JP7320544B2 - Si含有膜形成組成物およびその使用方法 - Google Patents
Si含有膜形成組成物およびその使用方法 Download PDFInfo
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- JP7320544B2 JP7320544B2 JP2021006237A JP2021006237A JP7320544B2 JP 7320544 B2 JP7320544 B2 JP 7320544B2 JP 2021006237 A JP2021006237 A JP 2021006237A JP 2021006237 A JP2021006237 A JP 2021006237A JP 7320544 B2 JP7320544 B2 JP 7320544B2
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- 239000000203 mixture Substances 0.000 title claims description 192
- 238000000034 method Methods 0.000 title claims description 81
- 239000002243 precursor Substances 0.000 claims description 191
- 239000000758 substrate Substances 0.000 claims description 63
- 230000008569 process Effects 0.000 claims description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 47
- 229910052710 silicon Inorganic materials 0.000 claims description 47
- 239000010703 silicon Substances 0.000 claims description 43
- 238000000151 deposition Methods 0.000 claims description 39
- 239000000376 reactant Substances 0.000 claims description 39
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 37
- 238000010926 purge Methods 0.000 claims description 23
- 229920006395 saturated elastomer Polymers 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 125000003277 amino group Chemical group 0.000 claims description 17
- 235000012431 wafers Nutrition 0.000 claims description 16
- 150000001412 amines Chemical class 0.000 claims description 11
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 11
- JCXJVPUVTGWSNB-UHFFFAOYSA-N Nitrogen dioxide Chemical compound O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 10
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
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- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 5
- 125000000623 heterocyclic group Chemical group 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 3
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 2
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- 125000004888 n-propyl amino group Chemical group [H]N(*)C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 125000004430 oxygen atom Chemical group O* 0.000 claims 1
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 33
- 229910003828 SiH3 Inorganic materials 0.000 description 29
- OLRJXMHANKMLTD-UHFFFAOYSA-N silyl Chemical compound [SiH3] OLRJXMHANKMLTD-UHFFFAOYSA-N 0.000 description 29
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- -1 mono-substituted trisilylamine Chemical class 0.000 description 26
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 24
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- 238000005229 chemical vapour deposition Methods 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 21
- 239000002184 metal Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 18
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- 229910052757 nitrogen Inorganic materials 0.000 description 17
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 150000003254 radicals Chemical class 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 14
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 12
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- 239000004065 semiconductor Substances 0.000 description 12
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- 229910052799 carbon Inorganic materials 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000003708 ampul Substances 0.000 description 10
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- 125000005843 halogen group Chemical group 0.000 description 10
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- 238000005137 deposition process Methods 0.000 description 9
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- 238000004519 manufacturing process Methods 0.000 description 9
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- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Natural products C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 9
- 229910052718 tin Inorganic materials 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 8
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 8
- 229910052698 phosphorus Inorganic materials 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 239000010936 titanium Substances 0.000 description 8
- 239000012808 vapor phase Substances 0.000 description 8
- 229910052787 antimony Inorganic materials 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 7
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 125000004178 (C1-C4) alkyl group Chemical group 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 6
- 238000000137 annealing Methods 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- 239000012043 crude product Substances 0.000 description 6
- VEYJKODKHGEDMC-UHFFFAOYSA-N dichloro(trichlorosilyl)silicon Chemical compound Cl[Si](Cl)[Si](Cl)(Cl)Cl VEYJKODKHGEDMC-UHFFFAOYSA-N 0.000 description 6
- 229910052735 hafnium Inorganic materials 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910052723 transition metal Inorganic materials 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 5
- 229910052797 bismuth Inorganic materials 0.000 description 5
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- 229910052681 coesite Inorganic materials 0.000 description 5
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- 238000004821 distillation Methods 0.000 description 5
- 230000006870 function Effects 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 5
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- 125000001261 isocyanato group Chemical group *N=C=O 0.000 description 5
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 5
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
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- XAXYLKQEHXPTGZ-UHFFFAOYSA-N Cl[SiH2]N([SiH3])[SiH3] Chemical compound Cl[SiH2]N([SiH3])[SiH3] XAXYLKQEHXPTGZ-UHFFFAOYSA-N 0.000 description 4
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- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 4
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- 229910004298 SiO 2 Inorganic materials 0.000 description 4
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- 239000002585 base Substances 0.000 description 4
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- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 description 2
- JFWLFXVBLPDVDZ-UHFFFAOYSA-N [Ru]=O.[Sr] Chemical compound [Ru]=O.[Sr] JFWLFXVBLPDVDZ-UHFFFAOYSA-N 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
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 2
- FXOCTISBMXDWGP-UHFFFAOYSA-N dichloro(silyl)silane Chemical compound [SiH3][SiH](Cl)Cl FXOCTISBMXDWGP-UHFFFAOYSA-N 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
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- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
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- 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
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- 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
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- 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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/308—Oxynitrides
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
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- 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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
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- 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]
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- 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
- C23C16/50—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 using electric discharges
- C23C16/515—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 using electric discharges using pulsed discharges
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- 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
- H01L21/02205—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 the layer being characterised by the precursor material for deposition
- H01L21/02208—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02219—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen
- H01L21/02222—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen the compound being a silazane
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- H01L21/02107—Forming insulating materials on a substrate
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- 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
- H01L21/02123—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 silicon
- H01L21/02164—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 silicon the material being a silicon oxide, e.g. SiO2
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Description
本出願は、2015年6月12日に出願された米国特許出願第14/738,039号明細書および2015年3月30日に出願された米国仮特許出願第62/140,248号明細書の利益を主張するものであり、どちらもあらゆる目的のためにその全体を本明細書に援用する。
ications Thereof)について記載している。米国特許第7,122,222号明細書(これもAir Products and Chemicals,Inc.へ付与されている)は、ケイ素含有膜を付着させるための前駆体およびその方法(Precursors for Depositing Silicon Containing Films and Processes Thereof)を開示している。国際公開第2013/058061号パンフレットに開示されているシラザン化合物N-(SiR1R2R3)mR4 3-mは、コーティングガスとして使用される。米国特許第5,332,853号明細書に開示されている(RR1R2Ma)yA(R3)xは、官能基化されたアルキルアルカリ金属化合物を製造するための触媒化合物として使用される。類似の特許として、米国特許第5,663,398A号明細書、米国特許第5,332,853A号明細書、米国特許第5,340,507A号明細書、欧州特許出願公開第525881A1号明細書がある。
・一置換TSA前駆体において、Xがハロゲン原子である;
・一置換TSA前駆体が(SiH3)2N-SiH2-Clである;
・一置換TSA前駆体が(SiH3)2N-SiH2-Brである;
・一置換TSA前駆体が(SiH3)2N-SiH2-Iである;
・一置換TSA前駆体において、Xがイソシアネート(-NCO)である一置換TSA前駆体(すなわち、(SiH3)2N-SiH2-NCO);
・Xがアミノ基[-NR1R2]である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NMe2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NMeEtである;
・一置換TSA前駆体が(SiH3)2N-SiH2-NEt2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NiPr2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NHiPrである;
・一置換TSA前駆体が(SiH3)2N-SiH2-NMeiPrである;
・一置換TSA前駆体が(SiH3)2N-SiH2-NEtiPrである;
・一置換TSA前駆体が(SiH3)2N-SiH2-NHtBuである;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NHEt))(すなわち、X=NR1R2であり、R1がSiH3であり、R2がNHE
tである)ではない;
・一置換TSA前駆体において、Xが-N(SiR3)2である[式中、各Rは、独立に、ハロゲン、H、またはC1-C4のアルキル基から選択される];
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiCl3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiBr3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiI3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiH3)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2Cl)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NEt2)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NiPr2)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NHtBu)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2OEt)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2OiPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiMe3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NH(SiMe3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiEt3)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2Et)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2iPr)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2nPr)2である;
・一置換TSA前駆体において、XがC4-C10の窒素含有複素環である;
・一置換TSA前駆体において、C4-C10の窒素含有複素環がピロリジン、ピロール、およびピペリジンから選択される;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピロリジン)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピロール)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピペリジン)である;
・一置換TSA前駆体において、Xがアルコキシ基[-O-R]である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OH)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OMe)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OEt)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OiPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OnPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OtBu)である;
・一置換TSA前駆体において、Xが-O-SiR3であり、各Rは独立に、H、ハロゲン、またはC1-C4のヒドロカルビル基から選択される;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiH3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiCl3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiBr3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiI3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiMe3)である;
・Si含有膜形成組成物がおよそ95% w/w~およそ100% w/wの前駆体を含む;
・Si含有膜形成組成物がおよそ5% w/w~およそ50% w/wの前駆体を含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのAlを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのAsを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのBaを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのBeを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのBiを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのCdを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのCaを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのCrを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのCoを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのCuを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのGaを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのGeを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのHfを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのZrを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのInを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのFeを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのPbを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのLiを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのMgを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのMnを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのWを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのNiを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのKを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのNaを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのSrを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのThを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのSnを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのTiを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのUを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのVを含む;
・Si含有膜形成組成物がおよそ0ppbw~およそ500ppbwのZnを含む;
・Si含有膜形成性オルガノシラン組成物がおよそ0ppmw~およそ500ppmwのClを含む;
・Si含有膜形成組成物がおよそ0ppmw~およそ500ppmwのBrを含む;
・Si含有膜形成組成物がおよそ0ppmw~およそ500ppmwのIを含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのTSAを含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wの(SiH3)2-N-SiH2X[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wの(SiH3)2-N-SiHX2[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのSiH4を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのSiH3X[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのSiH2X2[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのSnX2[式
中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのSnX4[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのHX[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのNH3を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのNH4X[式中、XはCl、Br、またはIである]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのROH[式中、RはC1-C4のアルキル基である]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのNH2R[式中、RはC1-C4のアルキル基である]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのNR2H[式中、RはC1-C4のアルキル基である]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのHN=R[式中、RはC1-C4のアルキル基である]を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのテトラヒドロフラン(THF)を含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのエーテルを含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのペンタンを含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのシクロヘキサンを含む;
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのヘプタンを含む;または
・Si含有膜形成組成物がおよそ0.0% w/w~0.1% w/wのトルエンを含む。
・Si含有膜形成組成物が、10ppmw未満の金属不純物の総濃度を有する;
・注入管側の先端がSi含有膜形成組成物の表面の上に位置し、排出管の先端がSi含有膜形成組成物の表面の下に位置する;
・注入管側の先端がSi含有膜形成組成物の表面の下に位置し、排出管の先端がSi含有膜形成組成物の表面の上に位置する;
・注入管および排出管に、隔膜バルブをさらに含む;
・Si含有膜形成組成物が(H3Si)2N-SiH2(NEt2)である;
・Si含有膜形成組成物が(H3Si)2N-SiH2(NiPr2)である;
・Si含有膜形成組成物が(H3Si)2N-SiH2Clである;
・Si含有膜形成組成物が(H3Si)2N-SiH2(N(SiMe3)2である。
・第2前駆体を含む蒸気を反応器に送り込む;
・第2前駆体の元素が、第2族、第13族、第14族、遷移金属、ランタニド、および
これらの組合せからなる群から選択される;
・第2前駆体の元素が、As、B、P、Si、Ge、Al、Zr、Hf、Ti、Nb、Ta、またはランタニドから選択される;
・反応物を反応器に送り込む;
・反応物が、O2、O3、H2O、H2O2、NO、NO2、カルボン酸、アルコール、ジオール、それらのラジカル、およびそれらの組合せからなる群から選択される;
・反応物がプラズマ処理酸素である;
・Si含有層が酸化ケイ素含有層である;
・反応物が、N2、H2、NH3、ヒドラジン類(N2H4、MeHNNH2、MeHNNHMeなど)、有機アミン(NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NHなど)、ピラゾリン、ピリジン、ジアミン(エチレンジアミンなど)、それらのラジカル種、およびそれらの混合物からなる群から選択される;
・蒸着法が化学蒸着プロセスである;
・蒸着法がALDプロセスである;
・蒸着法が空間的ALDプロセス(spatial ALD process)である;
・蒸着プロセスが流動性CVDプロセス(flowable CVD process)である;
・ケイ素含有層がSiである;
・ケイ素含有層がSiO2である;
・ケイ素含有層がSiNである;
・ケイ素含有層がSiONである;
・ケイ素含有層がSiOCである;
・ケイ素含有層がSiOCNである;
・ケイ素含有層がSiCNである;
・Si含有層を熱アニールする;
・反応性雰囲気下でSi含有層を熱アニールする;
・Si含有層をUV硬化させる;
・Si含有層を電子ビーム硬化させる。
・送り込む工程と送り込む工程との間に不活性ガスで反応器をパージする;
・一置換TSA前駆体において、Xがハロゲン原子である;
・一置換TSA前駆体が(SiH3)2N-SiH2-Clである;
・一置換TSA前駆体が(SiH3)2N-SiH2-Brである;
・一置換TSA前駆体が(SiH3)2N-SiH2-Iである;
・一置換TSA前駆体において、Xがイソシアネート-NCOである(すなわち、(SiH3)2N-SiH2-NCO);
・一置換TSA前駆体において、Xがアミノ基[-NR1R2]である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NiPr2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NHiPrである;
・一置換TSA前駆体が(SiH3)2N-SiH2-NHtBuである;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NHEt))(すなわち、X=NR1R2であり、R1がSiH3であり、R2がNHEt)ではない;
・一置換TSA前駆体が(SiH3)2N-SiH2-NEt2である;
・一置換TSA前駆体が(SiH3)2N-SiH2NEtMeである;
・一置換TSA前駆体が(SiH3)2N-SiH2NMe2である;
・一置換TSA前駆体が(SiH3)2N-SiH2NMeiPrである;
・一置換TSA前駆体が(SiH3)2N-SiH2NEtiPrである;
・一置換TSA前駆体において、Xが-N(SiR3)2[式中、各Rは独立に、ハロゲン、H、またはC1-C4のアルキル基から選択される]である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiCl3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiBr3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiI3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiH3)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2Cl)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NEt2)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NiPr2)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2(NHtBu)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2OEt)である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiH3)(SiH2OiPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiMe3)2である;
・一置換TSA前駆体が(SiH3)2N-SiH2-NH(SiMe3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-N(SiEt3)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2Et)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2iPr)2である;
・一置換TSA前駆体が(SiH3)2-N-SiH2-N(SiMe2nPr)2である;
・一置換TSA前駆体において、XがC4-C10の窒素含有複素環である;
・一置換TSA前駆体において、C4-C10の窒素含有複素環が、ピロリジン、ピロール、およびピペリジンから選択される;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピロリジン)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピロール)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(ピペリジン)である;
・一置換TSA前駆体において、Xがアルコキシ基[-O-R]である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OH)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OMe)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OEt)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OiPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OnPr)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OtBu)である;
・一置換TSA前駆体において、Xが-O-SiR3であり、各Rが独立に、H、ハロゲン、またはC1-C4のヒドロカルビル基から選択される;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiH3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiCl3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiBr3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiI3)である;
・一置換TSA前駆体が(SiH3)2N-SiH2-(OSiMe3)である;
・反応物が、O2、O3、H2O、H2O2、NO、NO2、カルボン酸、アルコール、ジオール、それらのラジカル、およびそれらの組合せからなる群から選択される;
・反応物が、N2、H2、NH3、ヒドラジン類(N2H4、MeHNNH2、MeHNNHMeなど)、有機アミン(NMeH2、NEtH2、NMe2H、NEt2H、NMe3、NEt3、(SiMe3)2NHなど)、ピラゾリン、ピリジン、ジアミン(エチレンジアミンなど)、それらのラジカル種、およびそれらの混合物からなる群から選択される。
ある特定の略号、記号、および用語は、以下に続く記述および請求項全体で使用されており、それには以下のものが含まれる。
(SiH3)2N-SiH2-X
[式中、Xは、Cl、BrまたはIから選択されるハロゲン原子;イソシアナト基[-NCO];アミノ基[-NR1R2];C4-C10の飽和または不飽和の窒素含有複素環;またはアルコキシ基[-O-R]から選択され;ここで、R1、R2およびRはそれぞれ、H;シリル基(SiR’3);またはC1-C6の直鎖または分枝の飽和または不飽和ヒドロカルビル基から選択され、ここで、各R’は独立に、H;Cl、Br、またはIから選択されるハロゲン原子;C1-C4の飽和または不飽和ヒドロカルビル基;C1-C4の飽和または不飽和アルコキシ基;またはアミノ基[-NR3R4](式中、R3およびR4はそれぞれ、HまたはC1-C6の直鎖または分枝の飽和または不飽和ヒドロカルビル基から選択される)から選択されるが、但し、R1=Hである場合、R2≠H、MeまたはEtである]。C1-C6の直鎖または分枝の飽和または不飽和ヒドロカルビル基は、アミンまたはエーテルを含みうる。あるいはまた、R1およびR2は独立に、Me、Et、iPr、nPr、tBu、nBu、およびsecBuから選択できる。
、当業者なら理解するであろう。
る流れを形成することができる。その流れから、当業者が容易に考え出す方法(分別蒸留といった方法)によって(SiH3)2-N-SiH2[N(SiH3)2]を分離できる。
N(SiH3)3+EtOH→N(SiH3)2(SiH2OEt)
ウム(K)、ナトリウム(Na)、ストロンチウム(Sr)、トリウム(Th)、スズ(Sn)、チタン(Ti)、ウラン(U)、バナジウム(V)および亜鉛(Zn)があるが、これらに限定されない。精製された一置換TSA前駆体組成物中のX(ここで、X=Cl、Br、I)の濃度は、およそ0ppmw~およそ100ppmw、より好ましくはおよそ0ppmw~およそ10ppmwの範囲であり得る。
注入管30の端部31はSi含有膜形成組成物10の表面の下に位置しているが、排出管40の端部41は、Si含有膜形成組成物10の表面の上に位置している。図2はまた、Si含有膜形成組成物10の温度を上昇させることができる任意選択の加熱エレメント25を含む。Si含有膜形成組成物10は、固体状であっても液体状であってもよい。不活性ガス(窒素、アルゴン、ヘリウム、およびそれらの混合物があるが、それらに限定されない)は、注入管30に送り込まれる。不活性ガスは、Si含有膜形成組成物10の中を流れ、不活性ガスと蒸気化されたSi含有膜形成組成物10との混合物を、排出管40および半導体加工手段内の構成部分に運ぶ。
・室温で液体であるか、融点が50℃より低い;
・粒子を発生することなくふさわしく分配(気相注入または直接液体注入)できるよう熱的に安定している;および/または
・広い自己制御ALDウィンドウとなるような、基板との適切な反応性(これにより、様々なSi含有膜の付着が可能になる)。
・ハロゲン化金属(例えば、TiCl4、TiI4、TaCl5、HfCl4、ZrC
l4、AlCl3、NbF5など);
・アルキル(Al、Ge、Ga、In、Sb、Sn、Zn)(トリメチルアルミニウム、ジエチル亜鉛、トリエチルガリウムなど);
・水素化物(GeH4、アランなど);
・アルキルアミド(第IV族および第V族遷移金属の金属);
・イミド基(第V族および第VI族の金属);
・アルコキシド(第IV族、第V族の金属);
・シクロペンタジエニル(Ru、Co、Fe、第IV族の遷移金属、ランタニドなど);
・カルボニル(例:Ru、Co、Fe、Ni);
・アミジナートおよびグアニジネート(例:Co、Mn、Ni、Cu、Scなど);
・ベータ-ジケトナート(例:Sc、Cu、ランタニド);
・ベータ-ジケトイミン(Cu、Ni、Coなど);
・ビス-トリアルキルシリルアミド(Ni、Co、Feなど);
・オキソ基(RuO4、WOCl4、PO(OEt)3、AsO(OEt)3など);
・または上記の配位子の組合せを有するヘテロレプチック分子。
の上に配置された(あるいは広げられた)ある物質の厚さを表すこと、またその表面は溝または線であってよいことを、当業者なら理解するであろう。本明細書および請求項全体を通じて、ウェーハおよびその上にある関連した層はいずれも、基板と呼ばれる。但し、多くの例で、使用される好ましい基板は、銅、酸化ケイ素、フォトレジスト、水素化炭素、スズ、SRO、Ru、およびSiタイプの基板(ポリシリコン基板または結晶シリコン基板など)から選択できる。例えば、窒化ケイ素膜は、Si層の上に付着させることができる。その後の処理では、酸化ケイ素層と窒化ケイ素層とを交互に、窒化ケイ素層に付着させて、3D NANDゲートで使用される複数のSiO2/SiN層のスタックを形成することができる。さらに、基板は、パターン化された有機または無機膜、あるいはパターン化されていない有機または無機膜で被覆することができる。
、以下のもの(但し、それらに限定されない)から選択される金属含有前駆体を含むことができる:
・ハロゲン化金属(例えば、TiCl4、TiI4、TaCl5、HfCl4、ZrCl4、AlCl3、NbF5など);
・アルキル(Al、Ge、Ga、In、Sb、Sn、Zn)(トリメチルアルミニウム、ジエチル亜鉛、トリエチルガリウムなど);
・水素化物(GeH4、アランなど);
・アルキルアミド(第IV族および第V族遷移金属の金属);
・イミド基(第V族および第VI族の金属);
・アルコキシド(第IV族、第V族の金属);
・シクロペンタジエニル(Ru、Co、Fe、第IV族遷移金属、ランタニドなど);
・カルボニル(例:Ru、Co、Fe、Ni);
・アミジナートおよびグアニジネート(例:Co、Mn、Ni、Cu、Scなど);
・ベータ-ジケトナート(例えば、Sc、Cu、ランタニド);
・ベータ-ジケトイミン(Cu、Ni、Coなど);
・ビス-トリアルキルシリルアミド(Ni、Co、Feなど);
・オキソ基(RuO4、WOCl4、PO(OEt)3、AsO(OEt)3など);
・上記のファミリーから選択される配位子の組合せを有するヘテロレプチック分子。
剰の金属含有前駆体はいずれも、反応チャンバーのパージおよび/または排気により反応チャンバーから除去する。もう一度、酸素源を反応チャンバーに送り込んで金属含有前駆体と反応させることができる。過剰の酸素源は、反応チャンバーのパージおよび/または排気により反応チャンバーから除去する。所望の厚さの膜が得られたなら、プロセスを終了させることができる。しかし、より厚い膜が望ましいなら、4段階プロセス全体を繰り返すことができる。Si含有膜形成組成物、金属含有前駆体、および酸素源の供給量を変えることにより、所望の組成および厚さの膜を付着させることができる。
応物(典型的にはNH3)と混合される。このようにして、薄いなじみやすいSiN膜を基板に付着させることができる。一置換TSA前駆体およびN源の流量を調整することにより、膜におけるSi/N比率を調整できることを、当業者なら理解するであろう。
であるが、当然ながらMの酸化状態によって異なる]を含むことができる。適切な一置換TSA前駆体および反応物をふさわしく判断して選ぶなら、所望の膜組成物を得られることを、当業者なら理解するであろう。
オーバーヘッド機械式撹拌器(overhead mechanical stirrer)と窒素バブラーと冷却装置と水素化物スクラバーとを備えた、反応器である1リットルのフィルターフラスコに、300gのジイソプロピルアミン(3.0mol)を充填した。60g(0.4mol)のクロロトリシリルアミン(chlorotrisilylamine)を滴下漏斗に注いだ。滴下漏斗は、反応器に取り付けられていた。滴下漏斗を窒素洗浄して、漏斗の先端に塩が形成されないようにした。冷却装置を18℃に設定し、1.5時間かけて滴下漏斗を介してクロロトリシリルアミンを添加した。添加の間、反応器温度は22~23℃に設定した。添加を終えた後、0.5時間の間、反応器が撹拌されるようにした。
オーバーヘッド機械式撹拌器と窒素バブラーと冷却装置と水素化物スクラバーとを備えた、反応器である1リットルのフィルターフラスコに、300gのイソプロピルアミン(3.0mol)を充填した。60g(0.4mol)のクロロトリシリルアミンを滴下漏斗に注いだ。滴下漏斗は、反応器に取り付けられていた。滴下漏斗を窒素洗浄して、漏斗の先端に塩が形成されないようにした。冷却装置を18℃に設定し、1.5時間かけて滴下漏斗を介してクロロトリシリルアミンを添加した。添加の間、反応器温度は22~23℃に設定した。添加を終えた後、0.5時間の間、反応器が撹拌されるようにした。その後、アミン塩酸塩を濾過した。濾過ケークは、50ml×2の分量のイソプロピルアミンで洗浄した。イソプロピルアミンの大部分を留去すると、72gの粗生成物が残った。この粗生成物を、同様にして行われたより小規模のいくらかの(SiH3)2N-SiH2-NHiPrの調製からの別の粗生成物と一緒にした。その後、(SiH3)2N-SiH2-NHiPrを、86℃において-28inHgの真空下で蒸留し、純度が99%を超える79gの生成物を回収した。
(SiH3)2N-SiH2-Brおよび(SiH3)2N-SiH2-N(SiH3)2は、SnBr4をTSAと反応させて得ることができる:SnBr4+H3SiN(SiH3)2=BrH2SiN(SiH3)2+(SiH3)2N-SiH2-N(SiH3)2+SnBr2+HBr。次いで、上記の反応の副生成物(HBr)を、出発物質TSAと反応させて除去できる。すなわち、N(SiH3)3+4HBr=NH4Br+3BrSiH3。合成プロセスは以下の通りである。
DNF Co.,Ltd.に付与された国際公開第2015/190749号パンフレットでは、実施例1は、n-ペンタン中のクロロジメチルシラン[Me2HSiCl]をNH3と反応させて、テトラメチルジシラザン[(Me2SiH)2NH]を形成することにより、ジメチルアミノジメチルシリルビスジメチルシリルアミン[(Me2SiH)2NSiMe2(NMe2)]を合成することを開示している。その後、テトラメチルジシラザンをn-ヘキサン溶媒中のn-BuLiと反応させて、(Me2SiH)2N-Liを形成する。クロロジメチルジメチルアミノシラン[ClSiMe2(NMe2)]を混合物に加えると、(Me2SiH)2NSiMe2(NMe2)生成物が形成される。
以下のPEALD試験を、4インチのウェーハを備えたPicosun R200 PEALD 8インチ付着器具を用いて実施した。一置換TSA前駆体の蒸気を、図3に示すようにPicosun器具に送った。
70℃に加熱されたアンプル中に置かれた(SiH3)2N-SiH2-NiPr2、酸化反応物であるO2プラズマ、および追加反応物であるNH3プラズマを用いて、窒素をドープした酸化ケイ素を付着させるALD試験を実施した。反応器の圧力を約9hPaに固定して、典型的なALD条件を使用した。3方向空気圧弁を用いて、前駆体蒸気の2つの0.1秒パルスを、アンプル内の過剰圧力によって蒸着チャンバーに送り込んだ。0.5秒の休止を入れて、0.1秒パルスと0.1秒パルスの間を分けた。4秒間のN2パージによって過剰の前駆体を除去した。16秒間のプラズマO2パルスの後に、3秒間のN2パージを行った。3方向空気圧弁を用いて、前駆体蒸気の2つの0.1秒パルスを、
アンプル内の過剰圧力によって蒸着チャンバーに送り込んだ。0.5秒の休止を入れて、0.1秒パルスと0.1秒パルスの間を分けた。4秒間のN2パージによって過剰の前駆体を除去した。11秒間のプラズマNH3パルスの後に、3秒間のパージを行った。厚さが少なくとも300Åに達するまで、プロセス全体(前駆体-プラズマO2-前駆体-プラズマNH3)を繰り返した。付着は150℃で行った。
26℃に加熱されたアンプル中に置かれた(SiH3)2N-SiH2-N(SiH3)2、および酸化反応物としてのO2プラズマを用いて、ALD試験を行った。反応器の圧力を約9hPaに固定して、典型的なALD条件を使用した。3方向空気圧弁を用いて、前駆体蒸気の3つの0.1秒パルスを、アンプル内の過剰圧力によって蒸着チャンバーに送り込んだ。0.5秒の休止を入れて、0.1秒パルスと0.1秒パルスの間を分けた。4秒間のN2パージによって過剰の前駆体を除去した。16秒間のプラズマO2パルスの後に、3秒間のN2パージを行った。厚さが少なくとも300Åに達するまで、プロセス全体(前駆体-プラズマO2)を繰り返した。図6に示すように、付着温度を150℃から300℃に上昇させるにつれて、1サイクル当たりの成長は増大した。図6は、5つの0.1秒パルスの結果と3つの0.1秒パルスの結果とを比較した、1サイクル当たりの成長も示している。どちらもおよそ0.6Å/サイクルであったが、これは実際のALD飽和を示す。というのは、5つのパルスでより多くの量の前駆体を送り込んでも、3つのパルスで生成される膜より成長速度が速くなっていないからである。
Claims (7)
- Si含有膜を形成するための方法であって、
基板を含む反応器に、
次式:
(SiH3)2N-SiH2-X
[式中、Xは、C4~C10の飽和または不飽和の窒素含有複素環である。]を有する一置換TSA前駆体を含む、Si含有膜形成組成物を含む蒸気を送り込む工程と、
蒸着プロセスを用いて、前記一置換TSA前駆体の少なくとも一部を前記基板上に付着させて、前記基板上に前記Si含有膜を形成する工程と、
を含み、
前記基板が、ケイ素ウェーハ、ガラス基板、およびプラスチック基板からなる群から選択される、方法。 - 前記基板を、有機質または無機質のパターン化または非パターン化膜で被覆する、請求項1に記載の方法。
- 前記反応器に反応物を送り込む工程であって、前記反応物が、O2、O3、H2O、H2O2、NO、NO2、N2O、アルコール、ジオール、カルボン酸、ケトン、エーテル、O原子、Oラジカル、Oイオン、アンモニア、N2、N原子、Nラジカル、Nイオン、飽和または不飽和ヒドラジン、アミン、ジアミン、エタノールアミン、H2、H原子、Hラジカル、Hイオン、およびこれらの組合せからなる群から選択される、工程をさらに含む、請求項1に記載の方法。
- a)基板を含む反応器に、
次式:
(SiH3)2N-SiH2-X
[式中、Xは、アミノ基[-NR1R2]またはC4~C10の飽和または不飽和の窒素含有複素環から選択され、かつ、
アミノ基[-NR1R2]のR1およびR2は、それぞれ、H、1つのC3の直鎖の飽和または不飽和ヒドロカルビル基、1つのC4の直鎖または分岐の飽和または不飽和ヒドロカルビル基を表し、但し、ここで、R1がHである場合、R2はHまたはtert-Buではない。]で表される一置換TSA前駆体を含む、Si含有膜形成組成物を含む、蒸気を送り込みケイ素含有層を形成し;
b)酸化剤を前記反応器に送り込むことにより、前記酸化剤を前記ケイ素含有層と反応させて酸化ケイ素含有層を形成し;
c)前記一置換TSA前駆体を前記反応器に送り込むことにより、前記一置換TSA前駆体を前記酸化ケイ素含有層と反応させてケイ素を多く含む酸化ケイ素含有層を形成し;および
d)窒素含有反応物を前記反応器に送り込むことにより、前記窒素含有反応物を前記ケイ素含有層と反応させて窒素をドープした酸化ケイ素膜を形成する
というプロセスにより、窒素をドープした酸化ケイ素膜を形成する方法。 - それぞれの送り込む工程と送り込む工程との間に、前記反応器を不活性ガスでパージすることをさらに含む、請求項4に記載の方法。
- 前記一置換TSA前駆体が、
次式:
(SiH3)2N-SiH2-NHR2
[式中、R2が、n-Pr、n-Bu、または、sec-Buから選択される。]
で表される、請求項4または5に記載の方法。 - 前記一置換TSA前駆体が、
次式:
(SiH3)2N-SiH2-NH(n-Pr)
で表される、請求項6に記載の方法。
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