CN105307977A - 包含氢化硅烷和氢化硅烷低聚物的配制品、其制备方法及其用途 - Google Patents
包含氢化硅烷和氢化硅烷低聚物的配制品、其制备方法及其用途 Download PDFInfo
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- CN105307977A CN105307977A CN201480034636.6A CN201480034636A CN105307977A CN 105307977 A CN105307977 A CN 105307977A CN 201480034636 A CN201480034636 A CN 201480034636A CN 105307977 A CN105307977 A CN 105307977A
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- hydrosilanes
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- oligopolymer
- silane
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Classifications
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- 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
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-
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
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- 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
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- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic System
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1864—Annealing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/547—Monocrystalline silicon PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明涉及包含至少一种通式为SinH2n+2,其中n=7-10的氢化硅烷和至少一种氢化硅烷低聚物的配制品,涉及其制备方法及其用途。
Description
本发明涉及包含至少一种低分子量氢化硅烷和至少一种氢化硅烷低聚物的配制品,涉及其制备方法及其用途,尤其是用于制造含硅层的用途。
氢化硅烷或其低聚物在文献中已被描述为用于制造含硅层的可能的反应物。
在此,氢化硅烷被理解为是指基本仅含硅和氢原子并具有少于20个硅原子的化合物。氢化硅烷原则上可以是气体、固体或液体并 - 尤其在固体的情况下 - 基本可溶于溶剂,如甲苯或环己烷中或可溶于液体硅烷,如环戊硅烷中。实例包括单硅烷、二硅烷、三硅烷、环戊硅烷和新戊硅烷。具有至少三个或四个硅原子的氢化硅烷可具有含Si-H键的直链、支链或环状(任选双环/多环)结构并可优选由各自的通式SinH2n+2(直链或支链;其中n = 2-20)、SinH2n(环状;其中n = 3 - 20)或SinH2(n-i)(双环或多环;n = 4-20;i = {环数} – 1)描述。
例如在US 6,027,705 A中公开了制备具有至少3个硅原子的氢化硅烷的方法。WO 2011/104147 A1公开了用于制备氢化硅烷的低聚物的热法。此外,WO
2012/041837 A2公开了制备更高级的氢化硅烷化合物的方法,其中在至少500 g/mol的氢化硅烷聚合物存在下热转化低级氢化硅烷化合物。
可以在真空室中例如通过PECVD由气相沉积含硅层。但是,气相法在技术上复杂并通常没有产生所需品质的层。因此,液相法通常优选用于制造含硅层。
现有技术描述了各种含氢化硅烷的配制品。例如,US 5,866,471 A公开了含有半导体前体的配制品,可用其制造半导体层。可用的半导体前体还包括氢化硅烷。WO 2008/137811
A2也公开了含有选自一组并包括(聚)硅烷的一种或多种半导体前体的组合物。US 2009/0215219 A1也公开了一种制造半导体层的方法,其中将含硅原子的液体涂料组合物施加到基底上。该涂料组合物可含有硅烷聚合物,其可以是聚氢化硅烷。US
2010/0197102 A1公开了含有优选为具有4至9个硅原子的硅烷的化合物的溶液。在EP 1
357 154 A1中也描述了含有聚硅烷的涂料组合物。EP 1 640 342 A1进一步公开了具有800至5000 g/mol的重均分子量的硅烷聚合物,其可用于制造含硅薄膜。JP 2008-270603 A和JP 09-45922 A也公开了用于制造含硅薄膜的涂料组合物,其中可以使用各种硅化合物作为前体。在提及的文献中没有公开各种氢化硅烷前体的混合物。
JP
2004-134440 A公开了用于制造含硅薄膜的涂料组合物,其含有各种硅烷化合物和环状硅烷。EP 1
085 579 A1和EP 1 087 428 A1也公开了用于制造含硅层的涂料组合物,其中使用两种硅前体。这些是环状硅化合物和掺杂的硅化合物。JP 2000-031066 A公开了含有通式SinH2n+2或SinH2n的氢化硅烷或两者的混合物的液体涂料组合物。DE 10 2010 030 696 A1同样公开了可能具有氢化硅烷作为硅前体的液体涂料组合物。
仅含低分子量氢化硅烷作为硅前体的涂料组合物在含硅层的制造中具有缺点。它们尤其不适用于制造极薄含硅层(厚度最多25纳米的层),因为该低分子量材料在典型转化温度下在可交联之前汽化。因此,通常使用含有高分子量氢化硅烷低聚物的涂料组合物。这些高分子量氢化硅烷低聚物原则上适用于制造含硅层,但它们具有在有机溶剂中仅微溶的缺点,这导致用其制成的层的缺点。因此,在现有技术中存在除了高分子量氢化硅烷低聚物之外还具有低分子量氢化硅烷的涂料组合物,其中后者充当助溶剂。
现有技术中描述了含有与环状氢化硅烷混合的氢化硅烷低聚物的用于制造含硅层的涂料组合物(Masuda等人, Thin Solid Films 520 (2012) 5091-5096)。但是,含有环状氢化硅烷的相应涂料组合物的缺点在于它们仅在环状氢化硅烷的高浓度下稳定。在环状氢化硅烷的低浓度下,该配制品快速变浑浊并随之不适用于制造高品质含硅层。
还已经发现,具有3-6个硅原子的低级氢化硅烷,尤其是式SinH2n+2的那些,在包含氢化硅烷低聚物的配制品中具有在转化时不构建在该层状复合物中的缺点。因此,在使用相应的涂料组合物时,基于所有含硅前体计的收率是不利的。
本发明的目的因此是提供适用于制造克服了现有技术中的缺点的含硅层的涂料组合物。本发明的目的具体是,提供稳定的涂料组合物,该组合物除氢化硅烷低聚物外,只需要小比例的其它组分。此外,所述其它组分也应以好的收率构建在该层状复合物中。
在本文中通过包含至少一种氢化硅烷和至少一种氢化硅烷低聚物的本发明的配制品实现所述目的,其中该氢化硅烷具有通式SinH2n+2,其中n = 7至10。相应的配制品不仅实现了本发明的目的,而且尤其适用于由液相制造具有至少25纳米的厚度,尤其具有50-1000纳米的厚度的高品质厚层,并在涂覆工艺中良好润湿常用的基底。
本文中要求保护的配制品是包含至少一种氢化硅烷和至少一种氢化硅烷低聚物或由这两者的混合物构成的组合物。该配制品优选是液体,因为其因此可以特别有效地操作。此外,本发明的配制品优选是涂料组合物,尤其用于液相或CVD沉积法。相应的涂料组合物具有适用于沉积含硅层,尤其是用于所提到的方法的优点。本发明的组合物最优选是适用于液相沉积法的涂料组合物。
式SinH2n+2 的氢化硅烷,其中n = 7-10,是非环状氢化硅烷。该化合物的异构体可为直链或支链的。优选的非环状氢化硅烷是八硅烷 (即,正八硅烷、2-甲硅烷基七硅烷、3-甲硅烷基七硅烷、4-甲硅烷基七硅烷、2,2-二甲硅烷基六硅烷、2,3-二甲硅烷基六硅烷、2,4-二甲硅烷基六硅烷、2,5-二甲硅烷基六硅烷、3,4-二甲硅烷基六硅烷、2,2,3-三甲硅烷基五硅烷、2,3,4-三甲硅烷基五硅烷、2,3,3-三甲硅烷基五硅烷、2,2,4-三甲硅烷基五硅烷、2,2,3,3-四甲硅烷基四硅烷、3-二甲硅烷基六硅烷、2-甲硅烷基-3-二甲硅烷基五硅烷和3-甲硅烷基-3-二甲硅烷基五硅烷)和九硅烷(即,正九硅烷、2-甲硅烷基八硅烷、3-甲硅烷基八硅烷、4-甲硅烷基八硅烷、2,2-二甲硅烷基七硅烷、2,3-二甲硅烷基七硅烷、2,4-二甲硅烷基七硅烷、2,5-二甲硅烷基七硅烷、2,6-二甲硅烷基七硅烷、3,3-二甲硅烷基七硅烷、3,4-二甲硅烷基七硅烷、3,5-二甲硅烷基七硅烷、4,4-二甲硅烷基七硅烷、3-二甲硅烷基七硅烷、4-二甲硅烷基七硅烷、2,2,3-三甲硅烷基六硅烷、2,2,4-三甲硅烷基六硅烷、2,2,5-三甲硅烷基六硅烷、2,3,3-三甲硅烷基六硅烷、2,3,4-三甲硅烷基六硅烷、2,3,5-三甲硅烷基六硅烷、3,3,4-三甲硅烷基六硅烷、3,3,5-三甲硅烷基六硅烷、3-二甲硅烷基-2-甲硅烷基六硅烷、4-二甲硅烷基-2-甲硅烷基六硅烷、3-二甲硅烷基-3-甲硅烷基六硅烷、4-二甲硅烷基-3-甲硅烷基六硅烷、2,2,3,3-四甲硅烷基五硅烷、2,2,3,4-四甲硅烷基五硅烷、2,2,4,4-四甲硅烷基五硅烷、2,3,3,4-四甲硅烷基五硅烷、3-二甲硅烷基-2,2-二甲硅烷基五硅烷、3-二甲硅烷基-2,3-二甲硅烷基五硅烷、3-二甲硅烷基-2,4-二甲硅烷基五硅烷和3,3-二甲硅烷基五硅烷),它们的配制品产生特别好的结果。所述通式的氢化硅烷同样优选是支化的氢化硅烷,其产生比线性氢化硅烷更稳定的溶液和更好的层。该氢化硅烷非常特别优选是九硅烷异构体的混合物,其可通过热处理新戊硅烷或根据由Holthausen等人描写的准则(展示报告: A. Nadj, 6th
European Silicon Days, 2012)来制备。用相应的配制品可获得最好的结果。
该氢化硅烷低聚物是氢化硅烷化合物的低聚物,并优选是氢化硅烷的低聚物。当该氢化硅烷低聚物具有200至10 000 g/ml的重均分子量时,本发明的配制品特别适用于制造含硅层。其制备方法是本领域技术人员已知的。可以通过凝胶渗透色谱法使用线性聚苯乙烯柱用环辛烷作为洗脱剂对照作为标样的聚丁二烯测定相应的分子量。
优选通过非环状氢化硅烷的低聚获得该氢化硅烷低聚物。不同于由环状氢化硅烷形成的氢化硅烷低聚物,这些低聚物由于进程不同的离解聚合机制而具有高交联比例。相反,由于环状氢化硅烷经受的开环反应机制,由环状氢化硅烷形成的低聚物只有极低的交联比例(如果有的话)。不同于由环状氢化硅烷形成的低聚物,由非环状氢化硅烷制成的相应低聚物使得基底表面在溶液中良好润湿,可以特别有效地用于制造薄层并产生均匀和光滑的表面。由非环状支化氢化硅烷形成的低聚物表现出更好的结果。
一种特别优选的氢化硅烷低聚物是可通过包含至少一种具有最多20个硅原子的非环状氢化硅烷的组合物在没有催化剂的情况下在<235℃的温度下的热转化获得的低聚物。在WO 2011/104147 A1中描述了相应的氢化硅烷低聚物及其制备,其关于该化合物及其制备的内容经此引用并入本文。这种低聚物具有比由非环状支化氢化硅烷形成的其它氢化硅烷低聚物更好的性质。
该氢化硅烷低聚物还可具有除氢和硅以外的其它残基。因此,当该低聚物含有碳时,可能产生用该配制品制成的层的优点。可以通过氢化硅烷与烃的共低聚来制备相应的含碳氢化硅烷低聚物。但是,该氢化硅烷低聚物优选是只含氢和硅的化合物,因此其没有卤素或烷基。
为了制备掺杂含硅层,此外优选掺杂的氢化硅烷低聚物。该氢化硅烷低聚物优选是硼-或磷-掺杂的且相应的配制品适用于制造p-或n-掺杂的硅层。相应的氢化硅烷低聚物可通过在其制备期间就已添加相应的掺杂剂来制备。或者,也可以借助高能法(例如紫外线照射或热处理)用选自p掺杂剂的物质,优选硼氢化试剂(尤其是B2H6、BH3*THF、BEt3、BMe3)p掺杂已制成的未掺杂氢化硅烷低聚物,或用n掺杂剂(尤其是PH3、P4)n掺杂它们。
基于该配制品的总质量计,一种或多种氢化硅烷的比例优选为0.1至99重量%,更优选1至40重量%,非常特别优选1至30重量%。
基于该配制品的总质量计,一种或多种氢化硅烷低聚物的比例优选为0.1至99重量%,更优选1至60重量%,非常特别优选1至40重量%。
基于存在的氢化硅烷和氢化硅烷低聚物的总质量计,为了实现特别好的结果,该配制品中的氢化硅烷低聚物比例优选为40-99.9重量%,更优选60-99重量%,非常特别60-80重量%。该氢化硅烷低聚物的比例还更优选为60-低于70重量%,基于存在的氢化硅烷和氢化硅烷低聚物的总质量计。该氢化硅烷低聚物的比例同样更优选为70-80重量%,基于存在的氢化硅烷和氢化硅烷低聚物的总质量计。
在60重量%以下,可能产生不均匀的、粗糙的层。此外,相应的配制品可能造成问题,因为其可能太稀并在涂覆过程中展现出润湿问题。尽管通常可以通过改变溶剂比例和溶剂组成消除这一问题,但这是昂贵和不便的。
在80重量%以上,可能产生不均匀、不完整或结成块的层,且该膜在涂覆工艺中断裂。此外,在该层中形成缺陷(“彗星”)。
因此,在该配制品中氢化硅烷低聚物的最佳比例是60-80重量%,基于存在的氢化硅烷和氢化硅烷低聚物的总质量计。
本发明的配制品不需要含有任何溶剂。但是,其优选具有至少一种溶剂。如果其含有溶剂,则基于该配制品的总质量计,其比例优选为0.1至99重量%,更优选25至95重量%,非常特别优选60至95重量%。
非常特别优选的是基于该配制品的总质量计,具有1-30重量%的氢化硅烷、10-40重量%的氢化硅烷低聚物和50-85重量%的溶剂的配制品,用此可获得最好的结果。
优选可用的溶剂是选自具有1至12个碳原子的直链、支链或环状的、饱和、不饱和或芳族的烃(任选部分或完全卤化)、醇、醚、羧酸、酯、腈、胺、酰胺、亚砜和水的那些。特别优选的是正戊烷、正己烷、正庚烷、正辛烷、正癸烷、十二烷、环己烷、环辛烷、环癸烷、二环戊烷、苯、甲苯、间二甲苯、对二甲苯、均三甲苯、二氢化茚、茚、四氢化萘、十氢化萘、二乙醚、二丙醚、乙二醇二甲醚、乙二醇二乙醚、乙二醇甲基乙基醚、二乙二醇二甲醚、二乙二醇二乙醚、二乙二醇甲基乙基醚、四氢呋喃、p-二氧杂环己烷、乙腈、二甲基甲酰胺、二甲亚砜、二氯甲烷和氯仿。
此外,本发明的配制品除所述至少一种氢化硅烷和所述至少一种氢化硅烷低聚物和一种或多种任选存在的任何溶剂之外还可包含其它物质,尤其是掺杂剂(优选B2H6、BH3*THF、BEt3、BMe3、PH3、P4)、纳米颗粒或用于调节流变性质的添加剂。相应的物质是本领域技术人员已知的。
本发明还提供一种制造本发明的配制品的方法,其中将通式SinH2n+2的氢化硅烷(其中n = 7-10)与氢化硅烷低聚物和任选的溶剂混合。
本发明还提供一种制造含硅层的方法,其中将本发明的配制品,尤其是涂料组合物从气相或液相施加到未涂覆或预涂覆的基底上,并热转化和/或借助电磁辐射转化成含硅层。
许多基底可以用于本发明的方法。优选的是由玻璃、石英玻璃、石墨、金属、硅构成或由存在于耐热载体上的硅、氧化铟锡、ZnO:F、ZnO:Al或SnO2:F的层构成的基底。优选的金属是铝、不锈钢、Cr-钢、钛、铬或钼。此外,在选择合适的转化条件下,也可以使用塑料膜(例如PEEK、PEN、PET或聚酰亚胺)。
该配制品的施加优选经由选自印刷法(尤其是柔性版/凹版印刷、纳米压印或微米压印、喷墨印刷、胶版印刷、反向胶版印刷、数字胶版印刷和丝网印刷)、喷涂法、气溶胶辅助的化学气相沉积、直接液体注射化学气相沉积、旋涂法、浸涂法的气相或液相涂覆法和选自弯月面涂覆(Meniscus
Coating)、狭缝涂覆、狭缝-模头涂覆和幕涂的方法进行。在上文提到的方法中,气溶胶辅助的化学气相沉积和直接液体注射化学气相沉积应包括在气相法中。优选经由液相涂覆法施加。
在施加该配制品后,优选可经由基底上的液体薄膜的紫外线照射进行预交联,此后仍为液体的薄膜具有交联的前体成分。
此外,在该配制品的施加和任选的预交联后,经涂覆的基底可优选在转化前干燥,以除去任选存在的溶剂。用于此用途的相应措施和条件是本领域技术人员已知的。为了仅除去挥发性配制品成分,在热干燥的情况中,加热温度应小于200℃。
本发明的方法中的热转化优选在200-1000℃,优选250-750℃,尤其优选300-700℃的温度下进行。热转化时间优选为0.1毫秒至360分钟。该转化时间更优选为0.1毫秒至10分钟,尤其优选1秒至120秒。
例如,可以通过使用红外灯、热板、烘箱、闪光灯、具有合适气体组成的等离子体、RTP装置、微波装置或电子束处理(如果需要,在各自的预热或温热状态下)进行相应的快速高能法。
备选或补充地,可以通过用电磁辐射,尤其用紫外线照射实现转化。转化时间可优选为1秒至360分钟。
此外,在转化过程中或在转化后,可以优选进行含硅层的氢富集。这被称作“氢钝化”,其消除材料中的缺陷并可以例如用反应性氢通过热丝法、用含氢等离子体(远程或直接;在真空中或在大气压下)或借助在供氢下的电晕处理或电子束处理进行。此外,也可以在富氢气氛中进行已提到的干燥和/或转化步骤,以使该材料从一开始就富氢。
为了制造含氧化硅的层,也可以在氧化条件下进行施加、预交联、干燥和/或转化。怎样能建立氧化条件是本领域技术人员已知的。
为了制造完全或部分结晶的含硅层,可以在转化后通过引入热能、电磁辐射和/或粒子轰击使该层结晶。用于此用途的方法是本领域技术人员已知的。
所述用于制造含硅层的方法也可以基于基底同时进行或按时间顺序依次进行多次(同时或相继沉积,在这种情况下所得薄膜部分或完全叠置)。这种制造多层系统的方法优选适用于制造例如太阳能电池所必需的由本征(即未掺杂)的层和掺杂层构成的系统。在基底上施加薄本征(即未掺杂)含硅层,然后施加与基底相反的掺杂层时,该方法特别优选适用于制造用于最佳钝化或避免与基底的界面处的缺陷的多层系统。在这种情况中,因此首先在掺杂基底上施加基本无掺杂剂的配制品,然后在其上施加具有与基底相反的掺杂剂的配制品。此外,该基底可以在两面都被涂覆。
可根据本发明制造的氢化硅烷配制品适合多种用途。它们特别适用于 - 独自或与其它配制品一起 - 制造电子或光电部件层。本发明因此还提供本发明的氢化硅烷配制品用于制造光电或电子部件层的用途。本发明还提供本发明的氢化硅烷配制品用于制造电子和光电部件的用途。可通过本发明的方法获得的氢化硅烷配制品优选适用于制造光电或电子部件中的电荷传输部件。可通过本发明的方法获得的氢化硅烷配制品此外适用于制造含硅层。
本发明的配制品和本发明的方法特别适用于制造下列层或部件:
- 异质发射(Heteroemitter)太阳能电池
- HIT(具有固有薄层的异质结)太阳能电池
- 选择性发射极太阳能电池
- 背接触太阳能电池
- 场效应晶体管、薄层晶体管
- 微电子部件中的介电层
- 半导体材料的表面钝化
- 含有量子点的层和部件的制造
- 防止成分从环境中透过层扩散的屏障,
- 用于层的上侧和下侧的热解耦的屏障层。
实施例:
实施例 1
将0.21 g 九硅烷、0.29
g 由新戊硅烷形成的氢化硅烷低聚物 (相当于58重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~ 2200 g/mol)、0.37 g 环辛烷和0.87 g 甲苯的混合物在3000转/min、6000转/min和9000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所得层厚度为48-74 nm。
由附图1可知,相对稀的涂料组合物原则上适用于半导体用途。但是,由那里示出的照片和显微图像可知,所产生的涂层较不均匀且粗糙。
实施例 2
将0.25 g 由新戊硅烷形成的未掺杂氢化硅烷低聚物 (相当于62.5重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计)
(Mw ~2300 g)和0.150 g 九硅烷在0.180 g 环辛烷和0.420 g 甲苯中的混合物在6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度为113 nm。
所产生的层是均匀而光滑的。
实施例 3
将0.17 g 九硅烷、0.33
g 由新戊硅烷形成的氢化硅烷低聚物 (相当于66重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~ 2200 g/mol)、0.87 g 甲苯和0.37 g 环辛烷在3000转/min、6000转/min和9000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度在66-104 nm的范围。
如由图2的照片和显微图像可知,所产生的层是均匀而光滑的。
实施例 4
将0.13 g 九硅烷、0.37
g 由新戊硅烷形成的氢化硅烷低聚物 (相当于74重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~ 2200 g/mol)、0.87 g 甲苯和0.37
g 环辛烷的混合物在3000转/min、6000转/min和9000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度在90-140 nm的范围。
如由图3的照片和显微图像可知,所产生的层是均匀而光滑的。
实施例 5
将0.25 g 由新戊硅烷形成的未掺杂氢化硅烷低聚物 (相当于76.9重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~2300 g)和0.075 g 九硅烷在0.158 g 环辛烷和0.368 g 甲苯中的混合物在6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度为130 nm。
所产生的层是均匀而光滑的。
实施例 6
将0.08 g 九硅烷、 0.42
g 由新戊硅烷形成的氢化硅烷低聚物 (84重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~ 2000 g/mol)、0.24 g 环辛烷和0.96
g 甲苯的混合物在4500转/min和6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度分别为164 nm和150 nm。
由附图4可知,相对稀的涂料组合物原则上适用于半导体用途。但是,由那里示出的照片和显微图像可知,所产生的涂层较不均匀且不完整并结成块。此外,可看出层中的缺陷。
对比例1
将0.25 g 由新戊硅烷形成的未掺杂氢化硅烷低聚物 (Mw ~2300 g)在0.203 g 环辛烷和0.472
g 甲苯中的混合物在6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度为102 nm。但是,但是,所产生的层有缺点。
对比例2
将0.25 g 由新戊硅烷形成的未掺杂氢化硅烷低聚物 (Mw ~2300 g)和0.150 g 新戊硅烷在0.180
g 环辛烷和0.420 g 甲苯中的混合物在6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的层厚度为99 nm。因此,与共混有通式为SinH2n+2 (其中n = 7-10)的氢化硅烷时相比,该收率不佳。
对比例3
将0.27 g 九硅烷、0.03
g 由新戊硅烷形成的氢化硅烷低聚物 (10重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计) (Mw ~ 2200 g/mol)和0.30 g 甲苯的混合物在1000转/min、2000转/min、3000转/min和6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的涂层不均匀、不完整(nicht flächendeckend)且有许多缺陷。
对比例4
将
0.27 g 九硅烷、0.03
g 由新戊硅烷形成的氢化硅烷低聚物 (10重量%,基于氢化硅烷和氢化硅烷低聚物的总质量计)(Mw ~ 2200 g/mol)、0.48 g 甲苯和0.20 g 环辛烷的混合物在1000转/min、2000转/min、3000转/min和6000转/min下涂覆在EagleXG玻璃上,然后在500℃/60 s下转化。所产生的涂层不均匀、不完整且有许多缺陷。
Claims (18)
1.配制品,其包含至少一种氢化硅烷和至少一种氢化硅烷低聚物,
其特征在于
所述氢化硅烷具有通式SinH2n+2,其中n = 7-10。
2.根据权利要求1的配制品,
其特征在于
所述氢化硅烷是八硅烷异构体或九硅烷异构体。
3.根据权利要求1或2的配制品,
其特征在于
所述氢化硅烷是支化的氢化硅烷。
4.根据前述权利要求任一项的配制品,
其特征在于
所述氢化硅烷低聚物具有200至10 000 g/mol的重均分子量。
5.根据前述权利要求任一项的配制品,
其特征在于
所述氢化硅烷低聚物通过非环状氢化硅烷的低聚获得。
6.根据权利要求5的配制品,
其特征在于
所述氢化硅烷低聚物可在没有催化剂的情况下在小于235℃的温度下通过热转化包含至少一种具有最多20个硅原子的非环状氢化硅烷的组合物获得。
7.根据前述权利要求任一项的配制品,
其特征在于
所述氢化硅烷低聚物含有碳。
8.根据前述权利要求任一项的配制品,
其特征在于
所述氢化硅烷低聚物是掺杂的。
9.根据前述权利要求任一项的配制品,
其特征在于
所述至少一种氢化硅烷的比例为基于所述配制品的总质量计1至40重量%。
10.根据前述权利要求任一项的配制品,
其特征在于
所述至少一种氢化硅烷低聚物的比例为基于所述配制品的总质量计1至60重量%。
11.根据前述权利要求任一项的配制品,
其特征在于
基于存在的氢化硅烷低聚物和氢化硅烷低聚物的总质量计,所述氢化硅烷低聚物的比例为40-99.9重量%,优选60-99重量%,特别优选60-80重量%。
12.根据前述权利要求任一项的配制品,
其特征在于
其具有至少一种溶剂。
13.根据权利要求12的配制品,
其特征在于
所述溶剂的比例为基于所述配制品的总质量计25至95重量%。
14.根据权利要求12或13的配制品,
其特征在于
基于所述配制品的总质量计,其具有1-30重量%的氢化硅烷、1-40重量%的氢化硅烷低聚物和50-85重量%的溶剂。
15.制备根据前述权利要求任一项的配制品的方法,其中将通式SinH2n+2的氢化硅烷与氢化硅烷低聚物和任选的溶剂混合,其中n = 7-10。
16.根据权利要求1至14任一项的配制品用于制造含硅层的用途。
17.根据权利要求1至14任一项的配制品用于制造电子层或光电层的用途。
18.根据权利要求1至14任一项的配制品用于制造电子部件或光电部件的用途。
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CN112839902A (zh) * | 2018-10-11 | 2021-05-25 | 乔治洛德方法研究和开发液化空气有限公司 | 用于生产富含异构体的高级硅烷的方法 |
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JP6410807B2 (ja) | 2018-10-24 |
DE102013010101A1 (de) | 2014-12-18 |
US20160145440A1 (en) | 2016-05-26 |
US10385217B2 (en) | 2019-08-20 |
CN105307977B (zh) | 2018-09-14 |
KR20160021121A (ko) | 2016-02-24 |
EP3010854A1 (de) | 2016-04-27 |
TW201518209A (zh) | 2015-05-16 |
WO2014202453A1 (de) | 2014-12-24 |
JP2016522153A (ja) | 2016-07-28 |
EP3010854B1 (de) | 2018-09-05 |
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