CN110546210A - 包括乙硅烷基胺化合物的含硅薄膜沉积组合物以及用其制备含硅薄膜的方法 - Google Patents
包括乙硅烷基胺化合物的含硅薄膜沉积组合物以及用其制备含硅薄膜的方法 Download PDFInfo
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- CN110546210A CN110546210A CN201880025614.1A CN201880025614A CN110546210A CN 110546210 A CN110546210 A CN 110546210A CN 201880025614 A CN201880025614 A CN 201880025614A CN 110546210 A CN110546210 A CN 110546210A
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- silicon
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 92
- 239000010703 silicon Substances 0.000 title claims abstract description 91
- 239000000203 mixture Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims description 23
- 230000008021 deposition Effects 0.000 title abstract description 13
- 150000001875 compounds Chemical class 0.000 title description 40
- 238000004519 manufacturing process Methods 0.000 claims abstract description 28
- -1 amine compound Chemical class 0.000 claims abstract description 23
- 239000010408 film Substances 0.000 claims description 68
- 239000000126 substance Substances 0.000 claims description 61
- 238000000151 deposition Methods 0.000 claims description 47
- 239000001257 hydrogen Substances 0.000 claims description 40
- 229910052739 hydrogen Inorganic materials 0.000 claims description 40
- 239000010409 thin film Substances 0.000 claims description 39
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 20
- 125000003342 alkenyl group Chemical group 0.000 claims description 16
- 229910052701 rubidium Inorganic materials 0.000 claims description 16
- 238000000231 atomic layer deposition Methods 0.000 claims description 15
- 125000006701 (C1-C7) alkyl group Chemical group 0.000 claims description 13
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 10
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 10
- 239000012495 reaction gas Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 8
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 7
- 150000002431 hydrogen Chemical group 0.000 claims description 7
- 238000004518 low pressure chemical vapour deposition Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 125000006726 (C1-C5) alkenyl group Chemical group 0.000 claims description 5
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 5
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 5
- 239000001272 nitrous oxide Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 4
- 229930195735 unsaturated hydrocarbon Natural products 0.000 claims description 4
- 125000006729 (C2-C5) alkenyl group Chemical group 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 150000004985 diamines Chemical class 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 claims 3
- 229910044991 metal oxide Inorganic materials 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 230000009257 reactivity Effects 0.000 abstract description 9
- 239000012686 silicon precursor Substances 0.000 abstract description 7
- 125000000217 alkyl group Chemical group 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000002243 precursor Substances 0.000 description 11
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- 125000004433 nitrogen atom Chemical group N* 0.000 description 6
- 230000004913 activation Effects 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000012280 lithium aluminium hydride Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- 229910005091 Si3N Inorganic materials 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009530 blood pressure measurement Methods 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OWKFQWAGPHVFRF-UHFFFAOYSA-N n-(diethylaminosilyl)-n-ethylethanamine Chemical compound CCN(CC)[SiH2]N(CC)CC OWKFQWAGPHVFRF-UHFFFAOYSA-N 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 125000006592 (C2-C3) alkenyl group Chemical group 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- LVQCDXDMYGLLOX-UHFFFAOYSA-N CC(C)C.C(COCCOCCOCCO)O Chemical compound CC(C)C.C(COCCOCCOCCO)O LVQCDXDMYGLLOX-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910005540 GaP Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- BIVNKSDKIFWKFA-UHFFFAOYSA-N N-propan-2-yl-N-silylpropan-2-amine Chemical compound CC(C)N([SiH3])C(C)C BIVNKSDKIFWKFA-UHFFFAOYSA-N 0.000 description 1
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910003811 SiGeC Inorganic materials 0.000 description 1
- 229910003818 SiH2Cl2 Inorganic materials 0.000 description 1
- 229910003828 SiH3 Inorganic materials 0.000 description 1
- 229910000577 Silicon-germanium Inorganic materials 0.000 description 1
- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 description 1
- XMIJDTGORVPYLW-UHFFFAOYSA-N [SiH2] Chemical compound [SiH2] XMIJDTGORVPYLW-UHFFFAOYSA-N 0.000 description 1
- VOSJXMPCFODQAR-UHFFFAOYSA-N ac1l3fa4 Chemical compound [SiH3]N([SiH3])[SiH3] VOSJXMPCFODQAR-UHFFFAOYSA-N 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- YEPRSAYQHDAYGU-UHFFFAOYSA-N difluoro-methyl-trifluorosilylsilane Chemical compound C[Si](F)(F)[Si](F)(F)F YEPRSAYQHDAYGU-UHFFFAOYSA-N 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229920002457 flexible plastic Polymers 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 125000001339 silanediyl group Chemical group [H][Si]([H])(*)* 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- OLRJXMHANKMLTD-UHFFFAOYSA-N silyl Chemical compound [SiH3] OLRJXMHANKMLTD-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PPDADIYYMSXQJK-UHFFFAOYSA-N trichlorosilicon Chemical compound Cl[Si](Cl)Cl PPDADIYYMSXQJK-UHFFFAOYSA-N 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N 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
- C23C16/24—Deposition of silicon only
-
- 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]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45536—Use of plasma, radiation or electromagnetic fields
-
- 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
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Abstract
本发明涉及包括乙硅烷基胺化合物的含硅薄膜沉积组合物以及使用该组合物制造含硅薄膜的方法。本发明的含硅薄膜沉积组合物能借助包括作为硅前体的乙硅烷基胺化合物来制备高质量含硅薄膜,该乙硅烷基胺化合物显示出优异的反应性、热稳定性和高挥发性。
Description
技术领域
本发明涉及包括乙硅烷基胺化合物的用于沉积含硅薄膜的组合物以及使用该组合物制造含硅薄膜的方法。
背景技术
通过半导体领域中的各种沉积工艺制造成各种薄膜形式的含硅薄膜,诸如硅膜(silicon)、氧化硅膜(silicon oxide)、氮化硅膜(silicon nitride)、碳氮化硅膜(Silicon carbonitride)和氧氮化硅膜(Silicon oxynitride)等,并且其广泛应用于许多领域。特别是,由于氧化硅膜和氮化硅膜具有非常优良的阻挡性和抗氧化性,所以它们在制造装置中用作绝缘膜、扩散阻挡层、硬掩模、蚀刻停止层、种子层、间隔物、沟槽隔离、金属间介电材料和保护膜层。近来,多晶硅薄膜用于薄膜晶体管(TFT,thin film transistor)、太阳能电池等,其应用领域逐渐多样化。
作为已知用于制造本领域的含硅薄膜的代表性技术,存在使混合气体型硅前体和反应气体反应以在基底的表面上形成膜或通过在基底表面上直接反应以形成膜的金属有机化学气相沉积(MOCVD),以及通过在基底表面上物理或化学吸附气体型硅前体并且相继投入反应气体以形成膜的原子层沉积(ALD),用于制造薄膜的各种技术,诸如低压化学气相沉积(LPCVD)、使用能够在低温下沉积的等离子体的等离子体增强化学气相沉积(PECVD)、等离子体增强原子层沉积(PEALD)等,应用于制造下一代半导体和显示装置的工艺,从而用于形成超精细图案并在沉积具有均匀和优异性质的纳米级厚度的超薄膜。
作为用于形成含硅薄膜的代表性前体,可列出硅烷、硅烷氯化物、氨基硅烷和烷氧基硅烷形式的化合物,并且通常需要的前体特性如下:
①常温及常压下为液体形式的化合物,以及具有优异挥发性的化合物;
②具有高热稳定性和低活化能以具有优异的反应性的化合物;
③在薄膜形成过程中不产生非挥发性副产物的化合物;以及
④易于处理、运输和储存的化合物。
目前,各种文献中已经报道了使用诸如二氯硅烷(dichlorosilane:SiH2Cl2)和六氯乙硅烷(hexachlorodisilane:Cl3SiSiCl3)等的硅烷氯化物以及诸如三甲硅烷基胺(trisilylamine:N(SiH3)3)、双-二乙基氨基硅烷(bis-diethylaminosilane:H2Si(N(CH2CH3)2)2)和二异丙基氨基硅烷(di-isopropylaminosilane:H3SiN(i-C3H7)2)等的氨基硅烷形式的化合物等进行含硅薄膜沉积的研究,并且该前体用于大规模生产半导体和显示器。然而,根据器件的超高集成度引起的器件小型化、纵横比的增加和器件材料的多样化,已经要求在所需的低温下形成具有均匀和薄的厚度和优异的电性能的超细薄膜的技术,因此,在使用现有硅前体时,在600℃或更高温度下的高温工艺、台阶覆盖率、蚀刻性质和薄膜的物理和电学性质方面正在出现问题。
然而,即使在器件中在所需的低温下形成具有均匀和薄的厚度和优异的电性能的超细薄膜情况下,由于薄膜形成速度低,生产率也成问题,因此,需要开发具有改进性能的新型硅前体。
发明内容
技术问题
本发明提供一种用于沉积含硅薄膜的组合物,该组合物包含作为硅前体的具有高热稳定性和优异反应性从而在低温下具有优异的内聚力的乙硅烷基胺化合物。
此外,本发明提供一种制造含硅薄膜的方法,该方法使用根据本发明一实施例的用于沉积含硅薄膜的组合物,能够形成具有优异物理和电学性质诸如高沉积速率、优异的台阶覆盖率等的含硅薄膜。
解决问题的方案
本发明提供一种用于沉积含硅薄膜的组合物,包括具有低活化能以具有优异的反应性、热稳定性和具有优异的挥发性,因此非常适合用作沉积薄膜的前体的乙硅烷基胺化合物,并且,本发明的用于沉积含硅薄膜的组合物中包含的乙硅烷基胺化合物由下列化学式1表示:
[化学式1]
(所述化学式1中,
Ra、Rb和R1至R9各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基,条件是Ra和Rb不同时为氢。)
优选地,在根据本发明一实施例的所述化学式1中,Ra和Rb可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基,条件是Ra和Rb不同时为氢;R1至R3可以是氢;R4至R9可各自独立地为氢、(C1-C5)烷基或(C1-C5)烯基。
优选地,本发明的所述化学式1可以由以下化学式2表示:
[化学式2]
(所述化学式2中,R为(C1-C7)烷基,R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基。)
就沉积具有更好纯度和耐久性的薄膜而言,优选在根据本发明一实施例的所述化学式2中,R11至R14可各自独立地为氢或(C1-C5)烷基。
具体地,本发明的所述化学式1的乙硅烷基胺化合物可选自以下化合物,但不限于此:
另外,本发明提供一种制造含硅薄膜的方法,使用本发明的用于沉积含硅薄膜的组合物。
本发明的制造含硅薄膜的方法可以通过原子层沉积(ALD)、化学气相沉积(CVD)、金属有机化学气相沉积(MOCVD)、低压化学气相沉积(LPCVD)、等离子体增强化学气相沉积(PECVD)或等离子体增强原子层沉积(PEALD)进行。
本发明的制造含硅薄膜的方法具体可以包括以下步骤:
a)将安装在腔室中的基底的温度保持在30至400℃;
b)注入载气和权利要求1所述的用于沉积含硅薄膜的组合物;以及
c)注入反应气体以在所述基底上沉积含硅薄膜。
根据本发明一实施例的反应气体可以是选自以下组成的组中的任何一种、两种或更多种:氧气(O2)、臭氧(O3)、蒸馏水(H2O)、过氧化氢(H2O2)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、氨气(NH3)、氮气(N2)、肼(N2H4)、胺、二胺、一氧化碳(CO)、二氧化碳(CO2)、C1至C12饱和或不饱和烃、氢气、氩气和氦气。
本发明的效果
本发明的用于沉积含硅薄膜的组合物包含作为沉积含硅薄膜前体的乙硅烷基胺化合物,该化合物具有低活化能,以具有优异的反应性,优异的热稳定性和高挥发性,从而能够制造具有优异物理和电学性质,诸如高沉积速率和优异的台阶覆盖率以及优异的纯度和耐久性的薄膜。
此外,本发明的用于沉积含硅薄膜的组合物中包含的乙硅烷基胺化合物在室温或能够处理的压力下以液态存在,从而易于处理,因此,更容易制造含硅薄膜。
另外,根据本发明的含硅薄膜的制造方法,可以使用包含乙硅烷基胺化合物的用于沉积的含硅薄膜的组合物来制造含硅薄膜,该乙硅烷基胺化合物具有高热稳定性和优异的反应性,从而允许制造具有高硅含量和优异热稳定性、耐久性和高质量的含硅薄膜。
附图说明
图1是实施例1中制备的双二甲基甲硅烷基甲基乙硅烷基胺的蒸气压测量图。
具体实施方式
在下文中,将详细描述本发明的乙硅烷基胺化合物、其制备方法和含有乙硅烷基胺化合物的用于沉积含硅薄膜的组合物。
本文所述的“烷基”是指具有1至7个,优选1至5个,更优选1至3个碳原子的直链、支链和环状、饱和和不饱和的烃,并且例如包括甲基、乙基、丙基、异丙基、丁基、异丁基、戊基等。
本文所述的“卤素”是指卤素族元素,包括例如氟、氯、溴和碘。
本文所述的术语“烯基”单独或作为另一基团的一部分是指具有2-7个碳原子和一个或多个碳碳双键的直链、支链或环状烃基。更优选的烯基是具有2至5个碳原子的低级烯基。最优选的低级烯基是具有2至约3个碳原子的基。另外,烯基可以在任何可用的附连点被取代。烯基的实例包括乙烯基、丙烯基、烯丙基、丁烯基和4-甲基丁烯基。术语“烯基”和“低级烯基”包括为顺式和反式取向的基,或者替代地,具有E和Z取向的基。
本发明提供用于沉积含硅薄膜的组合物,组合物包含由以下化学式1表示的乙硅烷基胺化合物,该化合物作为沉积薄膜的前体具有优异的反应性和热稳定性,同时,在室温下主要以液体形式存在,从而易于处理:
[化学式1]
在所述化学式1中,
Ra、Rb和R1至R9各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基,条件是Ra和Rb不同时为氢。
用于沉积本发明的含硅薄膜的组合物中包含的乙硅烷基胺化合物具有另外提供给分子中的硅原子的未共用的氮原子电子对,从而增加了硅和氮原子的结合能,并且具有低活化能,具有三角平面Si3N分子结构形式,其中三个硅原子与氮原子键合,从而具有优异的反应性和优异的热稳定性,因此,作为含硅薄膜前体非常有用。
此外,本发明的乙硅烷基胺化合物是在常温常压下主要为液体形式的化合物,其具有优异的挥发性和分子中高含量的硅原子,因此,包含该化合物的用于沉积含硅薄膜的组合物可以以高沉积速率制造高质量的含硅薄膜。
优选地,在本发明的所述化学式1中,Ra和Rb可各自独立地为氢、(C1-C5)烷基或(C2-C5)烯基,条件是Ra和Rb不同时为氢;R1至R3可以为氢;R4至R9可各自独立地为氢、(C1-C5)烷基或(C1-C5)烯基,更优选地Ra和Rb各自独立地为氢或(C1-C5)烷基,条件是Ra和Rb不同时为氢;R1至R3可以为氢;R4至R9可各自独立地为氢、(C1-C5)烷基或(C1-C5)烯基。
更优选地,本发明的所述化学式1可以由以下化学式2表示:
[化学式2]
(在所述化学式2中,R为(C1-C7)烷基,R11至R14各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基。)
由上述化学式2表示的乙硅烷基胺化合物是包含在本发明的用于沉积含硅薄膜的组合物中的硅前体,其具有另外提供给分子中的硅原子的未共用的氮原子电子对,使得硅和氮原子的结合能增加,具有三角平面Si3N分子结构形式,其中三个硅原子键合到氮原子上,并且还具有通过具有两个硅而具有电子敏感性的Si2分子结构形式,其包括与其结合的三个具有阳离子性质的氢从而降低活化能以具有更好的反应性,因此,可以以高沉积速率容易地沉积含硅薄膜。
此外,热稳定性优异,因此,可以制造具有高耐久性和优异纯度的薄膜。
就制造更好的含硅薄膜而言,更优选地在所述化学式2中,R11至R14可各自独立地为氢或(C1-C5)烷基,更优选地R为(C1-C3)烷基,并且R11至R14可各自独立地为氢、(C1-C3)烷基或(C2-C3)烯基。
根据本发明一实施例的化学式1可由以下化学式1-1或1-2表示:
[化学式1-1]
[化学式1-2]
(在所述化学式1-1和1-2中,
Ra和Rb各自独立地为(C1-C7)烷基;R21和R22各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基。)
具体地,本发明的所述化学式1的乙硅烷基胺化合物可选自以下化合物,但不限于此:
此外,本发明提供包含在本发明的用于沉积含硅薄膜的组合物中的上述化学式1的化合物。
优选地,在本发明的所述化学式1中,Ra和Rb可各自独立地为氢或(C1-C7)烷基,条件是Ra和Rb不同时为氢;R1至R3可以是氢;R4至R9可各自独立地为氢、(C1-C5)烷基或(C1-C5)烯基,更优选地化学式1可由上述化学式2表示。
优选地,在根据本发明一实施例的所述化学式2中,R11至R14可各自独立地为氢或(C1-C5)烷基。
根据本发明一实施例的所述化学式1的乙硅烷基胺化合物可选自以下化合物,但不限于此。
此外,作为制备根据本发明一实施例的化学式1的化合物的方法,任何方法都是可能的,只要其在本领域技术人员的认知范围内,然而,作为具体实例,该方法包括:
使下述化学式3的化合物与下述化学式4的化合物在碱的存在下反应以制备化学式5的化合物;以及
在还原剂存在下还原下列化学式5的化合物,以制备以下化学式1的乙硅烷基胺化合物,从而能够制备以下化学式1的乙硅烷基胺化合物:
[化学式1]
[化学式3]
[化学式4]
[化学式5]
(在化学式1和化学式3至5中,Ra、Rb和R1至R9各自独立地为氢、(C1-C7)烷基或(C2-C7)烯基,条件是Ra和Rb不同时为氢;以及
X1至X4各自独立地为卤素。)
作为本发明的乙硅烷基胺化合物的制备方法的一实施例的碱,任何碱都是可能的,只要其在本发明所属领域的技术人员的认知范围内即可,然而碱可以优选为三(C1-C5)烷基胺或吡啶,特别是三甲胺、三乙胺、吡啶等,碱与所述化学式4的化合物的摩尔比可以在1:1至1:2、1:1至1:1.5的范围内,以快速完成反应,并且更优选为1:1.25。
根据本发明的乙硅烷基胺化合物的制备方法的一实施例的还原剂没有限制,但可以优选LiAlH4、NaBH4或MH(其中M是碱金属),并且所述碱金属可以是Li、Na或K。
本发明的还原剂可以与所述化学式5的化合物的摩尔比为1:1.25至1:6,优选1:1.25至1:5.5使用,所述化学式3的化合物可以相对于1摩尔所述化学式2的化合物为1至2摩尔的比例使用。
作为本发明的制备方法中使用的溶剂,任何常用的有机溶剂都是可以的,但是,优选使用选自己烷、戊烷、二氯甲烷(DCM)、二氯乙烷(DCE)、甲苯(Toluene)、乙腈(MeCN)、硝基甲烷(Nitromethane)、四氢呋喃(THF)、N,N-二甲基甲酰胺(DMF)、四乙二醇二甲基乙烷和N,N-二甲基乙酰胺(DMA)、聚醚(二乙二醇二甲醚(Diglyme)、三乙二醇二甲醚(Triglyme)和/或四乙二醇二甲醚(Tetraglyme))组成的组中的一种或多种。
反应温度可以是常规有机合成中使用的温度,但是根据反应物质和起始原料的量而变化,并且在通过NMR等确认原料完全消耗后完成反应。当反应完成时,在萃取过程后在减压下蒸馏溶剂,然后可以通过典型的方法诸如柱色谱法分离和纯化所需的物质。
此外,本发明提供用于沉积含硅薄膜的组合物,该组合物包含本发明的乙硅烷基胺化合物。
本发明的用于沉积含硅薄膜的组合物必须包括由所述化学式1表示的乙硅烷基胺化合物作为前体,但可包括一种或多种乙硅烷基胺化合物,以及,考虑到薄膜的成膜条件或厚度、性质等,用于沉积含硅薄膜的组合物中乙硅烷基胺化合物的含量可以在本领域技术人员的认识范围内。
此外,本发明提供一种使用本发明的用于沉积含硅薄膜的组合物制造含硅薄膜的方法。
根据本发明一实施例的制造含硅薄膜的方法,使用本发明的用于沉积含硅薄膜的组合物来制备薄膜,该组合物包含由上述化学式1表示的乙硅烷基胺化合物,其作为前体在常温下为液体,具有高挥发性和优异的热稳定性,从而易于处理前体,可制造多种薄膜,并制造具有高硅含量的高纯度薄膜,具有高沉积速率和优异的台阶覆盖率。
作为制造本发明的含硅薄膜的方法,任何方法都是可以的,只要它在本领域技术人员的认知范围内,然而,它可以优选地通过原子层沉积(ALD)、化学气相沉积(CVD)、金属有机化学气相沉积(MOCVD)、低压化学气相沉积(LPCVD)、等离子体增强化学气相沉积(PECVD)或等离子体增强原子层沉积(PEALD)、更优选等离子体增强原子层沉积(PEALD)或等离子体增强化学气相沉积(PECVD)来进行。
本发明的制造含硅薄膜的方法具体可以包括以下步骤:
a)将安装在腔室中的基底的温度保持在30至400℃;
b)注入载气和根据本发明一实施例的用于沉积含硅薄膜的组合物;以及
c)注入反应气体以在所述基底上沉积含硅薄膜。
优选地,当根据本发明一实施例通过等离子体增强原子层沉积(PEALD)或等离子体增强化学气相沉积(PECVD)沉积含硅薄膜时,可以在a)步骤之后还包括产生等离子体的步骤,以及
b)步骤的用于沉积含硅薄膜的组合物可以与载气一起注入。
在根据本发明一实施例的制造含硅薄膜的方法中,可以根据所需薄膜的结构或热性质来调节沉积条件。作为根据本发明一实施例的沉积条件,实例有含有乙硅烷基胺化合物的用于沉积含硅薄膜的组合物的输入流速,反应气体和载气的输入流速、压力、RF功率、基底温度等,并且作为沉积条件的非限制性实例,可以如下调整条件:用于沉积含硅薄膜的组合物的输入流速为10至1000cc/min,载气流速为10-1000cc/min,反应气体流速为1至1000cc/min,压力为0.5至10托,RF功率为200至1000W,基底温度为30至400℃,但不限于此。
本发明的制造含硅薄膜的方法可以使用包含根据本发明一实施例的乙硅烷基胺化合物作为前体的用于沉积含硅薄膜的组合物,从而在低基底温度30至200℃下,或甚至在30至100℃的较低温度下形成薄膜,这是非常经济的,并且非常有利于商业应用。
用于制造本发明的含硅薄膜的方法中的反应气体不受限制,然而,可以是选自以下组成的组中的一种或两种或更多种:氧气(O2)、臭氧(O3)、蒸馏水(H2O)、过氧化氢(H2O2)、一氧化氮(NO)、氧化亚氮(N2O)、二氧化氮(NO2)、氨气(NH3)、氮气(N2)、肼(N2H4)、胺、二胺、一氧化碳(CO)、二氧化碳(CO2)、C1-C12饱和或不饱和烃、氢气、氩气和氦气、载气可以是选自氩气、氦气和氮气中的一种或两种或更多种。
在根据本发明一实施例的制造含硅薄膜的方法中使用的基底可以是包括Si、Ge、SiGe、GaP、GaAs、SiC、SiGeC、InAs和InP中的一种或多种半导体材料的基底;SOI(绝缘体上硅)基底;石英基底;或用于显示器的玻璃基底;聚酰亚胺、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚醚砜(PES)和聚酯的柔性塑料基底;但不限于此。
所述含硅薄膜可以直接形成在所述基底上,但是另外,可以在所述基底和所述含硅薄膜之间形成多个导电层、介电层、绝缘层等。
在下文中,将通过以下实施例详细描述本发明。在此之前,本说明书和权利要求中使用的术语和词语不应被解释为一般或词典含义,而应被理解满足本发明的技术构思的含义和概念,这是基于发明人可适当限定术语的概念以便以最佳方式描述他们自己的发明的原则。
因此,这里描述的实施例和附图中示出的配置仅仅是本发明的最优选一实施例,而不代表本发明的所有技术构思,因此,应该理解,在提交本申请时,存在可替换它们的各种等同物和修改的实例。
另外,以下所有实施例均通过已知的等离子体增强原子层沉积(PEALD)使用200mm单晶片型(single wafer type)ALD设备(CN1,Atomic Premium)以常用的淋浴头模式进行。另外,可以通过已知等离子体增强化学气相沉积(PECVD)使用200mm单晶片型(singlewafer type)CVD设备(CN1,Atomic Premium)以常用的淋浴头模式来进行。
通过椭偏仪(Ellipsometer,M2000D,Woollam)和透射电子显微镜(TransmissionElectron Microscope)测量沉积的含硅薄膜的厚度,并使用红外光谱(InfraredSpectroscopy,IFS66V/S&Hyperion 3000,Bruker Optiks)、X射线光电子能谱(X-rayphotoelectron spectroscopy)和二次离子质谱仪(SIMS,Secondary Ion MassSpectrometer)分析其组成。
[实施例1]双二甲基甲硅烷基甲基乙硅烷基胺的制备
步骤1:双二甲基甲硅烷基四氯甲基乙硅烷基胺的制备
向无水气氛和惰性气氛下干燥的5L SUS反应器中,加入2000g(8.05mol)甲基五氯乙硅烷(Si2Cl5CH3)和1500mL作为有机溶剂的正戊烷,并且在搅拌下缓慢加入752.7g(8.05mol)三乙胺((CH3CH2)3N),同时保持温度在-20℃。加完后,再缓慢加入1073g(8.05mol)四甲基二硅氮烷((((CH3)2)SiH)2NH),同时保持温度在-20℃。将添加完成后的反应溶液缓慢加热至常温,搅拌6小时,同时保持温度在25℃。反应完成后过滤反应混合物,除去过滤产生的白色固体,得到滤液,减压下除去溶剂,从而得到2501g(7.24mol)双二甲基甲硅烷基四氯甲基乙硅烷基胺(((CH3)2)SiH)2NSi(Cl)2SiCl2CH3),收率90%。
1H NMR(in CDCl3):δ0.14(d,12H,(((CH3)2)SiH)2NSi(Cl)2SiCl2CH3),δ4.60(m,2H,(((CH3)2)SiH)2NSi(Cl)2SiCl2CH3),δ0.19(s,3H(((CH3)2)Si H)2NSi(Cl)2SiCl2CH3)
步骤2:双二甲基甲硅烷基甲基乙硅烷基胺的制备
向在无水气氛和惰性气氛下干燥的20L SUS反应器中,加入2000ml作为有机溶剂的四乙二醇二甲醚(TEGDME),并在搅拌下缓慢加入379g(9.99mol)氢化铝锂(LiAlH4),同时保持温度为-10℃。加完后,向其中缓慢加入2501g(7.24mol)双二甲基甲硅烷基四氯甲基乙硅烷基胺((((CH3)2)SiH)2NSi(Cl)2SiCl2CH3),同时保持温度在-10℃。加完后,将反应溶液搅拌20小时,同时保持温度在-10℃。反应完成后过滤反应混合物,除去过滤产生的白色固体,得到滤液,减压下除去溶剂,进行真空蒸馏,得到752g(3.62mol)双二甲基甲硅烷基甲基乙硅烷基胺(((CH3)2)SiH)2NSi(H)2SiH2CH3),产率50%。
1H NMR(in CDCl3):δ0.14(d,12H,(((CH3)2)SiH)2NSi(H)2SiH2CH3),δ4.76(m,2H,(((CH3)2)SiH)2NSi(H)2SiH2CH3),δ4.60(m,2H(((CH3)2)SiH)2NSi(H) 2SiH2CH3),δ3.80(m,2H(((CH3)2)SiH)2NSi(H)2SiH2 CH3),δ0.26(m,3H(((CH3)2)SiH)2NSi(H)2SiH2 CH3 )
图1中示出了实施例1中制备的双二甲基甲硅烷基甲基乙硅烷基胺的蒸气压力测量的图。从图1中可以看出使用含有本发明的乙硅烷基胺化合物的用于沉积含硅薄膜的组合物,可以容易地沉积薄膜。
Claims (9)
1.一种用于沉积含硅薄膜的组合物,包括由以下化学式1表示的乙硅烷基胺化合物:
[化学式1]
所述化学式1中,
Ra、Rb和R1至R9各自独立地为氢、C1-C7烷基或C2-C7烯基,条件是Ra和Rb不同时为氢。
2.根据权利要求1所述的用于沉积含硅薄膜的组合物,其中,
在所述化学式1中,
Ra和Rb各自独立地为氢、C1-C5烷基或C2-C5烯基,条件是Ra和Rb不同时为氢;
R1至R3为氢;
R4至R9各自独立地为氢、C1-C5烷基或C1-C5烯基。
3.根据权利要求1所述的用于沉积含硅薄膜的组合物,其中,
所述化学式1由以下化学式2表示:
[化学式2]
所述化学式2中,R为C1-C7烷基,R11至R14各自独立地为氢、C1-C7烷基或C2-C7烯基。
4.根据权利要求3所述的用于沉积含硅薄膜的组合物,其中,
在所述化学式2中,R11至R14各自独立地为氢或C1-C5烷基。
5.根据权利要求1所述的用于沉积含硅薄膜的组合物,其中,
所述化学式1的乙硅烷基胺化合物选自由以下化合物组成的组:
6.一种使用根据权利要求1至5中任一项所述的用于沉积含硅薄膜的组合物的含硅薄膜的制造方法。
7.根据权利要求6所述的含硅薄膜的制造方法,其中,
所述制造方法通过原子层沉积、化学气相沉积、金属有机化学气相沉积、低压化学气相沉积、等离子体增强化学气相沉积或等离子体增强原子层沉积来执行。
8.根据权利要求6所述的含硅薄膜的制造方法,包括以下步骤:
a)将安装在腔室中的基底的温度保持在30至400℃;
b)注入载气和权利要求1所述的用于沉积含硅薄膜的组合物;以及
c)注入反应气体以在所述基底上沉积所述含硅薄膜。
9.根据权利要求8所述的含硅薄膜的制造方法,其中,
所述反应气体是选自以下组成的组的任何一种或两种或多种:氧气、臭氧、蒸馏水、过氧化氢、一氧化氮、氧化亚氮、二氧化氮、氨、氮气、肼、胺、二胺、一氧化碳、二氧化碳、C1至C12饱和或不饱和烃、氢气、氩气和氦气。
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