CN110036139A - 用于薄膜沉积的短无机三甲硅烷基胺基聚硅氮烷 - Google Patents
用于薄膜沉积的短无机三甲硅烷基胺基聚硅氮烷 Download PDFInfo
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- CN110036139A CN110036139A CN201780072505.0A CN201780072505A CN110036139A CN 110036139 A CN110036139 A CN 110036139A CN 201780072505 A CN201780072505 A CN 201780072505A CN 110036139 A CN110036139 A CN 110036139A
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- 125000004122 cyclic group Chemical group 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 229940031098 ethanolamine Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
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- 239000004519 grease Substances 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 239000004700 high-density polyethylene Substances 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
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- 238000005121 nitriding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
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- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
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- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- RDRCCJPEJDWSRJ-UHFFFAOYSA-N pyridine;1h-pyrrole Chemical compound C=1C=CNC=1.C1=CC=NC=C1 RDRCCJPEJDWSRJ-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical group 0.000 description 1
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- 239000010980 sapphire Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
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- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- QHAHOIWVGZZELU-UHFFFAOYSA-N trichloro(trichlorosilyloxy)silane Chemical compound Cl[Si](Cl)(Cl)O[Si](Cl)(Cl)Cl QHAHOIWVGZZELU-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 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
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—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
- H01L21/02211—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 being a silane, e.g. disilane, methylsilane or chlorosilane
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- 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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
-
- 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
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—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
- H01L21/0217—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 nitride not containing oxygen, e.g. SixNy or SixByNz
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—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 in the presence of a plasma [PECVD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/0228—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition deposition by cyclic CVD, e.g. ALD, ALE, pulsed CVD
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—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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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
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- Inorganic Chemistry (AREA)
- Plasma & Fusion (AREA)
- Chemical Vapour Deposition (AREA)
- Formation Of Insulating Films (AREA)
Abstract
披露了用于高纯度薄膜沉积的不含Si‑C并且是挥发性的硅氮烷前体。
Description
相关申请的交叉引用
本申请要求2017年7月27日提交的美国申请号15/661,576和2016年12月11日提交的美国临时申请号62/432,666号的权益，出于所有目的通过援引方式将两者以其全部内容结合在此。
技术领域
披露了形成含Si膜的组合物，这些组合物包含不含Si-C并且是挥发性的含硅氮烷前体。这些组合物可用于沉积高纯度薄膜。
背景技术
随着半导体器件按比例缩小，需要新的材料。普通材料，如氮化硅或氧化硅，需要在越来越严格的条件下沉积。例如，氮化硅沉积的一般趋势是在最低可能温度下进行化学气相沉积(CVD)或原子层沉积(ALD)，同时保持高沉积速率、高膜质量。对于这种工艺，前体分子对于获得具有低杂质并且具有合适的保形特性(从某些应用的高度保形到其他应用的自下而上填充)的高质量膜起着至关重要的作用。
Sanchez等人的美国专利申请公开号2015/047914披露了不含卤素的胺取代的三甲硅烷基胺和三二甲硅烷基胺化合物及其制备方法，其通过相应的未取代的三甲硅烷基胺与由过渡金属催化剂催化的胺之间的脱氢偶联。
Girard等人的US 2015/376211披露了经单取代的TSA前体的形成含Si膜的组合物。
Li等人的US 2016/0049293披露了一种方法和包括其的组合物，该方法通过提供额外的薄介电膜来密封多孔低介电常数层的孔。
Li等人的US 2016/0225616披露了一种包含多个含硅层的设备，其中含硅层选自氧化硅和氮化硅层或膜。
Lei等人的WO 2016/065221披露了组合物和使用这些组合物形成含硅膜或材料的方法。
由于Si-C键的低反应性和高热稳定性，已知没有Si-C直接键的分子比具有这种直接键的分子产生更纯的膜。
此外，具有烷氧基的硅烷很少通过原子层沉积表现出适当的自限制生长，并且不允许氮化硅膜的形成，由于氧通常保留在膜中，并且因此在可能的薄膜沉积应用方面不如具有Si-N键的氨基硅烷通用。然而，虽然烷氧基没有表现为在原子层沉积中表面反应的合适官能团，但是已经提出并可以使用具有Si-O-Si(硅氧烷)桥键的不含Si-C的分子。
已经提出并在工业上用于氧化硅和氮化硅薄膜沉积的典型不含Si-C的硅烷前体是
a-卤代硅烷，如二氯硅烷、一氯硅烷、六氯二硅烷、八氯三硅烷、二碘硅烷、五氯二硅烷等。
b-全氢化(聚)硅烷，如SiH4、Si2H6或Si3H8
c-具有通式SiHx(NR1R2)4-x的氨基硅烷，如双-二乙基氨基硅烷、三-二甲基氨基硅烷、二异丙基氨基硅烷、双(乙基甲基氨基)硅烷、四(乙基氨基)硅烷
d-氨基-二硅烷，如六(乙基氨基)二硅烷、二异丙基氨基硅烷、二乙基氨基二硅烷。
e-硅氧烷，如二硅氧烷、六氯二硅氧烷
f-三甲硅烷基胺，可用于多种沉积工艺，如可流动CVD、热低压CVD、等离子体增强CVD、ALD和等离子体增强ALD。
g-最近，其他富含硅的分子已被提出，如TSA-Cl或BDSASi。例如，已经报道了BDSASi通过PEALD产生每个周期高生长的SiN。
然而，仍然寻求能够在低温下实现较高生长速率(无论是通过ALD、CVD、可流动CVD或者其他形式的气相沉积)同时保持高膜纯度的分子，以进一步提高工艺生产率，或者能够在比通常的前体更低的温度条件下沉积。
发明内容
披露了形成含硅膜的组合物。形成含硅膜的组合物包含选自下组的前体，该组由以下各项组成：
(a)[(SiR3)2NSiH2]n-NL3-n，其中n＝2或3；
(b)(SiH3)2NSiH2-O-SiH2N(SiH3)2
(c)(SiR’3)2N-SiH2-N(SiR’3)2；以及
(d)[(SiR3)2NSiH2]m-NH2-m-C≡N，其中m＝1或2；
其中
-每个R独立地选自H、具有式-NR1R2的二烷基氨基、或脒基，
-每个R’独立地选自H、具有式-NR1R2的二烷基氨基、或脒基，前提是所有R’都不是H，
-R1和R2独立地选自H或C1-C12烃基，前提是R1和R2不能同时等于H，并且如果R1是H，则R2是C2-C12烃基，并且NR1R2可以一起形成含N杂环配体，并且
-L选自H或C1-C6烃基。
所披露的形成含硅膜的组合物可以包括以下方面中的一个或多个：
·前体是[(SiH3)2NSiH2]2NH；
·前体是[(SiH3)2NSiH2]3N；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NR1R2)；
·前体是(SiH3)2NSiH2-O-SiH2N(SiH3)2；
·前体是[(SiH3)2NSiH2]-NH-C≡N；
·前体是[(SiH3)2NSiH2]2N-C≡N；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NMe2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NEt2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NEtMe)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NiPr2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NtBu2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NnBu2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NsecBu2)；
·前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NHtBu)；
·形成含Si膜的组合物包含在大约95％w/w与大约100％w/w之间的前体；
·形成含Si膜的组合物包含在大约5％w/w与大约50％w/w之间的前体；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Al；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的As；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ba；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Be；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Bi；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Cd；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ca；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Cr；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Co；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Cu；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ga；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ge；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Hf；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Zr；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的In；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Fe；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Pb；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Li；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Mg；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Mn；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的W；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ni；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的K；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Na；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Sr；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Th；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Sn；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Ti；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的U；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的V；
·形成含Si膜的组合物包含在大约0ppbw与大约500ppbw之间的Zn；
·形成含Si膜的有机硅烷组合物包含在大约0ppmw与大约500ppmw之间的Cl；
·形成含Si膜的组合物包含在大约0ppmw与大约500ppmw之间的Br；
·形成含Si膜的组合物包含在大约0ppmw与大约500ppmw之间的I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的TSA；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的(SiH3)2-N-SiH2X，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的(SiH3)2-N-SiHX2，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的SiH4；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的SiH3X，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的SiH2X2，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的SnX2，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的SnX4，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的HX，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的NH3；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的NH4X，其中X为Cl、Br或I；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的ROH，其中R为C1-C4烷基；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的NH2R，其中R为C1-C4烷基；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的NR2H，其中R为C1-C4烷基；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的HN＝R，其中R为C1-C4烷基；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的四氢呋喃(THF)；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的乙醚；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的戊烷；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的环己烷；
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的庚烷；或
·形成含Si膜的组合物包含在大约0.0％w/w与0.1％w/w之间的甲苯。
披露了通过化学气相沉积法在基板上沉积含硅膜的方法。将以上披露的任何形成含Si膜的组合物的蒸气引入含有基板的反应器中。使用化学气相沉积法将前体的至少一部分沉积到基板上以在基板上形成含硅膜。所披露的方法可以包括以下方面中的一个或多个：
·该化学气相沉积法是原子层沉积工艺；
·该化学气相沉积法是等离子体增强的原子层沉积工艺；
·将包含第二前体的蒸气引入反应器中；
·第二前体的元素选自下组，该组由以下各项组成：第2族、第13族、第14族、过渡金属、镧系元素及其组合；
·第二前体的元素选自As、B、P、Si、Ge、Al、Zr、Hf、Ti、Nb、Ta或镧系元素；
·将反应物引入反应器中；
·反应物选自下组，该组由以下各项组成：O2、O3、H2O、H2O2、NO、NO2、羧酸、醇、二醇、其自由基及其组合；
·反应物为经等离子体处理的氧；
·该含硅膜是氧化硅膜；
·该含硅膜是氮化硅膜；
·该基板是硅晶片；
·该基板是玻璃；
·该基板是有机材料；
·对含Si层进行热退火；
·在反应氛围下对含Si层进行热退火；
·对含Si层进行UV固化；并且
·对含Si层进行电子束固化。
符号和命名法
贯穿以下说明及权利要求书中使用某些缩写、符号及术语，且其包括：
如本文所使用，不定冠词“一个/一种(a或an)”意指一个/一种或多个/多种。
如本文所使用，术语“大约(approximately)”或“约(about)”意指所陈述的值的±10％。
如本文所使用，当被用于描述R基团的上下文中时，术语“独立地”应当理解为表示对象R基团不仅相对于带有相同或不同下标或上标的其他R基团独立地选择，而且相对于同样的R基团的任何附加种类独立地选择。例如，在式MR1 x(NR2R3)(4-x)中，其中x是2或3，两个或三个R1基团与彼此或与R2或与R3可以但不必相同。此外，应当理解，除非另外特别说明，否则当在不同式中使用时，R基团的值彼此独立。
如本文所使用，术语“烃基”是指含有碳和氢的官能团；术语“烷基”是指仅仅含有碳和氢原子的饱和官能团。烃基可以是饱和的或不饱和的。这两个术语中的任何一个是指直链的、支链的、或环状基团。直链烷基的实例包括但不限于甲基、乙基、丙基、丁基等。支链烷基的实例包括但不限于叔丁基。环烷基的实例包括但不限于环丙基、环戊基、环己基等。
如本文所使用，“不含C”意指起始反应物不具有Si-C键。
如本文所使用，缩写“Me”是指甲基；缩写“Et”是指乙基；缩写“Pr”是指丙基；缩写“nPr”是指“正”或直链丙基；缩写“iPr”是指异丙基；缩写“Bu”是指丁基；缩写“nBu”是指“正”或直链丁基；缩写“tBu”是指叔丁基，也称为1,1-二甲基乙基；缩写“sBu”是指仲丁基，也称为1-甲基丙基；缩写“iBu”是指异丁基，也称为2-甲基丙基；术语“amyl”是指戊基(amyl)或戊基(pentyl group)(即C5烷基)；术语“tAmyl”是指叔戊基，也称为1,1-二甲基丙基。
术语“卤离子(halide)”是指卤素阴离子F-、Cl-、Br-、以及I-；术语“甲硅烷基”是指R3Si-配体，其中每个R独立地是H或C1-C4烷基。术语“卤盐”是指含有卤素离子的离子化合物。
如本文所使用，缩写“NR,R’R”-amd”或NR R”-amd(当R＝R’时)是指脒基配体[R-N-C(R”)＝N-R’]，其中R、R’和R”是H或所限定的烷基，如Me、Et、nPr、iPr、nBu、iBi、sBu或tBu；缩写“NR,R’-fmd”或NR-fmd(当R＝R’时)是指甲脒基(formidinate)配体[R-N-C(H)＝N-R’]，其中R和R’是所限定的烷基，如Me、Et、nPr、iPr、nBu、iBi、sBu或tBu。总体上，在脒基家族中选择的配体缩写为“AMD”。
本文使用元素周期表中元素的标准缩写。应当理解，可通过这些缩写提及元素(例如，Mn是指锰，Si是指硅，C是指碳等)。另外，第3族是指周期表的第3族(即Sc、Y、La、或Ac)。类似地，第4族是指周期表的第4族(即Ti、Zr、或Hf)并且第5族是指周期表的第5族(即V、Nb、或Ta)。
本文列举的任何及所有范围包括其端点(即，x＝1至4或x范围是从1至4，包括x＝1、x＝4及x＝其间的任何数)，不论是否使用术语“包括端点”。
请注意，所沉积的膜或层(诸如氧化硅或氮化硅)可以在整个说明书及权利要求书中在不提及其适当化学计量(即SiO2、SiO3、Si3N4)的情况下列举。这些层可以包括纯(Si)层、碳化物(SioCp)层、氮化物(SikNl)层、氧化物(SinOm)层或其混合物，其中k、l、m、n、o和p范围从1至6(包括端点)。例如，氧化硅为SinOm，其中n范围从0.5至1.5并且m范围从1.5至3.5。更优选地，氧化硅层为SiO2或SiO3。这些膜也可以含有氢，典型地从0at％至15at％。然而，由于没有常规测量，除非另有明确说明，否则任何给出的膜组成都忽略其H含量。
基板被理解为膜沉积在其上的主要固体材料。应当理解，膜可以被沉积在本身在基板上的层堆叠体上。基板典型地为，但不限于硅、玻璃、石英、蓝宝石、GaN、AsGa、Ge的晶片。基板可以是片材，典型地是金属、玻璃、有机材料如聚碳酸酯、PET、ABS、PP、HDPE、PMMA等。基板可以是类似材料的三维(3D)物体。在硅晶片上，基板上的典型层可以是Ge，SiGe，氧化硅，氮化硅，金属(如Cu、Co、Al、W、Ru、Ta、Ti、Ni)，金属硅化物和合金，金属氮化物(如TaN、TiN、VN、NbN、HfN、VN)；掺杂碳的二氧化硅膜(无论是致密的或多孔的)，碳氮化硅，无定形碳，氮化硼，碳氮化硼，有机材料，如旋涂碳、聚酰亚胺、光致抗蚀剂和减反射层；金属氧化物，如Ti、Hf、Zr、Ta、Nb、V、Mo、W、Al、以及镧系元素的氧化物。基板可具有如孔或沟槽的形貌，典型地具有在5nm至100μm范围内，并且通常在20nm与1μm之间的开口，以及高达1:1000，更通常在1:2至1:100范围内的纵横比。
附图说明
为了进一步理解本发明的本质和目的，应结合附图来参考以下详细说明，其中：
图是实例的全氢化聚硅氮烷油状物的气相色谱图。
具体实施方式
披露了形成含硅膜的组合物，其包含具有至少三甲硅烷基胺骨架的短链(Si范围从3至10)低聚硅氮烷，所述三甲硅烷基胺骨架选自以下家族：
(1)[(SiR3)2NSiH2]n-NL3-n，其中n＝2或3
(2)(SiH3)2NSiH2-O-SiH2N(SiH3)2
(3)(SiR’3)2N-SiH2-N(SiR’3)2
(4)[(SiR3)2NSiH2]m-NH2-m-C≡N，其中m＝1或2
其中
-每个R独立地选自H、具有式-NR1R2的二烷基氨基、或脒基；
-每个R’独立地选自H、具有式-NR1R2的二烷基氨基、或脒基，前提是所有R’都不是H
-R1和R2独立地选自H或C1-C12烃基，前提是R1和R2不能同时等于H，并且如果R1是H，则R2是C2烃基或更大，
-NR1R2可以形成含N杂环配体，并且
-L选自H或C1-C6烃基
以上化合物的优选实施例包括：
-家族(1)的分子，其中所有R＝H，L＝H并且n＝2：[(SiH3)2NSiH2]2NH
-家族(1)的分子，其中所有R＝H，L＝C1-C6烃基并且n＝2：[(SiH3)2NSiH2]2NL
o以上分子，其中L选自甲基、乙基、异丙基、正丙基、叔丁基、仲丁基、正丁基、己基、乙烯基、烯丙基，
-家族(1)的分子，其中所有R＝H并且n＝3：[(SiH3)2NSiH2]3N
-家族(3)的分子，其中除了一个R’＝H并且一个R’是NR1R2之外全部如以上所定义：(SiH3)2N-SiH2-N(SiH3)(SiH2N(R1R2))
o以上分子，其中R1＝R2＝Et
o以上分子，其中R1＝R2＝iPr
o以上分子，其中R1＝R2＝Me
o以上分子，其中R1＝Me并且R2＝Et
o以上分子，其中R1＝R2＝tBu
o以上分子，其中R1＝R2＝n-Bu
o以上分子，其中R1＝R2＝secBu
o以上分子，其中R1＝H并且R2＝tBu
o以上分子，其中NR1R2是吡咯、吡咯烷、哌啶、咪唑或氮丙啶(azidrine)
-家族(4)的分子是[(SiH3)2NSiH2]2N-C≡N
-家族(4)的分子是[(SiH3)2NSiH2]-NH-C≡N
此外，本发明包括从以下合成工艺合成家族(1)、(2)、(3)以及(4)的化合物：
家族1
(1)(SiR3)2NSiH2-X(X选自Cl、Br、I、SCN或NCO)与伯胺NH2L的反应根据以下反应进行：
n(SiR3)2NSiH2-X+NH2L→[(SiR3)2NSiH2]n-NL3-n+(n+1)NH3LX(盐)
-该反应优选在无水和非质子溶剂或溶剂混合物中进行，例如但不限于C3-C24烃溶剂、甲苯、苯、二乙醚、乙腈或四氢呋喃(THF)。
-该反应在-40℃与100℃之间的温度下，优选在室温下进行。
-任选地，从反应混合物中过滤所形成的盐，并通过蒸馏分离剩余液体组合物的组分。
-任选地，家族(1)的化合物通过蒸馏纯化以达到>98％、更优选或>99％、并且甚至更优选>99.5％的测定，这对于半导体级前体是典型的
-任选地，可以将家族(1)的产品进一步处理以降低溶解的NH3LX盐的含量，例如通过将产品暴露于固体吸附剂，如活性炭、干燥的Amberlyst树脂或其他这种离子交换树脂。
-任选地，可以将产品过滤以达到半导体工业中使用的产品的典型规格
-(SiR3)2NSiH2-X反应物可以如在共同未决的美国专利申请公开号2015/0376211中所披露的那样合成，更特别地通过SnX4+N(SiR3)3→N(SiR3)2(SiR2X)+SnX2↓+HXl，其中X是Cl、Br、或I(参见J.Chem.Soc.Dalton Trans.[英国化学会道尔顿会刊]1975，第1624页)。可替代地，二卤基硅烷[SiR2X2，其中X是Cl、Br或I]和单卤基硅烷[SiR3X，其中X是Cl、Br或I]可以在室温下，以1/20至1/4比率，与400sccm的NH3一起以气相连续引入如Miller的美国专利号US 8,669,387所述的流过式管式反应器中。NH3与2当量的单卤基硅烷发生反应，主要产生二甲硅烷基胺(DSA)。然后DSA与二卤基硅烷反应以形成(SiH3)2-N-SiH2X和HX(其中X是Cl、Br、或I)。本领域普通技术人员将认识到，反应可以以一个或两个步骤发生(首先由单卤基硅烷和NH3形成DSA且其次添加二卤基硅烷)或以一个步骤发生(在一个步骤中将单卤基硅烷、二氯硅烷和NH3合并)。
(2)如在美国专利申请公开号2015/0094470中描述的，(SiR3)2NSiH3与NH2L在催化剂的存在下的直接脱氢偶联反应根据以下反应进行：
n(SiR3)2NSiH3+NH2L→[(SiR3)2NSiH2]n-NL3-n+H2
-该反应或以纯的形式或在非质子溶剂中进行，例如但不限于C3-C24烃溶剂、甲苯、苯、二乙醚、乙腈、或THF。
-该反应在室温与150℃之间的温度下，优选在30℃-60℃下进行。
-任选地，从反应混合物中过滤催化剂，并通过蒸馏分离剩余液体组合物的组分。
-任选地，用试剂处理反应混合物以使催化剂失活，该试剂选自但不限于叔胺或配位化合物，如XNR4(X＝F、Cl、Br、I；R＝烷基)，R-CN，R2S，或PR3。
-任选地，家族(1)的化合物通过蒸馏纯化以达到>98％、更优选或>99％、并且甚至更优选>99.5％的测定，这对于半导体级前体是典型的
-任选地，产品可以被过滤以达到半导体工业中使用的产品的典型规格。
家族2
(3)(SiH3)2NSiH2-X(其中X选自Cl、Br、I、SCN NCO、或NR1R2基团，并且NR1R2如以上定义)与H2O反应物的反应根据以下反应进行：
2(SiH3)2NSiH2-X+H2O→(SiH3)2NSiH2-O-SiH2N(SiH3)2+2HX
-该反应优选在无水或非质子溶剂或溶剂混合物中进行，例如但不限于C3-C24烃溶剂、甲苯、苯、二乙醚、乙腈、或THF。
-将H2O缓慢加入到含硅烷的组合物中，以在整个反应中保持硅烷部分的恒定过量
-该反应在-40℃与100℃之间的温度下，优选在-20℃至室温下进行。
-任选地，以载气中的蒸汽的形式将水添加至表面下
-任选地，添加在极性非质子溶剂中稀释的水(典型地从1％至50％，更优选从5％至30％)
-任选地，并且优选当X是卤素时，反应混合物包含卤化物清除剂，例如但不限于吡啶、三烷基胺，其量高于在摩尔基础上的HX预期释放。该卤化物清除剂可以用作溶剂。然后可以过滤反应混合物以在最终产物分离之前除去形成的HX清除剂盐。
-任选地，家族(2)的化合物通过真空蒸馏纯化以达到>98％、更优选或>99％、并且甚至更优选>99.5％的测定，这对于半导体级前体是典型的
-任选地，可以将家族(2)的产品进一步处理以降低溶解盐的含量，例如通过将产品暴露于固体吸附剂，如活性炭、干燥的Amberlyst树脂或其他这种离子交换树脂。
-任选地，产品可以被过滤以达到半导体工业中使用的产品的典型规格。
家族3
根据如在美国专利申请公开号2015/0094470中所描述的相同方案，家族3的化合物优选通过脱氢偶联由(SiH3)2N-SiH2-N(SiH3)2(BDSASi)与胺的直接反应合成。
SiH2[N(SiH3)2]2+n HNR1R2→SiH2[N(SiH3-x(NR1R2)x][SiH3-y(NR1R2)y]+(x+y)H2
其中x＝0至3，y＝1至3
-该反应以纯的形式或在非质子溶剂中进行，例如但不限于C3-C24烃溶剂、甲苯、苯、二乙醚、乙腈、或THF。
-该反应在室温与150℃之间的温度下，优选在30℃-60℃下进行。
-任选地，从反应混合物中过滤催化剂，并通过蒸馏分离剩余液体组合物的组分。
-任选地，用试剂处理反应混合物以使催化剂失活，该试剂选自但不限于叔胺或配位化合物，如XNR4(X＝F、Cl、Br、I；R＝烷基)，R-CN，R2S，PR3。
-任选地，家族(3)的化合物通过蒸馏纯化以达到>98％、更优选或>99％、并且甚至更优选>99.5％的测定，这对于半导体级前体是典型的
-任选地，产品可以被过滤以达到半导体工业中使用的产品的典型规格。
-(SiR3)2NSiH2-X反应物可以如在共同未决的美国专利申请申请号62/432,592中所披露的那样合成，更特别地通过将三甲硅烷基胺与催化剂(如B(C6F5)3、BPh3、PdCl2、Co2(CO)8、或沸石Y(H)Si:Al)混合，而不需要NH3反应物或热量。
家族4
(SiR3)2NSiH2-X(X选自Cl、Br、I、SCN或NCO)与氰胺基H2N-C≡N的反应根据以下反应进行：
m(SiR3)2NSiH2-X+(m+1)H2N-C≡N
→[(SiR3)2NSiH2]mH2-mN-C≡N+m XH3N-C≡N(盐)
-该反应优选在无水和非质子溶剂或溶剂混合物中进行，例如但不限于C3-C24烃溶剂、甲苯、苯、二乙醚、乙腈、或THF。
-该反应在-40℃与100℃之间的温度下，优选在室温下进行。
-任选地，从反应混合物中过滤所形成的盐，并通过蒸馏分离剩余液体组合物的组分。
-任选地，家族(4)的化合物通过真空蒸馏纯化以达到>98％、更优选或>99％、并且甚至更优选>99.5％的测定，这对于半导体级前体是典型的
-任选地，可以将家族(4)的产品进一步处理以降低溶解的XH3N-C≡N盐的含量，例如通过将产品暴露于固体吸附剂，如活性炭、干燥的Amberlyst树脂或其他这种离子交换树脂。
为了确保方法可靠性，所披露的形成含Si膜的组合物在使用前可通过连续或分批式分馏法纯化至范围为从大约95％w/w至大约100％w/w，优选范围为从大约98％w/w至大约100％w/w的纯度。本领域普通技术人员将认识到纯度可通过H NMR或气相或液相色谱法连同质谱分析法测定。形成含Si膜的组合物可以含有以下杂质中的任一种：卤化物(X2)、三甲硅烷基胺、单卤基三甲硅烷基胺、二卤基三甲硅烷基胺、SiH4、SiH3X、SnX2、SnX4、HX、NH3、NH3X、一氯硅烷、二氯硅烷、醇、烷基胺、二烷基胺、烷基亚胺、THF、乙醚、戊烷、环己烷、庚烷或甲苯，其中X为Cl、Br或I。优选地，这些杂质的总量低于0.1％w/w。经纯化的组合物可通过再结晶、升华、蒸馏和/或将气体或液体传递通过适合吸附剂(诸如4A分子筛或基于碳的吸附剂(例如活性碳))来制得。
各溶剂(如THF、乙醚、戊烷、环己烷、庚烷和/或甲苯)在经纯化的经单取代的TSA前体的组合物中的浓度可在从大约0％w/w至大约5％w/w范围内，优选在从大约0％w/w至大约0.1％w/w范围内。溶剂可用于前体组合物的合成。若两者具有类似沸点，则可能难以自前体组合物中分离出溶剂。冷却混合物可在液体溶剂中产生固体前体，可通过过滤将其分离。还可使用真空蒸馏，前提是该前体组合物不被加热至大约高于其分解点。
所披露的形成含Si膜的组合物含有小于5％v/v、优选小于1％v/v、更优选小于0.1％v/v并且甚至更优选小于0.01％v/v的其单-、双-或三-类似物或其他反应产物中的任一种。此实施例可提供更好的工艺可重复性。此实施例可通过该形成含Si膜的组合物的蒸馏产生。
纯化所披露的形成含Si膜的组合物也可产生在从大约0ppbw至大约500ppbw、并且更优选从大约0ppbw至大约100ppbw范围内的浓度的痕量金属和类金属。这些金属或类金属杂质包括但不限于铝(Al)、砷(As)、钡(Ba)、铍(Be)、铋(Bi)、镉(Cd)、钙(Ca)、铬(Cr)、钴(Co)、铜(Cu)、镓(Ga)、锗(Ge)、铪(Hf)、锆(Zr)、铟(In)、铁(Fe)、铅(Pb)、锂(Li)、镁(Mg)、锰(Mn)、钨(W)、镍(Ni)、钾(K)、钠(Na)、锶(Sr)、钍(Th)、锡(Sn)、钛(Ti)、铀(U)、钒(V)及锌(Zn)。经纯化的经单取代的TSA前体组合物中的X(其中X＝Cl、Br、I)的浓度可在大约0ppmw与大约100ppmw之间的范围内且更优选在大约0ppmw至大约10ppmw之间的范围内。
任选地，产品可以被过滤以达到半导体工业中使用的产品的典型规格。
包含来自家族(1)至(4)的任何产品的任何组合物可用于含硅薄膜的化学气相沉积(CVD)，该含硅薄膜用于半导体、平板显示器、光伏应用中，并且更一般地，用于硅基涂料。应当理解，术语“CVD”包括其中使前体在气相中与要在其上沉积硅薄膜的基板接触的所有实施例。因此，术语CVD可以意指低压化学气相沉积(LPCVD)、低于大气压的化学气相沉积(SA-CVD)、大气压化学气相沉积(AP-CVD)、可流动化学气相沉积(F-CVD)、原子层沉积(ALD)、分子层沉积(MLD)、脉冲化学气相沉积(P-CVD)、流动调制化学气相沉积(FM-CVD)。这些技术中的每一种可以通过前体或反应物活化技术辅助，如原位等离子体(“等离子体增强”或PE)、远程等离子体(RP)、热线(HW)和光子(UV)。
家族(1)至(4)的前体可以与共反应物结合使用，该共反应物典型地选自：
-用于沉积含氧化硅膜的O2、O3、H2O、H2O2、HCOOH、CO2、自由基、离子及其混合物
-用于沉积含氮化硅膜的N2，H2，NH3，肼，伯、仲或叔胺，二胺，乙醇胺，自由基，离子及其混合物
家族(1)至(4)的前体可以与另一种金属或类金属挥发性前体结合使用以沉积含硅膜。这种膜的实例包括但不限于SiTiO、SiAlO、SiZrO、SiHfO、SiBO、SiPO、SiAsO、SiBPO、SiGeO、SiBN、SiAlN、SiTiN、CoSiN、NiSiN、TaSiN、WSiN，应当理解该组合物不考虑来自前体和配体的潜在的低水平碳杂质，典型地<5％并且优选<2％。
周期表中几乎每一种元素的多种挥发性前体均已公布并可获得，并且典型地涉及以下配体中的至少一种或配体的组合以获得足够的稳定性和挥发性：氢、卤化物(Cl、Br、I、F)、烷基、烷氧基、二烷基氨基、羰基、环戊二烯基和其他二烯、二氮杂二烯、脒基、硼氢化物、氨基硼烷、异氰酸酯、乙酰氧基、烷基甲硅烷氧基、甲硅烷基、双(三烷基甲硅烷基)酰胺。
具有可水解官能团(如NR1R2、N-C≡N、或-Si-NH-Si)的家族(1)、(2)和(4)的化合物特别适用于基于氧化硅或氮化硅的膜的ALD或PE-ALD，因为它们提供了使前体与表面基板上的羟基(-OH)或-NH2基团反应的反应位点并与其化学键合。它们还具有>3的硅原子数，并且因此与现有分子相比，预计每个周期会产生更高的生长。
所有家族的化合物也特别适用于LPCVD、PECVD和FCVD，因为它们的高硅含量并且接近氮化硅陶瓷前体(pre-ceramic)的结构。
这些化合物具有相当低的蒸气压并且适用于通过冷凝(C-CVD)沉积在基板上(通过将基板保持在低于沉积设备中前体的露点的温度)。然后可以在优选在0℃与900℃之间，更优选在300℃与800℃之间的温度下，通过暴露于氧化气氛(如O2、O3、蒸汽、或H2O2蒸气、其混合物和等离子体)，可能分几个步骤进一步处理热冷凝的组合物，以避免该组合物在基板上的再蒸发，从而将冷凝的硅氮烷组合物转化成二氧化硅膜。这种工艺对于在细沟槽或孔中沉积介电膜(间隙填充)特别有用。
类似地，可以在优选在100℃与1100℃之间，更优选在300℃与900℃之间的温度下将膜暴露于氮化气氛(N2、NH3、肼及其等离子体)，以将短链聚硅氮烷前体转化为大链聚硅氮烷和SiN陶瓷前体。
家族1至4的化合物，并且优选家族1和2的完全不含C的化合物，也可用在用于液相沉积(如旋涂、浸涂或喷涂)的配制品中，或作为合成这种配制品的中间体和成分。作为成分，可以将这些化合物聚合以增加硅氮烷的分子量，用胺或醇官能化以将一些Si-H键转化为更具活性的烷氧基或烷氨基键。它们可以与含有C＝C、C＝N或C＝O不饱和键的化合物反应以通过氢化硅烷化形成Si-C键，优选在催化剂的存在下。它们可以与氨、胺或多胺反应以在Si原子之间产生硅氮烷桥。
实例
以下实例说明结合本文的披露内容进行的实验。该实例不旨在包括所有情况并且并不旨在限制本文所述的披露内容的范围。
在手套箱内，将0.35g(2.7mmol)的(H3Si)2-N-SiH2Cl(TSA-Cl)*与0.39g的戊烷混合。将该混合物加入到在0.5g乙醚中的0.1g(2.4mmol)氰胺(H2N-CN)中。立即出现白色沉淀。将溶液过滤两次。两次最初澄清的滤液都变得浑浊。
推测的反应是2(SiH3)2NSiH2-Cl+4H2N-CN→[(SiH3)2NSiH2]2-NCN+2H2N-CN*HCl
气相色谱(GC)分析表明存在一氯硅烷、乙醚和戊烷、未反应的TSA-Cl、(SiH3)2NSiH2-N-C≡N-SiH3、或[(SiH3)2NSiH2]2-N-C≡N(TSA2-氰胺)。存在许多其他较小的、未鉴别的峰。混合物的GC谱示于图中。本领域普通技术人员将认识到合适的蒸馏塔能够从(H3Si)2-N-SiH2-NCN-SiH3中分离出TSA2-氰胺。
*具有如通过GC测定的初始约85％的纯度。诸位申请人认为图中所示的一氯硅烷是TSA-Cl反应物中的杂质。
尽管已示出且描述了本发明的实施例，但本领域技术人员可在不脱离本发明的精神或传授内容的情况下对其进行修改。本文所述的实施例仅为示例性的且是非限制性的。组合物和方法的许多变化和修改是可能的且在本发明的范围内。因此，保护范围不限于本文所述的实施例，而仅受随后的权利要求书所限定，其范围应包括这些权利要求的主题的所有等效物。
Claims (11)
1.一种形成含硅膜的组合物，其包含选自下组的前体，该组由以下各项组成：
(a)[(SiR3)2NSiH2]m-NH2-m-C≡N，其中m＝1或2；
(b)[(SiR3)2NSiH2]n-NL3-n，其中n＝2或3；
(c)(SiH3)2NSiH2-O-SiH2N(SiH3)2；以及
(d)(SiR’3)2N-SiH2-N(SiR’3)2；
其中
-每个R独立地选自H、具有式-NR1R2的二烷基氨基、或脒基，
-每个R’独立地选自H、具有式-NR1R2的二烷基氨基、或脒基，前提是所有R’都不是H，
-R1和R2独立地选自H或C1-C12烃基，前提是R1和R2不能同时等于H，并且如果R1是H，则R2是C2-C12烃基，并且NR1R2可以一起形成含N杂环配体，并且
-L选自H或C1-C6烃基。
2.如权利要求1所述的形成含硅膜的组合物，其中，该前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NR1R2)、(SiH3)2NSiH2-O-SiH2N(SiH3)2、[(SiH3)2NSiH2]-NH-C≡N、或[(SiH3)2NSiH2]2N-C≡N。
3.如权利要求1所述的形成含硅膜的组合物，其中，该前体是[(SiH3)2NSiH2]2NH或[(SiH3)2NSiH2]3N。
4.如权利要求1所述的形成含硅膜的组合物，其中，该前体是(SiH3)2N-SiH2-N(SiH3)(SiH2NMe2)、(SiH3)2N-SiH2-N(SiH3)(SiH2NEt2)、(SiH3)2N-SiH2-N(SiH3)(SiH2NEtMe)、(SiH3)2N-SiH2-N(SiH3)(SiH2NiPr2)、(SiH3)2N-SiH2-N(SiH3)(SiH2NtBu2)、(SiH3)2N-SiH2-N(SiH3)(SiH2NnBu2)、(SiH3)2N-SiH2-N(SiH3)(SiH2NsecBu2)、或(SiH3)2N-SiH2-N(SiH3)(SiH2NHtBu)。
5.一种通过化学气相沉积法在基板上沉积含硅膜的方法，该方法包括
将包含如权利要求1-4中任一项所述的形成含Si膜的组合物的蒸气引入含有基板的反应器中；
使用化学气相沉积法将该前体的至少一部分沉积到该基板上以在该基板上形成该含硅膜。
6.如权利要求5所述的方法，其中，该化学气相沉积法是原子层沉积工艺或等离子体增强的原子层沉积工艺。
7.如权利要求5或6所述的方法，其中，该含硅膜是氧化硅膜。
8.如权利要求5或6所述的方法，其中，该含硅膜是氮化硅膜。
9.如权利要求5或6所述的方法，其中，该基板是硅晶片。
10.如权利要求5或6所述的方法，其中，该基板是玻璃。
11.如权利要求5或6所述的方法，其中，该基板是有机材料。
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| US20170323783A1 (en) | 2017-11-09 |
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| JP2020507199A (ja) | 2020-03-05 |
| KR102511289B1 (ko) | 2023-03-20 |
| US10192734B2 (en) | 2019-01-29 |
| KR20190093597A (ko) | 2019-08-09 |
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