download PDFInfo
- Publication number
- TW201223957A TW201223957A TW100128015A TW100128015A TW201223957A TW 201223957 A TW201223957 A TW 201223957A TW 100128015 A TW100128015 A TW 100128015A TW 100128015 A TW100128015 A TW 100128015A TW 201223957 A TW201223957 A TW 201223957A
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- Prior art keywords
- magnesium
- group
- compound
- bis
- isopropyl
- Prior art date
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000011777 magnesium Substances 0.000 title claims abstract description 42
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 40
- 150000001875 compounds Chemical class 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000010409 thin film Substances 0.000 title claims abstract description 7
- 150000001408 amides Chemical class 0.000 title claims abstract description 5
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 title abstract 2
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 35
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims abstract description 24
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 17
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 15
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims abstract description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 239000010408 film Substances 0.000 claims description 39
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 125000005265 dialkylamine group Chemical group 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 5
- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004429 atom Chemical group 0.000 claims description 3
- 125000005843 halogen group Chemical group 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-O guanidinium Chemical compound NC(N)=[NH2+] ZRALSGWEFCBTJO-UHFFFAOYSA-O 0.000 claims 1
- -1 calcined magnesium Chemical class 0.000 description 23
- 238000000151 deposition Methods 0.000 description 16
- 230000008021 deposition Effects 0.000 description 15
- 239000007789 gas Substances 0.000 description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 15
- 239000000243 solution Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 4
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 4
- 238000002309 gasification Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 4
- 229910052707 ruthenium Inorganic materials 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 150000004796 dialkyl magnesium compounds Chemical class 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- MEKOFIRRDATTAG-UHFFFAOYSA-N 2,2,5,8-tetramethyl-3,4-dihydrochromen-6-ol Chemical compound C1CC(C)(C)OC2=C1C(C)=C(O)C=C2C MEKOFIRRDATTAG-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- USZGMDQWECZTIQ-UHFFFAOYSA-N [Mg](C1C=CC=C1)C1C=CC=C1 Chemical compound [Mg](C1C=CC=C1)C1C=CC=C1 USZGMDQWECZTIQ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 229910012375 magnesium hydride Inorganic materials 0.000 description 2
- KJJBSBKRXUVBMX-UHFFFAOYSA-N magnesium;butane Chemical compound [Mg+2].CCC[CH2-].CCC[CH2-] KJJBSBKRXUVBMX-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- MFGBPWSFVCIOQG-UHFFFAOYSA-N n-butyl-2-methylbutan-2-amine Chemical group CCCCNC(C)(C)CC MFGBPWSFVCIOQG-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N n-butylhexane Natural products CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-SVYQBANQSA-N oxolane-d8 Chemical compound [2H]C1([2H])OC([2H])([2H])C([2H])([2H])C1([2H])[2H] WYURNTSHIVDZCO-SVYQBANQSA-N 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- JUGRTVJQTFZHOM-UHFFFAOYSA-N 1,1,1-tribromo-2-methylpropan-2-ol Chemical compound CC(C)(O)C(Br)(Br)Br JUGRTVJQTFZHOM-UHFFFAOYSA-N 0.000 description 1
- HQDYNFWTFJFEPR-UHFFFAOYSA-N 1,2,3,3a-tetrahydropyrene Chemical compound C1=C2CCCC(C=C3)C2=C2C3=CC=CC2=C1 HQDYNFWTFJFEPR-UHFFFAOYSA-N 0.000 description 1
- PUNXVEAWLAVABA-UHFFFAOYSA-N 1,2,3,4-tetrahydroanthracene;1,2,5,6-tetrahydroanthracene Chemical compound C1=CC=C2C=C(CCCC3)C3=CC2=C1.C1=CCCC2=C1C=C1CCC=CC1=C2 PUNXVEAWLAVABA-UHFFFAOYSA-N 0.000 description 1
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical compound C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- MPPPKRYCTPRNTB-UHFFFAOYSA-N 1-bromobutane Chemical compound CCCCBr MPPPKRYCTPRNTB-UHFFFAOYSA-N 0.000 description 1
- GGVXCUYZOPPOAM-UHFFFAOYSA-N 1-butyl-1-ethylhydrazine Chemical group CCCCN(N)CC GGVXCUYZOPPOAM-UHFFFAOYSA-N 0.000 description 1
- VHJBXKJRGJVSOZ-UHFFFAOYSA-N 10,10-dibutyltetradecan-1-amine Chemical compound C(CCC)C(CCCCCCCCCN)(CCCC)CCCC VHJBXKJRGJVSOZ-UHFFFAOYSA-N 0.000 description 1
- WKYYYUWKFPFVEY-UHFFFAOYSA-N 2-ethylcyclohexan-1-one Chemical compound CCC1CCCCC1=O WKYYYUWKFPFVEY-UHFFFAOYSA-N 0.000 description 1
- GELMWIVBBPAMIO-UHFFFAOYSA-N 2-methylbutan-2-amine Chemical compound CCC(C)(C)N GELMWIVBBPAMIO-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- QWOJMRHUQHTCJG-UHFFFAOYSA-N CC([CH2-])=O Chemical compound CC([CH2-])=O QWOJMRHUQHTCJG-UHFFFAOYSA-N 0.000 description 1
- UQCZAENLOPBRPU-UHFFFAOYSA-N CCCCC(CCCC)C(C)(CCCC)N Chemical compound CCCCC(CCCC)C(C)(CCCC)N UQCZAENLOPBRPU-UHFFFAOYSA-N 0.000 description 1
- ODHFJIDDBSDWNU-UHFFFAOYSA-N CCCC[Mg]CCCC Chemical compound CCCC[Mg]CCCC ODHFJIDDBSDWNU-UHFFFAOYSA-N 0.000 description 1
- KONHWGKXRVKMAB-UHFFFAOYSA-N CC[N-]C(=NC(C)(C)C)N.CC[N-]C(=NC(C)(C)C)N.[Mg+2] Chemical compound CC[N-]C(=NC(C)(C)C)N.CC[N-]C(=NC(C)(C)C)N.[Mg+2] KONHWGKXRVKMAB-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000238366 Cephalopoda Species 0.000 description 1
- 239000005947 Dimethoate Substances 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- QECVIPBZOPUTRD-UHFFFAOYSA-N N=S(=O)=O Chemical compound N=S(=O)=O QECVIPBZOPUTRD-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000004990 Smectic liquid crystal Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 240000002816 Syzygium buxifolium Species 0.000 description 1
- XBDYBAVJXHJMNQ-UHFFFAOYSA-N Tetrahydroanthracene Natural products C1=CC=C2C=C(CCCC3)C3=CC2=C1 XBDYBAVJXHJMNQ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical group [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 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 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 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 1
- 238000010586 diagram Methods 0.000 description 1
- 125000004663 dialkyl amino group Chemical group 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000006138 lithiation reaction Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- YHNWUQFTJNJVNU-UHFFFAOYSA-N magnesium;butane;ethane Chemical compound [Mg+2].[CH2-]C.CCC[CH2-] YHNWUQFTJNJVNU-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QHCCDDQKNUYGNC-UHFFFAOYSA-N n-ethylbutan-1-amine Chemical group CCCCNCC QHCCDDQKNUYGNC-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
- OKRJGUKZYSEUOY-UHFFFAOYSA-N n-propan-2-ylbutan-1-amine Chemical group CCCCNC(C)C OKRJGUKZYSEUOY-UHFFFAOYSA-N 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- CATWEXRJGNBIJD-UHFFFAOYSA-N n-tert-butyl-2-methylpropan-2-amine Chemical group CC(C)(C)NC(C)(C)C CATWEXRJGNBIJD-UHFFFAOYSA-N 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229940070710 valerate Drugs 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium 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
- C23C16/22—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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C211/00—Compounds containing amino groups bound to a carbon skeleton
- C07C211/65—Metal complexes of amines
-
- 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
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/02—Magnesium compounds
-
- 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
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Abstract
Description
201223957 六、發明說明: 【發明所屬之技術領域】 本發明係關於一種新穎的雙(二烷基醯胺基)鎂化合物,及利用 該鎂化合物、藉由化學氣相沈積法(Chemical Vapor Deposition法; 以下稱為CVD法)製造含鎂薄膜的方法。 【先前技術】 迄今’作為含鎂薄膜製造用的鎂化合物,例如,烧基鎂、烧 氧化鎂、二嗣鎮(magnesium diketonate)等多種類的鎂化合物被研究 (例如,參照專利文獻丨〜幻。其中又以雙(環戊二烯基)鎮或其有關 化合物係主要被使用中的化合物。 另一方面,作為用以形成含鈦薄膜、含锆薄膜、含铪薄膜、 含銘薄膜等其他的含金㈣膜的原料,具有二絲_基配位子 的化合物被提出(參照專利文獻3)。 此外’也已知有雙(二烷基醯胺基)鎂化合物,其被利用於作 例如,聚合用觸媒、醫藥、或農藥等之製造原料 夂昭直 利文獻1及專利文獻4)。 …,、、非專 [習知技術文獻] [專利文獻] [專利文獻1]曰本特開2002-170993號公報 [專利文獻2]日本特開2005_298874號公報 [專利文獻3]日本特開2007-153869號公報 [專利文獻4]歐洲專利申請案第i〇3158l號 [非專利文獻] 曰 (1978[)非專利文獻 1U 〇取㈤瓜,V°L43,Na8,PP.1564·1566 【發明内容】 [發明所欲解決的問題] 然而,在含鎂_之製造中· f知賴化合物其蒸氣壓、熱 4 201223957 穩定^生、反應性等物性未必是最適合的,即使是目前最常使用的 ,(%<戊二贼)鎂’也無法稱其為用崎造含鎂賊之充分的鎮化 合物:因此,-直以來都在謀求蒸氣M、熱舣性、反應性等物 性均得以滿足的鎮化合物。 亦即,本發明之課題為解決上述問題,並提供一種鎮化合物, 其係π以藉由簡便的方法製造含鎂薄膜之工業上適用的鎂化合 物’更具體而言’係適用於藉由CVD法製造含鎂薄膜者。又,本 發明之課題為提供一種利用該鎂化合物之含鎂薄膜之製造方法。 發明係關於以下之事項。 1. 一種以通式(1)表示之雙(二烷基醯胺基)鎂化合物 RVMg、N/R1 I ⑴ R2 R2 _(式中,R表不異丙基、或碳原子數4〜6之分支狀的烷基,R2 表2示碳原子數1〜5之錢狀或分支狀的絲。但是,排除Ri及 R均气異丙基之情況、:^及R2均為異丁基之情況、及Rl為異丙 基且R-為曱基之情況。)。 2.7種雙(二烧基酿胺基)鎂化合物的製造方法,該雙(二烷基醯 胺基)鎮化合物係以上述通式(1)表示之雙(二烷基醯胺基)鎂化合 物,忒製造方法的特徵在於包含以下步驟: 使以通式(2)表示之二烷基鎂化合物 .Mg R 、R4 (2) (式中’ R3及R4可以相同亦可不同,分別相互獨立地表示碳 原子數1〜10之直鏈狀或分支狀的烧基。) 與以通式⑶表示之二院基胺反應的步驟 /R1201223957 VI. Description of the Invention: [Technical Field] The present invention relates to a novel bis(dialkylguanidinyl)magnesium compound, and the use of the magnesium compound by chemical vapor deposition (Chemical Vapor Deposition method) The method of producing a magnesium-containing film is hereinafter referred to as a CVD method. [Prior Art] As a magnesium compound for the production of a magnesium-containing film, for example, magnesium compounds such as calcined magnesium, burned magnesia, and magnesium diketonate have been studied (for example, refer to the patent document 丨~幻Among them, bis(cyclopentadienyl) or its related compounds are mainly used as compounds. On the other hand, as a titanium-containing film, a zirconium-containing film, a ytterbium-containing film, a film containing a film, etc. A raw material containing a gold-containing (tetra) film, and a compound having a two-chain ligand is proposed (see Patent Document 3). Further, a bis(dialkylguanidino) magnesium compound is also known, which is used for For example, a raw material for the production of a catalyst, a medicine, or a pesticide for polymerization, and the like, and the patent document 4). , 、 习 习 习 习 习 习 2002 2002 2002 2002 2002 2002 2002 2002 2002 2007 2007 2007 2007 2007 2007 2002 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 2007 [Patent Document 4] European Patent Application No. i No. 3158l [Non-Patent Document] 曰 (1978 [) Non-Patent Document 1U Extraction (5) Melon, V°L43, Na8, PP.1564·1566 [Invention Contents] [Problems to be Solved by the Invention] However, in the production of magnesium-containing products, the vapor pressure, heat 4 201223957 stability, reactivity, and other physical properties are not necessarily the most suitable, even at present. The use of (% < E. sinensis) magnesium can not be called as a sufficient town compound for the use of magnesium-containing thieves: therefore, - directly seeking vapor M, enthalpy, reactivity and other physical properties The town compound that is met. That is, the object of the present invention is to solve the above problems, and to provide an ionic compound which is an industrially applicable magnesium compound for producing a magnesium-containing film by a simple method, and more specifically, is suitable for CVD by CVD. The method of manufacturing magnesium-containing film. Further, an object of the present invention is to provide a method for producing a magnesium-containing film using the magnesium compound. The invention relates to the following matters. A bis(dialkylguanidinyl)magnesium compound RVMg represented by the formula (1), N/R1 I (1) R2 R2 _ (wherein R represents an isopropyl group or a carbon number of 4 to 6) Branched alkyl group, R2 Table 2 shows a money or branched filament having 1 to 5 carbon atoms. However, in the case where Ri and R are both isopropyl, R and R2 are isobutyl groups. The case, and the case where R1 is an isopropyl group and R- is a fluorenyl group.). A method for producing 2.7 kinds of bis(dialkylamino) magnesium compounds which are bis(dialkylguanidino) magnesium compounds represented by the above formula (1) The crucible manufacturing method is characterized by comprising the steps of: disposing a dialkyl magnesium compound represented by the general formula (2): Mg R and R 4 (2) (wherein R 3 and R 4 may be the same or different and independently of each other A linear or branched alkyl group having 1 to 10 carbon atoms.) A step of reacting with a diamine amine represented by the general formula (3) / R1
HN I (3) R2 201223957 (式中’ Rl表示異丙基、或碳原子數4〜6之分支狀的烷基,R2 表示碳原子數1〜5之直鏈狀或分支狀的烷基。但是,排除Ri及 R2均為異丙基之情況、R]及R2均為異丁基之情況、及R1為異丙 基且R2為曱基之情況。)。 3.—種雙(一燒基酸胺基)鎂化合物的製造方法’該雙(二烧基酸 胺基)鎂化合物係以上述通式(1)表示之雙(二烷基醯胺基)鎂化合 物,該製造方法的特徵在於包含以下步驟: 使以通式(3)表示之二烧基胺 /R1HN I (3) R2 201223957 (wherein R1 represents an isopropyl group or a branched alkyl group having 4 to 6 carbon atoms, and R2 represents a linear or branched alkyl group having 1 to 5 carbon atoms. However, the case where both Ri and R2 are isopropyl groups, the case where both R) and R2 are isobutyl groups, and the case where R1 is an isopropyl group and R2 is a fluorenyl group are excluded. 3. A method for producing a bis(monoalkyl amide) magnesium compound, wherein the bis(dialkyl amide) magnesium compound is a bis(dialkylguanidino) group represented by the above formula (1) A magnesium compound, which is characterized by comprising the steps of: using a dialkylamine represented by the formula (3) / R1
HN I (3) R2 (式中,R1表示異丙基、或碳原子數4〜6之分支狀的烷基,r2 表2不碳原子數1〜5之直離或分支狀基。但是,排除Rl及 丙曱=^及¥均為異丁基之情況、及Rl為異丙 物的^基=應,岭細赋(4)表示之二絲_基鐘化合HN I (3) R2 (wherein R1 represents an isopropyl group or a branched alkyl group having 4 to 6 carbon atoms, and r2 represents a straight or branched group having 1 to 5 carbon atoms. Excluding Rl and propylene 曱 = ^ and ¥ are isobutyl groups, and Rl is isopropyl ^ base = should, Ling fine (4) indicates the second wire _ base clock combination
LiN-^ 丨2 (4) R2 (式中,R及R2係與上述者同義。) -夕!!,ί(4)表不之二烷基醯胺基鋰化合物盘以通弋⑸矣 不之一鹵化鎬反應的步驟 /、通式(5)表 (5)LiN-^ 丨2 (4) R2 (where R and R2 are synonymous with the above.) - Xi! !, ί(4) indicates a step of reacting a dialkyl guanamine lithium compound disk with a ruthenium (5) 矣 not one of ruthenium halides. / (5)
MgX2 (式中,X表示鹵素原子 4. 一種含鎂薄膜之製造方半 雙(二烷基醯胺基)鎂化合物作為二仏览用^上述通式(1)表示之 之含鎮薄膜之製造方法。’’、、、’ Λ、、、·α源之藉由化學氣相沈積法 5. 一種含__賴原料,其包含以上述通式⑴表示之雙 6 201223957 C二烷基醯胺基)鎂化合物。 [發明之效果] 祕以提供特別適用於藉由cvd *之成膜之新穎 的又(一烧基酉邊基)鎂化合物。利用該鎂化合物,可以藉由c 法以良好的成膜的特性製造含鎂薄膜。 【實施方式】 本發明之雙(一烷基酸胺基)鎂化合物係以上述通式⑴表示。 在該通式(1)中,R1表示異丙基、三級丁基、三級戍基 戊基等碳原子數j〜6之分支狀的絲,示甲基、乙基、異丙 基、三級丁基、三級戍基、新戊基等碳原子數卜5之直鍵狀或分 支狀的烷基。但是,排除Ri及R2均為異丙基之情況、Rl及R2均 為異丁基之情況、及R1為異丙基且R2為曱基之情況。 _兩個Rl可以不同、兩個R2也可以不同,然而由於兩個R1相 同、且兩個R2也相同的化合物比較容易合成,因此較佳。 作為2本發明之較佳態樣’ R1為碳原子數4〜5之分支狀的燒 基1且R2為碳原子數丨〜5之直鏈狀或分支狀的烷基。作為Rl,^ 別疋較仏為二級丁基、二級戍基、新戊基。作為R2,特別g齡估 為甲基、乙基、異丙基、三級丁基、三級戊基、新戊基。 較佳為三級丁基、三級戊基,更佳為三級丁基;R2較佳為碳原子 數1〜5之直鏈狀或分支狀的烷基,更佳為曱基、乙基、異丙基、 三級丁基、三級戊基、新戊基。 土 作為本發明之雙(二烷基醯胺基)鎂化合物,可列舉:例如,藉 由下式(6)〜(20)表示之化合物。 7 201223957MgX2 (wherein, X represents a halogen atom. 4. Production of a magnesium-containing thin film. The production of a semi-bis(dialkylguanidinyl) magnesium compound as a two-layered film is produced by the above-mentioned general formula (1). Method of '',,, ' Λ,,, · α source by chemical vapor deposition method 5. A _ _ _ _ raw material comprising bis 6 201223957 C dialkyl decylamine represented by the above formula (1) Base) magnesium compound. [Effects of the Invention] The present invention provides a novel (a pyridyl) group of magnesium compounds which are particularly suitable for film formation by cvd*. With this magnesium compound, a magnesium-containing thin film can be produced by the c method with good film forming properties. [Embodiment] The bis(monoalkylamino)magnesium compound of the present invention is represented by the above formula (1). In the above formula (1), R1 represents a branched filament having a carbon number of from j to 6 such as an isopropyl group, a tertiary butyl group or a tertiary decylpentyl group, and represents a methyl group, an ethyl group, an isopropyl group, or the like. A straight-chain or branched alkyl group having a carbon number of 5 such as a tertiary butyl group, a tertiary sulfhydryl group or a neopentyl group. However, the case where both Ri and R2 are isopropyl groups, the case where both R1 and R2 are isobutyl groups, and the case where R1 is an isopropyl group and R2 is a fluorenyl group are excluded. _ Two R1 may be different, and two R2 may be different. However, since two compounds having the same R1 and the same two R2 are relatively easy to synthesize, it is preferable. The preferred embodiment of the present invention is as follows: R1 is a branched alkyl group having 4 to 5 carbon atoms, and R2 is a linear or branched alkyl group having a carbon number of 丨5. As Rl, ^ is not a secondary butyl group, a second sulfhydryl group, a neopentyl group. As R2, it is estimated that it is a methyl group, an ethyl group, an isopropyl group, a tertiary butyl group, a tertiary pentyl group or a neopentyl group. Preferably, it is a tertiary butyl group, a tertiary pentyl group, more preferably a tertiary butyl group; and R2 is preferably a linear or branched alkyl group having 1 to 5 carbon atoms, more preferably a fluorenyl group or an ethyl group. , isopropyl, tert-butyl, tertiary pentyl, neopentyl. Soil The bis(dialkylguanidinium) magnesium compound of the present invention may, for example, be a compound represented by the following formulas (6) to (20). 7 201223957
本發明之雙(二烷基醯胺基)鎂化合物的合成可以藉由以下之 以(A)或(B)表示的方法(以下,也稱為本發明的反應。)進行。 8 201223957The synthesis of the bis(dialkylguanidino)magnesium compound of the present invention can be carried out by the method represented by the following (A) or (B) (hereinafter, also referred to as the reaction of the present invention). 8 201223957
(式中’R1及R2係與上述者同義,R3及R4表示碳原子數丨〜仞 之直鏈狀或分支狀的烷基。此外,R3及R4可以相同亦可不同。又, X表示鹵素原子。) [方法㈧] 方法(A)係使二烧基鎂化合物與二烧基胺反應,以合成雙(二烧 基酸胺基)鎮化合物的方法。 在本發明的反應(A)中利用的二烷基鎂化合物以上述通式 表示。在該通式(;2)中,R3及R4表示曱基、乙基、正丙基、異丙基、 正I基、異丁基、三級丁基、正戊基、三級戊基、新戊基、正癸 基等碳原子數1〜10之直鏈狀或分支狀的烷基。此外,尺3及R4可 以相同亦可不同。 作為在本發明的反應(A)中利用的二烷基鎂化合物,可以利用 市售品,又,可以藉由周知的方法從金屬鎂製造。在本發明的反 應(A),,適當地利用二(正丁基)鎂或正丁基乙基鎂等。 一隹本發明的反應(A)中利用的二烷基胺以上述之通式(3)表 示。在該通式(3)中,r1及R2分別對應於式(1)中之R1及R2,盥上 述者同義。 ^ 因此,作為在本發明的反應(A)中利用的二烷基胺,較佳為三 級"I基Γ基胺、三級丁基乙基胺、三級丁基異丙基胺、二三級丁 基胺、二級丁基三級戊基胺、二三級戊基胺等。 9 201223957 上述二烷基胺的使用量係相對於二 1.5〜3.0莫耳、更佳為1.8〜2 2莫耳。、—凡基鎂1莫耳,較佳為 本發明的反應(A)較佳為在有撫a w a ^ 機溶劑,只妓不會抑制反進行。作為所利用的有 可列舉:例如,二乙_、即可^無特別限制,然而 _頁;己烧、庚烧、環己炫、甲基;:曱2,、—,陸圜等 烴類;甲苯、二曱苯等芳香族烴己烧等脂肪族 單獨使用或混合兩種以上使用。ή匕外5亥4有機溶劑可以 述制量係相對於二絲鎂b較佳為 本發明的反應(A)係藉由,例如 胺、及有機溶劑-邊混合、攪掉_、喜3化合物、二烷基 時的反應溫度較佳為_20〜12(rct更方;^行。反應 特別限制。 Μ為G〜⑽C ’反應壓力並無 [方法(B)] •化:ίΓ係基成的二烧基醯胺基鐘與二 取又(一沉基鹺胺基)鎂化合物的方法。 舉雜__,然而可列 鋰等,然而較佳為利用正丁基鐘。土、一級丁基鐘、三級丁基 基次從合成二_胺 該通反表=用的r傾以1述通式⑶表心在 表不氣原子、氯原子、溴原子、峨原子等齒素原 10 201223957 子,然而較佳為氯原子。 1莫耳,較佳為 情況下,二烧基_餘的使量^基酿胺基鋰_的 佳為L5〜3.0莫耳、更佳為18〜^=對於二鹵化鎮丨莫耳,較 mrn^ 可列舉:例如,二乙基醚、四氫呋喃、:別限制,然而 醚類;己烷、庚烷、環己烷、甲其 二τ軋乙烷、二氧陸園等 烴類;甲苯、二甲苯等芳香族烴口乙基環己燒等脂肪族 類、或_類與脂肪族烴類的混合溶劑。乂外利=類、脂肪族烴 單獨使用或混合兩種以上使用。θ 卜’§亥寻有機溶劑可以 上述有機溶劑的使用量係相 1〜I00g、更佳為WOge在將_ 烷基胺Ig,較佳為 院細胺基_二_麟反基料_情況下,使二 齒化鎮lg,較佳為的使用量係相對於二 本發明的反應⑼係藉由,例如^方 烧基胺、餘μ、及機^即,將二 合成二烧基醯胺基經化合物,接莫 _ 邊吏,、反應,以 細纖、二咖、及有::二丄接=得,二 反應等方法。反應時的反應温度較1佳=二^「邊使其 〇〜50(:,反應壓力並無特別限制。 ^ c、更佳為 合物與二_化鎂反應之前,可以—。吏一烷基醯胺基鋰化 直接利用該反應液,又,也可以適當=離而 有機溶劑。 更除去、及/或者追加 藉由本發明的反應(A)或(b),可 胺基)鎂化合物。在反應終了後,藉由萃V過广二ϊ基酸 昇華、再結晶、管柱層析法等周知的==慮6、錐辰备目、讀、 基)鎂化合物單離、精製。 万去將5成的雙(二烷基醯胺 201223957 製造中利魏合物及其 因此較佳為結树件鮮敎的情況多, 液的後處理等。 Μ 條件下進行反麟作或反應 法 ,可以一烧基酿胺基)鎮化合物,藉由例如CVD Z2良好的成膜的特性形成含鎮薄膜。 沈積含__方法,可以藉由周知的 或趣下法)進行,例如,可以:在常塵 -起送人域了 體) ===將該等氣體(也包含二: 在樣的補,以電漿CVD法沈積含鎂薄膜。 物氣化,铁而你為了形成薄膜必需將雙(二院基_基)鎂化合 的方法,‘例如,ί 了^^=雙(二絲醯胺細化合物氣化 將稀釋化的方法以外’也可以使用利用液體輸送用泵 可列舉:例如,己烧、環己烧、甲基環己烧' 溶液i氣基醯胺基)鎂化合物 产、、^利ϋ發明之氣二烧基酿胺基)鎂化合物沈積含鎂薄膜的 ill 9_ 4該沈積條件’例如,反應线_塵力較佳為 ira~200kPa > f >f4 * ι λώ i , λ sn Qr)n〇n在又1土马10Pa〜u〇kPa ;成膜對象物的溫度較佳為 的二佳為勘〜㈣。0 ;使雙(二烧基雜基)鎮化合物氣化 的>皿度較佳為3〇〜25(rc、更料6()〜2〇(rc。 童/μ d作為ί對於沈積含鎂__全氣體量的氧源(例如, 氣t水洛氣或醇蒸氣、或該等氣體的混合氣體)或還原性 12 201223957 氣體(例如,缝錢氣、或該魏體的混合·)的含有比例,較 佳為3〜99容量%、更佳為5〜98容量%。 I實施例】 接者,舉出貫施例具體說明本發明,然而本發明之範圍並不 限制於該等實施例。 1施例1(方法(A);雙(三級丁基曱基醯胺基)鎂(化合物(6))的 合成) 在氬裱境下,在具備攪拌裝置、溫度計、及滴液漏斗之内容 積100ml的燒瓶中添加金屬鎮5.5g(〇.23m〇i)及二乙基酿2〇ml之 後’將溴丁烧3.0g(21mmol)缓慢地滴下。接著,將二乙基崎⑽ 及溴丁烷25g(0_18mol)緩慢地滴下,一邊攪拌一邊在4〇〇c使其反 應2小時,再添加二氧陸圜55g(〇.62mol),一邊授拌一邊在4〇。〇 使其反應2小時。反應終了後’在氬環境下將反應液過濾,將濾 液在減塵之下農縮。對濃縮物一邊加熱一邊進行真空乾燥,而得 到二丁基鎂22g(單離產率;80%)。 接著,在氬環境下,在具備攪拌裝置、溫度計、及滴液漏斗 之内容積200ml的燒瓶中添加先前得到的二丁基鎂7 〇g(5〇mm〇1) 及庚烧70ml,一邊將液溫維持在25°C附近,一邊缓慢地滴下三級 丁基曱基胺lOg(O.llmol)’ 一邊攪拌一邊在^乞使其反應3小時。 反應終了後,將反應液濃縮之後,在減壓之下進行昇華(14〇。〇, 20Pa),而得到白色固體的雙(三級丁基曱基醯胺基)鎂6 4g(單離產 率;66%) 〇 此外,雙(二級丁基曱基酿胺基)鎮係顯示以下之物性値之新賴 的化合物。 h-NMRi;四氫0夫0南-d8 ’ δ(ρρπι)) ; 2.58(3H,s)、1.03(9H,s) 融點;140〜141°C。 實施例2(方法(A);雙(三級丁基乙基醯胺基)鎂(化合物(7))的 合成) 除了將實施例1中之二烷基胺改為三級丁基乙基胺 llg(O.llmol)以外,與實施例1同樣地進行了反應。其結果,得到 13 201223957 白色固體的雙(三級丁基乙基醯胺基)鎂5.8g(單離產率;52%)。 此外’雙(三級丁基乙基醯胺基)鎂係顯示以下之物性値之新颖 的化合物。 ' iH-NMR(四氫吱喃-d8,δ(ρριη));2.90(2Η,q,6.8Hz)、l.〇7(9H, s)、0.97(3H,t,6.8Hz) -(wherein R1 and R2 are synonymous with the above, and R3 and R4 represent a linear or branched alkyl group having a carbon number of 丨 to 仞. Further, R3 and R4 may be the same or different. Further, X represents a halogen. Atom.) [Method (8)] The method (A) is a method in which a dicalcium-based magnesium compound is reacted with a dialkylamine to synthesize a bis(dialkylamide)-based compound. The dialkylmagnesium compound used in the reaction (A) of the present invention is represented by the above formula. In the formula (;2), R3 and R4 represent a decyl group, an ethyl group, a n-propyl group, an isopropyl group, a n-l group, an isobutyl group, a tert-butyl group, a n-pentyl group, a tertiary pentyl group, A linear or branched alkyl group having 1 to 10 carbon atoms such as a neopentyl group or a n-decyl group. In addition, the rulers 3 and R4 may be the same or different. The dialkylmagnesium compound used in the reaction (A) of the present invention can be used as a commercially available product, and can be produced from magnesium metal by a known method. In the reaction (A) of the present invention, di(n-butyl)magnesium or n-butylethylmagnesium or the like is suitably used. The dialkylamine used in the reaction (A) of the present invention is represented by the above formula (3). In the formula (3), r1 and R2 correspond to R1 and R2 in the formula (1), respectively, and the above is synonymous. Therefore, as the dialkylamine used in the reaction (A) of the present invention, a tertiary 3-mercaptoamine, a tertiary butylethylamine, a tertiary butyl isopropylamine, Di-tertiary butylamine, secondary butyl tertiary pentylamine, di- or tertiary amylamine. 9 201223957 The above dialkylamine is used in an amount of from 1.5 to 3.0 moles, more preferably from 1.8 to 2 2 moles. Preferably, the reaction (A) of the present invention is in the presence of a solvent of the a w a ^ machine, and the antimony does not inhibit the reverse reaction. As the use, there may be mentioned, for example, diethyl _, ie, there is no particular limitation, but _ page; hexane, g-burn, cyclohexyl, methyl;: 曱2,, -, hydrocarbons, etc. An aliphatic group such as toluene or diphenylbenzene or the like may be used singly or in combination of two or more kinds. ή匕外五海4 Organic solvent can be described as relative to the two-filament magnesium b. The reaction (A) of the present invention is carried out by, for example, an amine, and an organic solvent-mixing, stirring, and compounding The reaction temperature in the case of dialkyl group is preferably _20 to 12 (rct is more square; ^ line. The reaction is particularly limited. Μ is G~(10)C 'reaction pressure is not [method (B)] • chemistry: Γ A method of using a bis-indole oxime and a bis(indenylamino)magnesium compound. However, it is possible to use lithium or the like, but it is preferably a n-butyl group. Clock, tertiary butyl group from the synthesis of di-amines, the reaction table = the use of r is poured into the formula (3) the center of the table is not a gas atom, chlorine atom, bromine atom, cesium atom and other odontogens 10 201223957 Preferably, the chlorine atom is preferably a chlorine atom. 1 mole, preferably, the amount of the second alkyl group is the L5 to 3.0 moles, more preferably 18 to ^= For the dihalogenated oxime, more than mrn^ can be enumerated: for example, diethyl ether, tetrahydrofuran,: other restrictions, however ethers; hexane, heptane, cyclohexane, acetonide, ethane, two Oxygen park a hydrocarbon, an aliphatic hydrocarbon such as toluene or xylene, or a mixed solvent such as an ethylcyclohexanone or a mixed solvent of an aliphatic hydrocarbon, or a mixture of an aliphatic hydrocarbon and an aliphatic hydrocarbon. The use of θ 卜 '§ 寻 organic solvent can be used in the above organic solvent phase 1 ~ I00g, more preferably WOge in the _ alkylamine Ig, preferably the hospital fine amine _ _ _ _ anti-base _ In the case of the dentate, it is preferred to use the amount of lg, relative to the reaction of the two inventions (9), for example, by using a sulphurylamine, a sulphur, and a succinct The guanamine group is subjected to a compound, which is coupled with a ruthenium, a ruthenium, a reaction, a fine fiber, a second coffee, and a method of: a second enthalpy connection, a second reaction, etc. The reaction temperature during the reaction is better than 1 = 2 Let 〇~50 (:, the reaction pressure is not particularly limited. ^ c, better before the reaction with the magnesium hydride, can be - 吏 醯 alkyl amide lithiation directly using the reaction liquid, and It is also possible to appropriately remove the organic solvent. Further, and/or add the amine compound which can be reacted by the reaction (A) or (b) of the present invention. After the end of the reaction, the magnesium compound is separated and refined by sublimation, recrystallization, column chromatography, etc., such as sublimation, recrystallization, column chromatography, and the like. 50% of the bis(dialkyl decylamine 201223957 is produced in the middle of the weiwei compound and thus is preferably a squid of the saplings, the liquid is post-treated, etc. 反 反 进行 反 反 反 反 反It is possible to form a smectic film by a good film forming property such as CVD Z2. The deposition method may be carried out by a known method or the like, for example, Normal dust - from the human body) === These gases (also include two: in the sample, the plasma CVD method deposits magnesium-containing film. Gasification, iron and you must combine the double (secondary base-based) magnesium in order to form a thin film, 'for example, ί ^^= double (dimethoate fine compound gasification will be diluted outside the method) It is also possible to use a pump for liquid transportation, for example, a calcined, a cyclohexane, a methylcyclohexane-solution, a solution, a gas-based sulfhydryl-based magnesium compound, and a gas-based diamine-based amine. The magnesium compound is deposited on the magnesium-containing film ill 9_ 4, the deposition condition 'for example, the reaction line _ dust force is preferably ira~200 kPa > f > f4 * ι λώ i , λ sn Qr) n〇n in another Tuma 10Pa~u〇kPa; the temperature of the film-forming object is preferably two (2). 0; the gasification of the bis(dialkyl-based) compound is preferably 3〇~25 (rc, more 6()~2〇(rc. 童/μd as ί for deposition) Magnesium__Oxygen source of total gas (for example, gas t water or alcohol vapor, or a mixed gas of such gases) or reducing 12 201223957 gas (for example, sewing money, or a mixture of the Wei body) The content ratio is preferably from 3 to 99% by volume, more preferably from 5 to 98% by volume. I. The present invention will be specifically described by way of examples, but the scope of the present invention is not limited thereto. EXAMPLES 1 Example 1 (Method (A); Synthesis of bis(tertiary butyl decyl guanidino) magnesium (compound (6))) Under a argon atmosphere, with a stirring device, a thermometer, and a drop After adding 65 g of metal town (〇23 m〇i) and 2 ml of diethyl ether to the inner tank of the liquid funnel, 3.0 g (21 mmol) of bromobutanol was slowly dropped. Then, diethyl ether was added. Saki (10) and 25 g of bromobutane (0-18 mol) were slowly dropped, and the mixture was reacted at 4 ° C for 2 hours while stirring, and then 55 g (〇.62 mol) of dioxane was added, and the mixture was stirred at 4 Torr. Make it react 2 small After the end of the reaction, the reaction solution was filtered under an argon atmosphere, and the filtrate was agglomerated under dust reduction. The concentrate was vacuum dried while heating to obtain 22 g of dibutylmagnesium (isolation yield; 80%). Next, in a argon atmosphere, a previously obtained dibutylmagnesium 7 〇g (5〇mm〇1) and a gargene 70 ml were placed in a 200 ml flask equipped with a stirrer, a thermometer, and a dropping funnel. While maintaining the liquid temperature at around 25 ° C, the tributyl decylamine 10 g (O.llmol) was slowly added dropwise while stirring for 3 hours. After the reaction was completed, the reaction solution was concentrated. Sublimation (14 Torr. 〇, 20 Pa) under reduced pressure afforded bis (tert-butyl decyl fluorinyl) magnesium 6 4 g (yield: 66%) as a white solid. The secondary butyl fluorenylamino group shows the following compounds of the new properties: h-NMRi; tetrahydro 0 funan-d8 'δ(ρρπι); 2.58(3H, s), 1.03 (9H, s) melting point; 140 to 141 ° C. Example 2 (Method (A); Synthesis of bis(tertiary butylethylguanidino) magnesium (compound (7))) except Example 1 The reaction was carried out in the same manner as in Example 1 except that the dialkylamine was changed to a tributyl butyl ethylamine (1. llmol). As a result, a bis (tertiary butylethyl hydrazine) was obtained as a white solid of 13 201223957. Amino)magnesium 5.8g (isomeric yield; 52%). Further, 'bis(tertiary butylethylguanidino)) magnesium is a novel compound which exhibits the following physical properties. 'iH-NMR(tetrahydroanthracene)喃-d8, δ(ρριη)); 2.90 (2Η, q, 6.8Hz), l.〇7(9H, s), 0.97(3H, t, 6.8Hz) -
融點;75〜78°C 實施例3(方法(B);雙(三級丁基異丙基醯胺基)鎂(化合物⑻) 的合成) 在氬環境下’在具備擾拌裝置、溫度計、及滴液漏斗之内容 積100ml的燒瓶中添加三級丁基異丙基胺i.8g(16mm〇1)及庚炫 30ml。接著’一邊將液温維持在25°C附近’一邊緩慢地滴下ι.6πιοΐ/ΐ 的正丁基裡/己烧溶液l〇ml(16mmol),一邊擾拌一邊在25。〇使其反 應2小時。反應終了後,將反應液在減壓下濃縮,而得到三級丁 基異丙基醯胺基鐘1.7g(單離產率;88%)。 接著,在具備攪拌裝置、溫度計、及滴液漏斗之内容積5〇ml 的燒瓶中添加氣化鎂0.40g(4.2mmol)及四氫π夫喃i〇mi。接著,一 邊將液溫維持在25 C附近,一邊緩慢地滴下三級丁基異丙基酿胺 基链1.0g(8.3mmol)的四氯α夫喃溶液10ml,一邊授掉一邊在25°C使 其反應8小時。反應終了後,將反應液在減壓之下濃縮之後,在 濃縮物中添加己烷20ml,在攪拌之後過濾。將濾液在減壓之下濃 縮,將濃縮物在減塵之下蒸鶴(120°C,5.7Pa),而得到淡黃色液體 的雙(三級丁基異丙基醯胺基)鎂0.53g(單離產率;5〇%)。 此外,雙(二級丁基異丙基酿胺基)鎮係顯示以下之物性値之新 穎的化合物。 b-NMR(四氫呋喃_d8,δ(ρΡιη));2·99(1Η,sept,6·6Ηζ),U4(9H, s) ’ 0.99(6Η,d,6.6Hz) 實施例4(方法(B);雙(三級丁基三級戊基醯胺基)鎂合物 (10))的合成) 在氬%境下,在具備攪拌裝置、溫度計、及滴液漏斗之内容 積100ml的燒瓶中添加三級丁基三級戊基胺Ug(8 〇mm〇1)及庚烷 14 201223957 / · 15ml ’ 一邊將液溫維持在25〇c附近,一邊緩慢地滴下i 的 正丁基經/己烷溶液5.〇ml(8.〇mm〇l),一邊攪拌一邊在25。〇使其反 應2小時。反應終了後,將反應液在減壓之下濃縮,而得到^級 丁基三級戊基醯胺基鋰Ug(單離產率;9〇%)。 接著,在具備攪拌裝置、溫度計、及滴液漏斗之内容積5〇mi 的燒瓶中添加氣化鎂〇.16g(1.7mmol)及四氫呋喃i〇m卜一邊將液 溫維持在25。(:附近,一邊缓慢地滴下三級丁基三級戊基醯胺基鋰 0,51g(3.4mm〇l)的四氫呋喃溶液1〇m卜一邊攪拌—邊二 反應8小時。反應終了後,將反應液濃縮之後,添加己烷2〇mi/,' 在攪拌之後過濾。將濾液在減壓之下濃縮,而得到淡黃色固體的 雙(二級丁基二級戊基酸胺基)鎮〇.31g(單離產率;。 一 此外,雙(三級丁基三級戊基醯胺基)鎂係顯示以下之物性 新穎的化合物。 h-NMR(四氫呋喃_d8 q,7.3Ηζ)、1.20(;18ΡΙ, s)、1.12(12Η,s)、0.85(6Η,t,7·3Ηζ) 融點;170°C以上 實施例5(沈積實驗;含鎂薄膜之製造) 利用在實施例1中得到的雙(三級丁基曱基醯胺基)鎂(化合物 ⑹)’進行藉由CVD法之沈積實驗,並對成膜的特性進行了評估。 在沈積貫驗中,使用了圖1所示之裝置。沈積條件及膜的特性係 如下所示。 (沈積條件) 鎂原料;雙(三級丁基甲基醯胺基)鎂(化合物(句) 氣化溫度;loot He載體流量;lOOsccm 氧流量;lOsccm 基板材料;Si02/Si 基板溫度;300°C 反應系統内壓力;1.33kPa 沈積時間;30分 15 201223957 (膜的特性(XPS縱深(XPS-depth)測定)) 膜厚;5Qnm以上 XPS分析;鎂氧化膜 含碳率;未檢出 含氮率;未檢出 圖1所示之裝置具有如下所述之構造。在藉由恆溫槽8保持 於一定之溫度的鎂原料容器(氣化器)7中,加熱鎂化合物使苴氣 化,其與經由質量流控制器4被導入的氦氣一起從原料容器:7、排 出。排出自原料容器7的氣體與經由質量流控制器5被導入的氦 氣一起被導入反應器9中。另一方面,也將反應氣體之氧氣經由 質量流控制器6導入反應器9中。藉由壓力計12監測反應系統内 壓力,並藉由真空泵14之前的閥的開關將反應系統内壓乂控制於 預定壓力。反應器9之中央部分具有可以藉由加熱器丨丨加^的構 導入反應器9中的鎂化合物被定位於反應器内中央部分,在 藉由加熱器11加熱至預定溫度之基板10的表面上被氧化熱分 解,而於基板10上形成含鎂薄膜。排出自反應器9的氣體經'由'收 集器(trap)13、真空泵Μ,被排出於大氣中。 、 比較例1(沈積貫驗;含鎂薄膜之製造) 利用雙(環戊二稀基)鎂,與實施例5同樣地進行藉由CVD法 之沈積貝驗’並對成膜的特性進行了評估^沈積條件及膜 係如下所示。此外,調整各種條件使原料之供給量與實 符,進行了沈積實驗。 (沈積條件)Melting point; 75~78 °C Example 3 (method (B); synthesis of bis(tertiary butyl isopropyl guanyl) magnesium (compound (8))) under argon environment with a scrambler, thermometer And a 100 ml flask of the dropping funnel was added with tributyl isopropylamine i.8 g (16 mm 〇1) and Gingxuan 30 ml. Then, while maintaining the liquid temperature at around 25 ° C, a n-butyl hexane/hexane solution (10 mmol) of ι.6 πιοΐ/ΐ was slowly dropped, while stirring was carried out at 25. 〇 Let it react for 2 hours. After the completion of the reaction, the reaction mixture was concentrated under reduced pressure to give yt. Next, 0.40 g (4.2 mmol) of vaporized magnesium and tetrahydropyrene was added to a flask equipped with a stirrer, a thermometer, and a dropping funnel of 5 〇ml. Next, while maintaining the liquid temperature at around 25 C, 10 ml of a solution of 1.0 g (8.3 mmol) of a tetrachloro-alpha valerate of a tertiary butyl isopropyl-branched amine chain was slowly dropped, and the mixture was allowed to stand at 25 ° C. It was allowed to react for 8 hours. After the completion of the reaction, the reaction solution was concentrated under reduced pressure, and then 20 ml of hexane was added to the concentrate, and the mixture was filtered. The filtrate was concentrated under reduced pressure, and the concentrate was evaporated under reduced dust (120 ° C, 5.7 Pa) to give a pale yellow liquid of bis(tri-butyl isopropyl phthalamide) magnesium 0.53 g. (single yield; 5〇%). In addition, the bis(secondary butyl isopropylamino) towns show novel compounds of the following physical properties. b-NMR (tetrahydrofuran_d8, δ(ρΡιη)); 2·99 (1Η, sept, 6·6Ηζ), U4(9H, s) '0.99 (6Η, d, 6.6Hz) Example 4 (Method (B (Synthesis of bis(tris-tert-butyltris-pentylguanidino)magnesium compound (10))) In a argon% atmosphere, in a 100 ml flask equipped with a stirring device, a thermometer, and a dropping funnel Adding tertiary butyl tertiary pentylamine Ug (8 〇mm〇1) and heptane 14 201223957 / · 15ml ' while slowly maintaining the liquid temperature around 25 〇c, slowly dropping i n-butyl group / The alkane solution was 5. 〇ml (8.〇mm〇l) and was stirred at 25 while stirring. 〇 Let it react for 2 hours. After the completion of the reaction, the reaction mixture was concentrated under reduced pressure to give <RTI ID=0.0>> Next, a glass magnesium hydride solution of 16 g (1.7 mmol) and tetrahydrofuran i〇m b was placed in a flask equipped with a stirring apparatus, a thermometer, and a dropping funnel of 5 〇mi to maintain the liquid temperature at 25. (: Near, while slowly dropping a third butyl tertiary pentyl guanidinium lithium 0,51g (3.4mm 〇l) in tetrahydrofuran solution while stirring - two reactions for 8 hours. After the reaction is over, After concentrating the reaction mixture, hexane 2 〇mi/, was added, and the mixture was filtered after stirring. The filtrate was concentrated under reduced pressure to give a pale yellow solid bis(di-butyl butyl-di- pentylamine). .31g (isolation yield;. In addition, bis (tri-butyl butyl tertiary amyl guanidino) magnesium is a novel compound exhibiting the following physical properties. h-NMR (tetrahydrofuran_d8 q, 7.3 Ηζ), 1.20 (; 18 ΡΙ, s), 1.12 (12 Η, s), 0.85 (6 Η, t, 7.3 Ηζ) melting point; 170 ° C above Example 5 (deposition experiment; manufacture of magnesium-containing film) utilized in Example 1. The obtained bis(tertiary butyl decyl guanidino) magnesium (compound (6)) was subjected to a deposition experiment by a CVD method, and the properties of the film formation were evaluated. In the deposition test, the use of Fig. 1 was used. The device shown. The deposition conditions and the characteristics of the film are as follows. (Deposition conditions) Magnesium raw material; bis(tertiary butylmethyl guanamine) magnesium (compound) Temperature; loot He carrier flow; lOOsccm oxygen flow; lOsccm substrate material; SiO2/Si substrate temperature; 300 °C reaction system pressure; 1.33 kPa deposition time; 30 minutes 15 201223957 (film characteristics (XPS depth) Measurement)) film thickness; XPS analysis of 5Qnm or more; carbon content of magnesium oxide film; no nitrogen content detected; no device shown in Fig. 1 having the structure described below, which is maintained by the constant temperature bath 8 In the magnesium raw material container (gasifier) 7 of the temperature, the magnesium compound is heated to vaporize the helium gas, and is discharged from the raw material container: 7 together with the helium gas introduced through the mass flow controller 4. The discharge from the raw material container 7 is performed. The gas is introduced into the reactor 9 together with the helium gas introduced via the mass flow controller 5. On the other hand, the oxygen of the reaction gas is also introduced into the reactor 9 via the mass flow controller 6. The reaction is monitored by a pressure gauge 12. The pressure in the system is controlled by a switch of a valve before the vacuum pump 14 to a predetermined pressure. The central portion of the reactor 9 has a magnesium which can be introduced into the reactor 9 by means of a heater. Compound The central portion of the reactor is oxidatively thermally decomposed on the surface of the substrate 10 heated to a predetermined temperature by the heater 11, and a magnesium-containing film is formed on the substrate 10. The gas discharged from the reactor 9 is collected by 'by' The trap 13 and the vacuum pump were discharged into the atmosphere. Comparative Example 1 (deposition test; production of magnesium-containing film) Using bis(cyclopentadienyl) magnesium, the same procedure as in Example 5 was carried out. The deposition of the CVD method was evaluated and the properties of the film formation were evaluated. The deposition conditions and film systems are shown below. In addition, deposition experiments were carried out by adjusting various conditions so that the amount of raw materials supplied was in accordance with the actual conditions. (deposition conditions)
鎂原料;雙(環戊二烯基)鎂 氣化溫度;30°C He載體流量;lOsccm 稀釋He流量;90sccm 氧流量;lOsccm 基板材料;Si02/Si 基板溫度;300°C 16 201223957 反應系統内壓力;lOTorr(約1.33kPa) 沈積時間;30分 (膜的特性(XPS縱深測定)) 膜厚;50nm以上 XPS分析;鎂氧化膜 含碳率;3〇%($炭原子換算) 含氮率;未檢出(原本於原料中就不存在氮原 從以上的結果確定了藉由湘本發明之“ 某 不含碳原子或氮原子—質^ 【產業上利用可能性】 丁酱:、2發明j可以提供能夠藉由簡便之方法製造含鎮薄膜之 山土上新„化合物’更具體而言,可以提供適用於藉 、—衣造含鎂薄膜的鎂化合物。又,利用該鎂化合物 ,可以 由CVD法於成膜對象物上製造含顯膜的方法。雙(二 化合物係例如’可以作為含鎂薄膜製造材料、聚合 用觸媒、醫樂或農藥等之製造補上之有用的化合物。 【圖式簡單說明】 π XΪ」係顯不於實施例中使用之用以利用雙(二烷基醯胺基)鎂 化5物衣造含鎂薄膜之沈積裝置的構造。 【主要元件符號說明】 1 载體氣體(He) 2 稀釋氣體(He) 3 反應氣體(02) 4 質量流控制器 5 質量流控制器 6 質量流控制器 7 鎂原料容器(氣化器) 17 201223957 8 恆溫槽 9 反應器 10 基板 11 反應器加熱器 12 壓力計 13 收集器 14 真空泵Magnesium raw material; bis(cyclopentadienyl)magnesium gasification temperature; 30 °C He carrier flow rate; lOsccm diluted He flow rate; 90 sccm oxygen flow rate; lOsccm substrate material; SiO 2 /Si substrate temperature; 300 ° C 16 201223957 reaction system Pressure; lOTorr (about 1.33 kPa) deposition time; 30 minutes (film characteristics (XPS depth measurement)) film thickness; XPS analysis above 50 nm; magnesium oxide film carbon content; 3 〇% ($ carbon atom conversion) nitrogen content ; not detected (originally in the raw material, there is no nitrogen source. From the above results, it was determined by the invention of "the carbon atom or nitrogen atom without a carbon atom". [Industrial use possibility] Ding sauce: 2 Invention j can provide a novel compound which can produce a film containing a film by a simple method, and more specifically, can provide a magnesium compound suitable for borrowing and coating a magnesium-containing film. Further, by using the magnesium compound, A method of producing a film containing a film can be produced by a CVD method on a film-forming object. A double compound can be used as a compound for producing a magnesium-containing film, a catalyst for polymerization, a medical or a pesticide, and the like. [Simple description of the diagram] π XΪ” is a structure which is not used in the embodiment to form a deposition apparatus containing a magnesium thin film by using a bis(dialkylguanidino)magnesium 5 coating. [Main component symbol description] 1 carrier gas ( He) 2 Dilution gas (He) 3 Reaction gas (02) 4 Mass flow controller 5 Mass flow controller 6 Mass flow controller 7 Magnesium raw material container (gasifier) 17 201223957 8 Constant temperature tank 9 Reactor 10 Substrate 11 Reaction Heater 12 pressure gauge 13 collector 14 vacuum pump
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