公开(公告)号：EP3170792B1

公开(公告)日：2020-09-09

申请号：EP15821599.6

申请日：2015-07-14

申请人： Thin Film Electronics ASA

发明人： Goto, Yuichi ,  Nagai, Kentaro ,  Endo, Masahisa ,  Son, Gun

IPC分类号： C01B33/04

公开(公告)号：EP3248940A1

公开(公告)日：2017-11-29

申请号：EP15857977.1

申请日：2015-10-13

申请人： Thin Film Electronics ASA

发明人： GOTO, Yuichi ,  ENDO, Masahisa ,  Son, Gun ,  NAGAI, Kentaro

IPC分类号： C01B33/145 ,  C01B33/12 ,  C08G77/60

CPC分类号： C01B33/113 ,  B01J23/464 ,  C01B33/04 ,  C08G77/60 ,  C09D183/16 ,  H01L21/02107

摘要： [Problem] To provide a method of producing a silicon hydride oxide-containing organic solvent (coating solution) with which a silicon hydride oxide coating film can be formed on a substrate. Using the silicon hydride oxide-containing organic solvent makes it unnecessary to place a coating solution in non-oxidizing atmosphere at the time of coating of the substrate or to perform heat treatment on the substrate after the coating because a silicon hydride oxide is formed in the coating solution before the coating.
[Solution] A method of producing a silicon hydride oxide-containing organic solvent including: blowing an oxygen-containing gas on an organic solvent containing a silicon hydride or a polymer thereof. The silicon hydride is cyclic silane. The silicon hydride is cyclopentasilane. An oxide of the silicon hydride or the polymer thereof is contained at a proportion of (residual Si-H groups)/(Si-H groups before oxidation) = 1 to 40 mol%. The cyclic silane can be obtained by causing the cyclic silane to react with a hydrogen halide in cyclohexane in the presence of an aluminum halide, dissolving the obtained cyclic silane in an organic solvent and reducing it.

摘要翻译： 本发明的目的在于提供一种在基板上形成氢化硅氧化物被膜的含氢氧化硅的有机溶剂（涂布液）的制造方法。 通过使用含有氢氧化硅的有机溶剂，不需要在涂布基板时在非氧化性气氛中涂布涂布液，或者在涂布后在基板上进行热处理，因为氢化硅氧化物在 涂层前的涂层溶液。 [含有氢氧化硅的有机溶剂的制造方法，其特征在于，包括：在含有氢化硅或其聚合物的有机溶剂上吹入含氧气体。 硅氢化物是环状硅烷。 氢化硅是环戊硅烷。 氢化硅或其聚合物的氧化物以（残留Si-H基）/（氧化前的Si-H基）= 1〜40摩尔％的比例含有。 环状硅烷可以通过在卤化铝存在下使环状硅烷与环己烷中的卤化氢反应，将所得到的环状硅烷溶解于有机溶剂中并还原而得到。

公开(公告)号：EP3170792A1

公开(公告)日：2017-05-24

申请号：EP15821599.6

申请日：2015-07-14

申请人： Thin Film Electronics ASA

发明人： Goto, Yuichi ,  Nagai, Kentaro ,  Endo, Masahisa ,  Son, Gun

IPC分类号： C01B33/04

CPC分类号： C01B33/04

摘要： There is provided a cyclic silane having high purity, particularly cyclopentasilane having high purity, and a composition containing a polysilane obtained by polymerization of the cyclic silane which a highly conductive and good silicon thin film is formed by applying the composition in a form of a coating-type polysilane composition to a substrate, followed by baking. A method for producing a cyclic silane of Formula (3):

         (SiH 2 )n      Formula (3)

(wherein n is an integer of 4 to 6)
comprising an (A) step of reacting a cyclic silane compound of Formula (1):

         (SiR 1 R 2 )n      Formula (1)

(wherein R 1 and R 2 are each a hydrogen atom, a C 1-6 alkyl group, or an optionally substituted phenyl group, and n is an integer of 4 to 6) with hydrogen halide in cyclohexane in the presence of aluminum halide to obtain a solution containing a cyclic silane compound of Formula (2):

        ( SiR 3 R 4 ) n      Formula (2)

(wherein R 3 and R 4 are each a halogen atom, and n is an integer of 4 to 6), and then distilling the solution to obtain a cyclic silane compound of Formula (2), and a (B) step of dissolving the cyclic silane compound of Formula (2) in an organic solvent, and reducing the cyclic silane compound of Formula (2) with hydrogen or lithium aluminum hydride. The distillation at the (A) step may be carried out at a temperature of 40 to 80°C under a reduced pressure of 0 to 30 Torr.

摘要翻译： 提供了一种高纯度的环状硅烷，特别是高纯度的环戊硅烷，以及一种含有通过聚合该环状硅烷得到的聚硅烷的组合物，该组合物通过以涂层形式涂布该组合物形成高导电性和良好的硅薄膜 型聚硅烷组合物涂布到基材上，随后进行烘烤。 （3）的环状硅烷的制造方法：（SiH 2）n式（3）（式中，n为4〜6的整数）包含使式（1）的环状硅烷化合物与式 （SiR 1 R 2）n其中R 1和R 2各自为氢原子，C 1-6烷基或任选取代的苯基，且n为4-6的整数）与环己烷中的卤化氢 得到含有式（2）的环状硅烷化合物的溶液：式（2）（SiR 3 R 4）n（式中，R 3和R 4分别为卤原子，n为4〜6的整数） 然后蒸馏该溶液以获得式（2）的环状硅烷化合物，和（B）将式（2）的环状硅烷化合物溶解在有机溶剂中并且用式 氢或氢化铝锂。 （A）工序中的蒸馏可以在40〜80℃的温度，0〜30Torr的减压下进行。