U.S. patent application number 14/342834 was filed with the patent office on 2014-08-07 for film deposition material, sealing film using the same and use thereof.
This patent application is currently assigned to TOSOH CORPORATION. The applicant listed for this patent is Daiji Hara, Masato Shimizu. Invention is credited to Daiji Hara, Masato Shimizu.
Application Number | 20140219903 14/342834 |
Document ID | / |
Family ID | 47832008 |
Filed Date | 2014-08-07 |
United States Patent
Application |
20140219903 |
Kind Code |
A1 |
Hara; Daiji ; et
al. |
August 7, 2014 |
FILM DEPOSITION MATERIAL, SEALING FILM USING THE SAME AND USE
THEREOF
Abstract
The present invention relates to a film composed of a
carbon-containing silicon oxide formed by CVD using, as the raw
material, an organosilicon compound having a secondary hydrocarbon
group directly bonded to at least one silicon atom and having an
atomic ratio of 0.5 or less oxygen atom with respect to 1 silicon
atom, which is used as a sealing film for a gas barrier equipment
and materials, an FPD device, a semiconductor device and the
like.
Inventors: |
Hara; Daiji; (Kanagawa,
JP) ; Shimizu; Masato; (Kanagawa, JP) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Hara; Daiji
Shimizu; Masato |
Kanagawa
Kanagawa |
|
JP
JP |
|
|
Assignee: |
TOSOH CORPORATION
Shunan-shi, Yamaguchi
JP
|
Family ID: |
47832008 |
Appl. No.: |
14/342834 |
Filed: |
August 24, 2012 |
PCT Filed: |
August 24, 2012 |
PCT NO: |
PCT/JP2012/071487 |
371 Date: |
March 5, 2014 |
Current U.S.
Class: |
423/325 ;
556/430; 556/453; 556/465 |
Current CPC
Class: |
H01L 21/02216 20130101;
C23C 16/401 20130101; C23C 16/50 20130101; H01L 21/02211 20130101;
H01L 21/02126 20130101; C23C 16/30 20130101; H01L 21/02274
20130101 |
Class at
Publication: |
423/325 ;
556/453; 556/465; 556/430 |
International
Class: |
C23C 16/30 20060101
C23C016/30 |
Foreign Application Data
Date |
Code |
Application Number |
Sep 5, 2011 |
JP |
2011-192741 |
Claims
1. A film deposition material for a chemical vapor deposition
method, comprising: an organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom.
2. The film deposition material according to claim 1, wherein the
organosilicon compound having a secondary hydrocarbon group
directly bonded to at least one silicon atom and having an atomic
ratio of 0.5 or less oxygen atom with respect to 1 silicon atom is
a disiloxane compound represented by the following formula (1):
##STR00012## wherein each of R.sup.1 and R.sup.2 represents a
hydrocarbon group having a carbon number of 1 to 20; R.sup.1 and
R.sup.2 may bond with each other to form a cyclic structure; and
each of R.sup.3 and R.sup.4 represents a hydrocarbon group having a
carbon number of 1 to 20 or a hydrogen atom.
3. The film deposition material according to claim 1, wherein the
organosilicon compound having a secondary hydrocarbon group
directly bonded to at least one silicon atom and having an atomic
ratio of 0.5 or less oxygen atom with respect to 1 silicon atom is
a silane compound represented by the following formula (2):
##STR00013## wherein each of R.sup.5 and R.sup.6 represents a
hydrocarbon group having a carbon number of 1 to 20; R.sup.5 and
R.sup.6 may bond with each other to form a cyclic structure; each
of R.sup.7, R.sup.8 and R.sup.9 represents a hydrocarbon group
having a carbon number of 1 to 20 or a hydrogen atom; and m
represents an integer of 1 to 20.
4. The film deposition material according to claim 1, wherein the
organosilicon compound having a secondary hydrocarbon group
directly bonded to at least one silicon atom and having an atomic
ratio of 0.5 or less oxygen atom with respect to 1 silicon atom is
a cyclic silane compound represented by the following formula (3):
##STR00014## wherein each of R.sup.10 and R.sup.11 represents a
hydrocarbon group having a carbon number of 1 to 20; R.sup.10 and
R.sup.11 may bond with each other to form a cyclic structure;
R.sup.12 represents a hydrocarbon group having a carbon number of 1
to 20 or a hydrogen atom; and n represents an integer of 4 to
40.
5. The film deposition material according to claim 2, wherein in
formula (1), (2) or (3), both R.sup.1 and R.sup.2, both R.sup.5 and
R.sup.6 or both R.sup.10 and R.sup.11 are methyl or are methyl and
ethyl, respectively.
6. The film deposition material according to claim 2, wherein the
organosilicon compound is 1,3-diisopropyldisiloxane,
1,3-diisopropyl-1,3-dimethyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetramethyldisiloxane,
1,3-di-sec-butyldisiloxane, 1,3-di-sec-butyl-1,3-dimethyldisiloxane
or 1,3-di-sec-butyl-1,1,3,3-tetramethyldisiloxane.
7. The film deposition material according to claim 3, wherein the
organosilicon compound is isopropylsilane, isopropylmethylsilane,
isopropyldimethylsilane, diisopropylsilane,
diisopropylmethylsilane, triisopropylsilane, sec-butylsilane,
sec-butylmethylsilane, sec-butyldimethylsilane, di-sec-butylsilane,
di-sec-butylmethylsilane or tri-sec-butylsilane.
8. The film deposition material according to claim 4, wherein the
organosilicon compound is 1,2,3,4-tetraisopropylcyclotetrasilane,
1,2,3,4,5-pentaisopropylcyclopentasilane,
1,2,3,4,5,6-hexaisopropylcyclohexasilane,
1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decaisopropylcyclopentasilane or
1,1,2,2,3,3,4,4,5,5,6,6-undecaisopropylcyclohexasilane.
9. The film deposition material according to claim 1, wherein the
chemical vapor deposition method is a plasma enhanced chemical
vapor deposition method.
10. The film deposition material according to claim 1, wherein the
chemical vapor deposition method is a catalytic chemical vapor
deposition method.
11. A sealing film, deposited by a chemical vapor deposition method
using the film deposition material according to claim 1.
12. A sealing film, obtained by further subjecting the sealing film
according to claim 11 to a heat treatment, an ultraviolet
irradiation treatment or an electron beam treatment.
13. A gas barrier equipment and materials, using the sealing film
according to claim 11 as a gas barrier layer.
14. A flat-panel display device, comprising: the sealing film
according to claim 11.
15. A semiconductor device, comprising: the sealing film according
to claim 11.
16. The film deposition material according to claim 3, wherein in
formula (1), (2) or (3), both R.sup.1 and R.sup.2, both R.sup.5 and
R.sup.6 or both R.sup.10 and R.sup.11 are methyl or are methyl and
ethyl, respectively.
17. The film deposition material according to claim 4, wherein in
formula (1), (2) or (3), both R.sup.1 and R.sup.2, both R.sup.5 and
R.sup.6 or both R.sup.10 and R.sup.11 are methyl or are methyl and
ethyl, respectively.
Description
TECHNICAL FIELD
[0001] The present invention relates to a film deposition material,
a sealing film using the same, and use thereof. More specifically,
the present invention relates to a sealing film composed of a
carbon-containing silicon oxide film obtained through deposition by
a chemical vapor deposition method (CVD: Chemical Vapor Deposition)
using, as the raw material, a hydrocarbon-substituted silicon
compound having a specific structure.
BACKGROUND ART
[0002] In a flat-panel display (hereinafter, referred to as FPD)
represented by a liquid crystal display and an organic EL display,
a glass substrate is used as the base material of its display
panel, but in view of thickness reduction, weight reduction,
enhancement of impact resistance and flexibility as well as
adaptability to a roll-to-roll process, the demand for replacement
by a transparent plastic film is increasing. Also, attempts are
being made to form an organic transistor on a plastic substrate by
using an organic semiconductor or to form LSI, an Si thin-film
solar cell, an organic dye-sensitized solar cell, an organic
semiconductor solar cell and the like.
[0003] Usually, in the case of forming the above-described device
on a commercially available plastic substrate, the device or device
formed, such as liquid crystal device, organic EL device, TFT
device, semiconductor device and solar cell, is weak to water
and/or oxygen and therefore, a dark spot or a dot dropout may be
generated during displaying on the display, or a semiconductor
device, a solar cell and the like may be prevented from fulfilling
their function and cannot withstand the practical use. Accordingly,
a gas barrier plastic substrate with a gas barrier performance
against water vapor and/or oxygen gas is required. On the other
hand, instead of an opaque aluminum foil laminate film, a
transparent plastic film provided with a gas barrier performance is
hereafter more and more expanding its use in the application as a
packaging material for food, medicines, electronic materials,
electronic components and the like.
[0004] The method for providing a transparent gas barrier
performance to a transparent plastic substrate or a transparent
plastic film includes a physical film deposition method and a CVD
method. Patent Document 1 has proposed a barrier bag film where a
gas barrier layer is formed by a plasma enhanced chemical vapor
deposition method (PECVD; Plasma Enhanced Chemical Vapor
Deposition) using, as the raw material, a mixed gas of
hexamethyldisiloxane, 1,1,3,3-tetramethyldisiloxane and/or
1,3-divinyl-1,1,3,3-tetramethyldisiloxane, oxygen, and an inert gas
such as helium and argon, but the gas barrier performance thereof
is as low as H.sub.2O=0.2 to 0.6 g/m.sup.2day and O.sub.2=0.4 to
0.5 cc/m.sup.2day.
[0005] In Patent Documents 2 and 3, the present inventors have
proposed a method for forming a low-dielectric insulating film by
PECVD using silane and siloxane compounds each having a structure
where a secondary or tertiary hydrocarbon group is directly bonded
to a silicon atom. However, these methods are a method for forming
a low-density thin film, and the thin film formed is not a
high-density thin film suitable for a sealing material,
particularly, for a gas barrier material.
BACKGROUND ART DOCUMENT
Patent Document
[0006] Patent Document 1: Japanese Patent No. 4,139,446
[0007] Patent Document 2: JP-A-2004-6607 (the term "JP-A" as used
herein means an "unexamined published Japanese patent
application")
[0008] Patent Document 3: JP-A-2005-51192
SUMMARY OF INVENTION
Problem that Invention is to Solve
[0009] The present invention has been made by taking into account
those problems, and an object of the present invention to provide a
sealing film composed of a carbon-containing silicon oxide film
obtained by CVD using, as the raw material, a
hydrocarbon-substituted silicon compound having a specific
structure, and a gas barrier equipment and materials, an FPD device
and a semiconductor device each containing the film.
Means for Solving Problem
[0010] The present inventors have found that a silicon compound
having a specific silicon to oxygen ratio and containing a
hydrocarbon substituent having a specific structure is suitable as
a film deposition material for CVD and a film obtained by CVD
using, as the raw material, this silicon compound having a specific
structure and a specific compositional ratio is useful as a sealing
film. The present invention has been accomplished based on this
finding.
[0011] That is, the present invention is a film deposition material
for CVD, containing an organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom. Also, the present invention is a sealing film
deposited by CVD using the film deposition material above. Also,
the present invention is a sealing film obtained by further
subjecting the sealing film above to a heat treatment, an
ultraviolet irradiation treatment or an electron beam treatment.
Also, the present invention is a gas barrier equipment and
materials characterized by using such a sealing film as a gas
barrier layer. Also, the present invention is a flat-panel display
device or a semiconductor device, characterized by containing such
a sealing film.
[0012] More specifically, the gist of the present invention resides
in the following (1) to (15).
[0013] (1) A film deposition material for a chemical vapor
deposition method, comprising:
[0014] an organosilicon compound having a secondary hydrocarbon
group directly bonded to at least one silicon atom and having an
atomic ratio of 0.5 or less oxygen atom with respect to 1 silicon
atom.
[0015] (2) The film deposition material as described in (1)
above,
[0016] wherein the organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom is preferably a disiloxane compound represented by the
following formula (1):
##STR00001##
(wherein each of R.sup.1 and R.sup.2 represents a hydrocarbon group
having a carbon number of 1 to 20; R.sup.1 and R.sup.2 may bond
with each other to form a cyclic structure; and each of R.sup.3 and
R.sup.4 represents a hydrocarbon group having a carbon number of 1
to 20 or a hydrogen atom).
[0017] (3) The film deposition material as described in (1)
above,
[0018] wherein the organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom is preferably a silane compound represented by the
following formula (2):
##STR00002##
(wherein each of R.sup.5 and R.sup.6 represents a hydrocarbon group
having a carbon number of 1 to 20; R.sup.5 and R.sup.6 may bond
with each other to form a cyclic structure; each of R.sup.7,
R.sup.8 and R.sup.9 represents a hydrocarbon group having a carbon
number of 1 to 20 or a hydrogen atom; and m represents an integer
of 1 to 20).
[0019] (4) The film deposition material as described in (1)
above,
[0020] wherein the organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom is preferably a cyclic silane compound represented by
the following formula (3):
##STR00003##
(wherein each of R.sup.10 and R.sup.11 represents a hydrocarbon
group having a carbon number of 1 to 20; R.sup.10 and R.sup.11 may
bond with each other to form a cyclic structure; R.sup.12
represents a hydrocarbon group having a carbon number of 1 to 20 or
a hydrogen atom; and n represents an integer of 4 to 40).
[0021] (5) The film deposition material according to any one of (2)
to (4) above,
[0022] wherein in formula (1), (2) or (3), preferably, both R.sup.1
and R.sup.2, both R.sup.5 and R.sup.6 or both R.sup.10 and R.sup.11
are methyl or are methyl and ethyl, respectively.
[0023] (6) The film deposition material as described in (2) or (5)
above,
[0024] wherein the organosilicon compound is preferably
1,3-diisopropyldisiloxane, 1,3-diisopropyl-1,3-dimethyldi siloxane,
1,3-diisopropyl-1,1,3,3-tetramethyldisiloxane,
1,3-di-sec-butyldisiloxane, 1,3-di-sec-butyl-1,3-dimethyldisiloxane
or 1,3-di-sec-butyl-1,1,3,3-tetramethyldisiloxane.
[0025] (7) The film deposition material as described in (3) or (5)
above,
[0026] wherein the organosilicon compound is preferably
isopropylsilane, isopropylmethylsilane, isopropyldimethylsilane,
diisopropylsilane, diisopropylmethylsilane, triisopropylsilane,
sec-butylsilane, sec-butylmethylsilane, sec-butyldimethylsilane,
di-sec-butylsilane, di-sec-butylmethylsilane or
tri-sec-butylsilane.
[0027] (8) The film deposition material as described in (4) or (5)
above,
[0028] wherein the organosilicon compound is preferably
1,2,3,4-tetraisopropylcyclotetrasilane,
1,2,3,4,5-pentaisopropylcyclopentasilane,
1,2,3,4,5,6-hexaisopropylcyclohexasilane,
1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decaisopropylcyclopentasilane or
1,1,2,2,3,3,4,4,5,5,6,6-undecaisopropylcyclohexasilane.
[0029] (9) The film deposition material as described in any one of
(1) to (8) above,
[0030] wherein the chemical vapor deposition method is preferably a
plasma enhanced chemical vapor deposition method.
[0031] (10) The film deposition material as described in any one of
(1) to (8) above,
[0032] wherein the chemical vapor deposition method is preferably a
catalytic chemical vapor deposition method.
[0033] (11) A sealing film, deposited by a chemical vapor
deposition method using the film deposition material described in
any one of (1) to (10) above.
[0034] (12) A sealing film, obtained by preferably further
subjecting the sealing film described in (11) above to a heat
treatment, an ultraviolet irradiation treatment or an electron beam
treatment.
[0035] (13) A gas barrier equipment and materials, using the
sealing film described in (11) or (12) above as a gas barrier
layer.
[0036] (14) A flat-panel display device, containing:
[0037] the sealing film described in (11) or (12) above.
[0038] (15) A semiconductor device, comprising:
[0039] the sealing film described in (11) or (12) above.
Advantage of the Invention
[0040] According to the present invention, a film deposition
material containing an organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom can be deposited by CVD to form a carbon-containing
silicon oxide film, and the film can be used as a sealing film.
Above all, this sealing film is very useful as a gas barrier film
or a gas barrier layer for a gas barrier substrate.
BRIEF DESCRIPTION OF THE DRAWINGS
[0041] FIG. 1 A view depicting a parallel plate capacitively
coupled PECVD set up.
[0042] FIG. 2 A view depicting an inductively coupled remote PECVD
set up.
[0043] FIG. 3 A view depicting a microwave PECVD set up.
MODE FOR CARRYING OUT THE INVENTION
[0044] The present invention is described in detail below.
[0045] In the present invention, the organosilicon compound having
a secondary hydrocarbon group directly bonded to at least one
silicon atom and having an atomic ratio of 0.5 or less oxygen atom
with respect to 1 silicon atom is not particularly limited but is
preferably a disiloxane compound represented by the following
formula (1):
##STR00004##
(wherein each of R.sup.1 and R.sup.2 represents a hydrocarbon group
having a carbon number of 1 to 20, R.sup.1 and R.sup.2 may bond
with each other to form a cyclic structure, and each of R.sup.3 and
R.sup.4 represents a hydrocarbon group having a carbon number of 1
to 20 or a hydrogen atom),
[0046] a silane compound represented by the following formula
(2):
##STR00005##
(wherein each of R.sup.5 and R.sup.6 represents a hydrocarbon group
having a carbon number of 1 to 20, R.sup.5 and R.sup.6 may bond
with each other to form a cyclic structure, each of R.sup.7,
R.sup.8 and R.sup.9 represents a hydrocarbon group having a carbon
number of 1 to 20 or a hydrogen atom, and m represents an integer
of 1 to 20), or
[0047] a cyclic silane compound represented by the following
formula (3):
##STR00006##
(wherein each of R.sup.10 and R.sup.11 represents a hydrocarbon
group having a carbon number of 1 to 20, R.sup.10 and R.sup.11 may
bond with each other to form a cyclic structure, R.sup.12
represents a hydrocarbon group having a carbon number of 1 to 20 or
a hydrogen atom, and n represents an integer of 4 to 40).
[0048] Each of R.sup.1 and R.sup.2 in formula (1), each of R.sup.5
and R.sup.6 in formula (2), or each of R.sup.10 and R.sup.11 in
formula (3) is a saturated or unsaturated hydrocarbon group having
a carbon number of 1 to 20 and may have any of linear, branched and
cyclic structures. In addition, compounds to which they are linked
together to form a cyclic structure are also included within the
scope of the present invention. If the carbon number exceeds 20,
procurement of the raw material such as corresponding organic
halide may be difficult and even if the raw material can be
procured, its purity may be low. Considering stable use of the CVD
apparatus, a hydrocarbon group having a carbon number of 1 to 10 is
particularly preferred, because the organosilicon compound can be
kept from excessive reduction in its vapor pressure.
[0049] Examples of the hydrocarbon group of R.sup.1 and R.sup.2 in
formula (1), R.sup.5 and R.sup.6 in formula (2), or R.sup.10 and
R.sup.11 in formula (3) include, but are not particularly limited
to, an alkyl group having a carbon number of 1 to 20, preferably a
carbon number of 1 to 10, an aryl group, an arylalkyl group, an
alkylaryl group, and an alkenyl group such as vinyl group. R.sup.1
and R.sup.2, R.sup.5 and R.sup.6, or R.sup.10 and R.sup.11 may be
the same as or different from one another.
[0050] Examples of the case where R.sup.1 and R.sup.2, R.sup.5 and
R.sup.6, or R.sup.10 and R.sup.11 are not bonded together include
compounds where each of R.sup.1 and R.sup.2, each of R.sup.5 and
R.sup.6, or each of R.sup.10 and R.sup.11 is methyl, ethyl,
n-propyl, isopropyl, n-butyl, i-butyl, sec-butyl, tert-butyl,
n-pentyl, tert-amyl, n-hexyl, cyclohexyl, phenyl, benzyl or
toluoyl.
[0051] As for examples of the group formed by combining together
R.sup.1 and R.sup.2, R.sup.5 and R.sup.6, or R.sup.10 and R.sup.11
and bonded to Si through a secondary hydrocarbon group,
representative examples include a case where the secondary
hydrocarbon group is cyclobutyl, cyclobutenyl, cyclopentyl,
cyclopentadienyl, cyclohexyl, cyclohexenyl, cyclooctenyl or
cyclooctadienyl.
[0052] Among others, as for the combination of R.sup.1 and R.sup.2,
R.sup.5 and R.sup.6, or R.sup.10 and R.sup.11, isopropyl when both
R.sup.1 and R.sup.2, both R.sup.5 and R.sup.6, or both R.sup.10 and
R.sup.11 are methyl; sec-butyl when R.sup.1 and R.sup.2, R.sup.5
and R.sup.6, or R.sup.10 and R.sup.11 are methyl and ethyl,
respectively; and cyclopentyl, cyclopentadienyl, cyclohexyl or
cyclohexenyl group when R.sup.1 and R.sup.2, R.sup.5 and R.sup.6,
or R.sup.10 and R.sup.11 are bonded together, are preferred from
the economical standpoint, and in this case, the gas barrier
performance may be greatly enhanced.
[0053] Each of R.sup.3 and R.sup.4 in formula (1), each of R.sup.7,
R.sup.8 and R.sup.9 in formula (2), or R.sup.12 in formula (3)
represents a hydrocarbon group having a carbon number of 1 to 20 or
a hydrogen atom, and the hydrocarbon group is a saturated or
unsaturated hydrocarbon group and may have any of linear, branched
and cyclic structures. If the carbon number exceeds 20, the vapor
pressure of the organosilicon compound produced may be
disadvantageously reduced to make use in a CVD apparatus
difficult.
[0054] As for the hydrocarbon group of R.sup.3 and R.sup.4 in
formula (1), R.sup.7, R.sup.8 and R.sup.9 in formula (2), or
R.sup.12 in formula (3), the same groups as examples of the
hydrocarbon group of R.sup.1 and R.sup.2 in formula (1), R.sup.5
and R.sup.6 in formula (2), or R.sup.10 and R.sup.11 in formula (3)
may be used.
[0055] In particular, when each of R.sup.3 and R.sup.4 in formula
(1), each of R.sup.7, R.sup.8 and R.sup.9 in formula (2), or
R.sup.12 in formula (3) is a hydrogen atom or a hydrocarbon group
having a carbon number of 1 to 4, i.e., methyl, ethyl, n-propyl,
isopropyl, n-butyl, i-butyl, sec-butyl or tert-butyl, this is
preferred in view of high vapor pressure and procurement of raw
material. Above all, when each of those members is a hydrogen atom
or a secondary or tertiary carbon substituent, i.e., isopropyl,
sec-butyl or tert-butyl, the gas barrier performance may be greatly
enhanced.
[0056] Among disiloxane compounds represented by formula (1), a
disiloxane compound having a hydrogen atom directly bonded to a
silicon atom, represented by the following formula (4):
##STR00007##
(wherein each of R.sup.1 and R.sup.2 represents a hydrocarbon group
having a carbon number of 1 to 20, R.sup.1 and R.sup.2 may bond
with each other to form a cyclic structure, and R.sup.3 represents
a hydrocarbon group having a carbon number of 1 to 20 or a hydrogen
atom), is preferred, and in this case, a sealing film having a very
high gas barrier performance may be formed at a high deposition
rate.
[0057] Specific examples of the disiloxane compound having a
structure where a secondary hydrocarbon group is directly bonded to
a silicon atom, represented by formula (1) or (4), include
[0058] 1,3-diisopropyldisiloxane,
[0059] 1,3-diisopropyl-1,3-dimethyldisiloxane,
1,3-diisopropyl-1,3-diethyldisiloxane,
1,3-diisopropyl-1,3-divinyldisiloxane,
1,3-diisopropyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetraisopropyldisiloxane,
1,3-diisopropyl-1,3-di-n-butyldisiloxane,
1,3-diisopropyl-1,3-diisobutyldisiloxane, 1,3-di
isopropyl-1,3-di-sec-butyldisiloxane,
1,3-diisopropyl-1,3-diphenyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetramethyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetraethyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetravinyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetra-n-propyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetra-n-butyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetraisobutyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetra-sec-butyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetraphenyldisiloxane,
[0060] 1,1,3,3,-tetraisopropyl-1,3-dimethyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-diethyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-divinyldisiloxane,
1,1,3,3,-tetraisopropyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-di-n-butyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-diisobutyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-di-sec-butyldisiloxane,
1,1,3,3-tetraisopropyl-1,3-diphenyldisiloxane,
1,1,1,3,3,3-hexaisopropyldisiloxane,
[0061] 1,3-di-sec-butyldisiloxane,
[0062] 1,3-di-sec-butyl-1,3-dimethyldisiloxane,
1,3-di-sec-butyl-1,3-diethyldisiloxane,
1,3-di-sec-butyl-1,3-divinyldisiloxane,
1,3-di-sec-butyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetra-sec-butyldisiloxane,
1,3-di-sec-butyl-1,3-di-n-butyldisiloxane,
1,3-di-sec-butyl-1,3-diisobutyldisiloxane,
1,3-di-sec-butyl-1,3-di-sec-butyldisiloxane,
1,3-di-sec-butyl-1,3-diphenyldisiloxane,
[0063] 1,3-di-sec-butyl-1,1,3,3-tetramethyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetraethyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetravinyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetra-n-propyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetra-n-butyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetraisobutyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetraphenyldisiloxane,
[0064] 1,1,3,3,-tetra-sec-butyl-1,3-dimethyldisiloxane,
1,1,3,3-tetra-sec-butyl-1,3-diethyldisiloxane,
1,1,3,3-tetra-sec-butyl-1,3-divinyldisiloxane,
1,1,3,3-tetra-sec-butylisopropyl-1,3-di-n-propyldi siloxane,
1,1,3,3-tetra-sec-butyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetra-sec-butyl-1,3-di-n-butyldisiloxane,
1,1,3,3-tetra-sec-butyl-1,3-diisobutyldisiloxane,
1,1,3,3-tetra-sec-butyl-1,3-diphenyldisiloxane,
1,1,1,3,3,3-hexa-sec-butyldisiloxane,
[0065] 1,3-dicyclopentyldisiloxane,
[0066] 1,3-dicyclopentyl-1,3-dimethyldisiloxane,
1,3-dicyclopentyl-1,3-diethyldisiloxane,
1,3-dicyclopentyl-1,3-divinyldisiloxane,
1,3-dicyclopentyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclopentyldisiloxane,
1,3-dicyclopentyl-1,3-di-n-butyldisiloxane,
1,3-dicyclopentyl-1,3-diisobutyldisiloxane,
1,3-dicyclopentyl-1,3-di-sec-butyldisiloxane,
1,3-dicyclopentyl-1,3-diphenyldisiloxane,
[0067] 1,3-dicyclopentyl-1,1,3,3-tetramethyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetraethyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetravinyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetra-n-propyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetra-n-butyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetraisobutyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetra-sec-butyldisiloxane,
1,3-dicyclopentyl-1,1,3,3-tetraphenyldisiloxane,
[0068] 1,1,3,3-tetracyclopentyl-1,3-dimethyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-diethyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-divinyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-di-n-propyldi siloxane,
1,1,3,3-tetracyclopentyl-1,3-di-n-butyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-diisobutyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-di-sec-butyldisiloxane,
1,1,3,3-tetracyclopentyl-1,3-diphenyldisiloxane,
1,1,1,3,3,3-hexacyclopentyldisiloxane,
1,3-dicyclopentadienyldisiloxane,
[0069] 1,3-dicyclopentadienyl-1,3-dimethyldisiloxane,
1,3-dicyclopentadienyl-1,3-diethyldisiloxane,
1,3-dicyclopentadienyl-1,3-divinyldisiloxane,
1,3-dicyclopentadienyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclopentadienyldisiloxane,
1,3-dicyclopentadienyl-1,3-di-n-butyldisiloxane,
1,3-dicyclopentadienyl-1,3-diisobutyldisiloxane,
1,3-dicyclopentadienyl-1,3-di-sec-butyldisiloxane,
1,3-dicyclopentadienyl-1,3-diphenyldisiloxane,
[0070] 1,3-dicyclopentadienyl-1,1,3,3-tetramethyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetraethyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetravinyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-n-propyldi siloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-n-butyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetraisobutyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-sec-butyldisiloxane,
1,3-dicyclopentadienyl-1,1,3,3-tetraphenyldisiloxane,
[0071] 1,1,3,3-tetracyclopentadienyl-1,3-dimethyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-diethyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-divinyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-propyldi siloxane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-butyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-diiosobutyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-di-sec-butyldisiloxane,
1,1,3,3-tetracyclopentadienyl-1,3-diphenyldi siloxane,
1,1,1,3,3,3-hexacyclopentadienyldisiloxane,
[0072] 1,3-dicyclohexyldisiloxane,
[0073] 1,3-dicyclohexyl-1,3-dimethyldisiloxane,
1,3-dicyclohexyl-1,3-diethyldisiloxane,
1,3-dicyclohexyl-1,3-divinyldisiloxane,
1,3-dicyclohexyl-1,3-di-n-propyldi siloxane,
1,1,3,3-tetracyclohexyldisiloxane,
1,3-dicyclohexyl-1,3-di-n-butyldisiloxane,
1,3-dicyclohexyl-1,3-diisobutyldisiloxane,
1,3-dicyclohexyl-1,3-di-sec-butyldisiloxane,
1,3-dicyclohexyl-1,3-diphenyldisiloxane,
[0074] 1,3-dicyclohexyl-1,1,3,3-tetramethyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetraethyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetravinyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetra-n-propyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetra-n-butyl di siloxane,
1,3-dicyclohexyl-1,1,3,3-tetraisobutyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetra-sec-butyldisiloxane,
1,3-dicyclohexyl-1,1,3,3-tetraphenyldisiloxane,
[0075] 1,1,3,3-tetracyclohexyl-1,3-dimethyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-diethyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-divinyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-di-n-propyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-di-n-butyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-diisobutyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-di-sec-butyldisiloxane,
1,1,3,3-tetracyclohexyl-1,3-diphenyldisiloxane, and
1,1,1,3,3,3-hexacyclohexyldisiloxane.
[0076] Among others, 1,3-diisopropyldisiloxane,
1,3-diisopropyl-1,3-dimethyldisiloxane,
1,3-diisopropyl-1,1,3,3-tetramethyldisiloxane,
1,3-di-sec-butyldisiloxane,
1,3-di-sec-butyl-1,3-dimethyldisiloxane,
1,3-di-sec-butyl-1,1,3,3-tetramethyldisiloxane and the like are
preferred.
[0077] The disiloxane compound having a structure where a secondary
hydrocarbon group is directly bonded to a silicon atom, represented
by formula (1) or (4), is not particularly limited in its
production method but can be produced from a hydrolyzable
organosilane compound.
[0078] For example, an organic compound represented by the
following formula (5):
##STR00008##
(wherein R.sup.1 and R.sup.2 are the same as respective members in
formula (1) or (4), and X represents a hydrogen atom, a chlorine
atom, a bromine atom or an iodine atom) is reacted with an
organolithium or metal lithium particle to produce a compound where
a secondary hydrocarbon group and/or an alkenyl group are directly
bonded to a lithium atom, and the produced compound is reacted with
halogenated alkoxysilanes represented by the following formula
(6):
[Chem. 9]
Y.sub.pSiR.sup.3R.sup.4(OR.sup.13).sub.2-p (6)
(wherein Y represents a fluorine atom, a chlorine atom, a bromine
atom or an iodine atom, R.sup.3 and R.sup.4 are the same as
respective members in formula (1) or (4), R.sup.13 represents a
hydrocarbon group having a carbon number of 1 to 20 or a hydrogen
atom, and p represents an integer of 0 to 2) to produce a
hydrolyzable organosilane compound represented by the following
formula (7):
##STR00009##
(wherein R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are the same as
respective members in formula (1) or (4), Y and R.sup.13 are the
same as those in formula (6), and q represents an integer of 0 or
1).
[0079] A hydrolyzable organosilane compound represented by formula
(7) can be produced also by using a metal magnesium in place of the
organolithium or metal lithium particle in the above-described
production method for a hydrolyzable organosilane compound.
[0080] Out of organic compounds represented by formula (5),
examples of the compound where X is a chlorine atom, a bromine atom
or an iodine atom include isopropyl chloride, isopropyl bromide,
isopropyl iodide, sec-butyl chloride, sec-butyl bromide, sec-butyl
iodide, cyclopentyl chloride, cyclopentyl bromide, cyclopentyl
iodide, cyclohexyl chloride, cyclohexyl bromide, and cyclohexyl
iodide.
[0081] Out of organic compounds represented by formula (5),
examples of the compound where X is a hydrogen atom include
cyclopentadiene, pentamethylcyclopentadiene, and
1,2,3,4-tetramethyl-1,3-cyclopentadiene, and by reacting such a
compound with an organolithium such as n-butyllithium and
tert-butyllithium, a compound where a secondary hydrocarbon group
and/or an alkenyl group are directly bonded to a lithium atom can
be produced.
[0082] Examples of the halogenated alkoxysilanes represented by
formula (6) include dichlorosilane, dibromosilane, diiodosilane,
dimethoxysilane, diethoxysilane,
[0083] methyldichlorosilane, methyldibromosilane,
methyldiiodosilane, methyldimethoxysilane,
methyldiethoxysilane,
[0084] ethyldichlorosilane, ethyldibromosilane, ethyldiiodosilane,
ethyldimethoxysilane, ethyldiethoxysilane,
[0085] n-propyldichlorosilane, n-propyldibromosilane,
n-propyldiiodosilane, n-propyldimethoxysilane,
n-propyldiethoxysilane, isopropyldichlorosilane,
isopropyldibromosilane, isopropyldiiodosilane,
isopropyldimethoxysilane, isopropyldiethoxysilane,
[0086] n-butyldichlorosilane, n-butyldibromosilane,
n-butyldiiodosilane, n-butyldimethoxysilane, n-butyldiethoxysilane,
isobutyldichlorosilane, isobutyldibromosilane,
isobutyldiiodosilane, isobutyldimethoxysilane,
isobutyldiethoxysilane, sec-butyldichlorosilane,
sec-butyldibromosilane, sec-butyldiiodosilane,
sec-butyldimethoxysilane, sec-butyldiethoxysilane,
tert-butyldichlorosilane, tert-butyldibromosilane,
tert-butyldiiodosilane, tert-butyldimethoxysilane, and
tert-butyldiethoxysilane.
[0087] Other examples include dimethyldichlorosilane,
dimethyldibromosilane, dimethyldiiodosilane,
dimethyldimethoxysilane, dimethyldiethoxysilane,
[0088] diethyldichlorosilane, diethyldibromosilane,
diethyldiiodosilane, diethyldimethoxysilane,
diethyldiethoxysilane,
[0089] di-n-propyldichlorosilane, di-n-propyldibromosilane,
di-n-propyldiiodosilane, di-n-propyldimethoxysilane,
di-n-propyldiethoxysilane, diisopropyldichlorosilane,
diisopropyldibromosilane, diisopropyldiiodosilane,
diisopropyldimethoxysilane, diisopropyldiethoxysilane,
[0090] di-n-butyldichlorosilane, di-n-butyldibromosilane,
di-n-butyldiiodosilane, di-n-butyldimethoxysilane,
di-n-butyldiethoxysilane, diisobutyldichlorosilane,
diisobutyldibromosilane, diisobutyldiiodosilane,
diisobutyldimethoxysilane, diisobutyldiethoxysilane,
di-sec-butyldichlorosilane, sec-butyldibromosilane,
di-sec-butyldiiodosilane, di-sec-butyldimethoxysilane,
di-sec-butyldiethoxysilane, di-tert-butyldichlorosilane,
di-tert-butyldibromosilane, di-tert-butyldiiodosilane,
di-tert-butyldimethoxysilane, di-tert-butyldiethoxysilane,
divinyldichlorosilane, diphenyldichlorosilane, and
diphenyldimethoxysilane.
[0091] By employing this production method, a hydrolyzable
organosilane compound represented by formula (7) can be obtained in
high yield and high purity while suppressing the production of
byproducts.
[0092] The production conditions for the compound where a secondary
hydrocarbon group is directly bonded to a lithium atom are not
particularly limited but are described below by referring to one
example.
[0093] As the metal lithium used, a lithium wire, a lithium ribbon,
a lithium shot and the like may be employed, but in view of
reaction efficiency, it is preferred to use a lithium fine particle
having a particle diameter of 500 .mu.m or less.
[0094] In the case of using a metal magnesium, a magnesium ribbon,
a magnesium particle, a magnesium powder and the like may be
employed.
[0095] As the organolithium used, an n-hexane solution of
n-butyllithium, an n-pentane solution of tert-butyllithium, and the
like may be employed.
[0096] The solvent used for the reaction is not particularly
limited as long as it is a solvent used in this technical field,
and for example, saturated hydrocarbons such as n-pentane, pentane,
n-hexane, cyclohexane, n-heptane and n-decane, unsaturated
hydrocarbons such as toluene, xylene and decene-1, and ethers such
as diethyl ether, dipropyl ether, tert-butyl methyl ether, dibutyl
ether and cyclopentyl methyl ether, may be used. Furthermore, a
mixed solvent thereof may also be used.
[0097] As for the reaction temperature, the reaction above is
preferably performed in a temperature range not involving
decomposition of the produced compound where a secondary carbon
atom is bonded to a lithium atom or where a secondary hydrocarbon
group is directly bonded to a magnesium atom. Usually, the reaction
is preferably performed at -100 to 200.degree. C. that is a
temperature employed in industry, more preferably at -85 to
150.degree. C. The reaction pressure condition may be any of under
pressure, under atmospheric pressure and under reduced
pressure.
[0098] The synthesized compound where a secondary hydrocarbon group
is directly bonded to a lithium atom or where a secondary
hydrocarbon group is directly bonded to a magnesium atom, may be
used as it is after the production or may be used after removing
unreacted organic halide, metal lithium or metal magnesium and
removing lithium halide or magnesium halide which are a reaction
byproduct.
[0099] The conditions for reacting the thus-obtained compound where
a secondary hydrocarbon group is directly bonded to a lithium atom
or where a secondary hydrocarbon group is directly bonded to a
magnesium atom, with halogenated alkoxysilanes of formula (7) are
not particularly limited and are described below by referring to
one example.
[0100] The usable reaction solvents are the same as those which can
be used in the reaction for the compound where a secondary
hydrocarbon group is directly bonded to a lithium atom (or a
magnesium atom). As for the reaction temperature, the reaction is
preferably preformed in a temperature range not involving
decomposition of the compound where a secondary hydrocarbon group
is directly bonded to a lithium atom or where a secondary
hydrocarbon group is directly bonded to a magnesium atom. Usually,
the reaction is preferably performed at -100 to 200.degree. C. that
is a temperature employed in industry, more preferably at -85 to
150.degree. C. The reaction pressure condition may be any of under
pressure, under atmospheric pressure and under reduced
pressure.
[0101] The production method for the disiloxane compound of formula
(1) or (4) is not particularly limited, but the compound can be
produced by reacting the hydrolyzable organosilane compound of
formula (7) with water in the presence of an acid or a base.
[0102] As the acid caused to be present together in the reaction,
an inorganic acid such as hydrochloric acid, nitric acid and
sulfuric acid, and an organic acid such as toluenesulfonic acid,
may be used.
[0103] The reaction solvent usable for producing the disiloxane
compound of formula (1) or (4) is not particularly limited as long
as it is a solvent used in this technical field, and, for example,
saturated hydrocarbons such as n-pentane, i-pentane, n-hexane,
cyclohexane, n-heptane and n-decane, unsaturated hydrocarbons such
as toluene, xylene and decene-1, ethers such as diethyl ether,
dipropyl ether, tert-butyl methyl ether, dibutyl ether, cyclopentyl
methyl ether and tetrahydrofuran, and alcohols such as methanol,
ethanol, isopropanol, n-butanol, tert-butanol and 2-ethylhexanol,
may be used. Furthermore, a mixed solvent thereof may also be
employed. In addition, the compound may also be produced only from
the hydrolyzable organosilane compound itself of formula (7)
without using a solvent.
[0104] As for the reaction temperature when producing the
disiloxane compound of formula (1) or (4), usually, the reaction is
preferably performed at -100 to 200.degree. C. that is a
temperature employed in industry, more preferably at -85 to
150.degree. C. The reaction pressure condition may be any of under
pressure, under atmospheric pressure and under reduced
pressure.
[0105] As to the method for purifying the synthesized disiloxane
compound of formula (1) or (4), in order to ensure a useful water
content in use as a film deposition material and at the same time,
reduce the amount of impurity elements derived from the production
raw materials, except for silicon, carbon, oxygen and hydrogen, the
by-produced lithium salt or magnesium salt may be removed by a
purification technique, for example, by filtration using a glass
filter, a sintered porous body or the like, by distillation under
atmospheric pressure or reduced pressure, or by column separation
using silica, alumina or a polymer gel. At this time, these
techniques may be used in combination, if desired.
[0106] Also, when a silanol structure-containing by-product is
contained, the hydrocarbon-substituted alkoxysilane as the main
product can be isolated/produced by distillation after the hydroxyl
group of silanol is precipitated as a sodium salt or a potassium
salt with sodium hydride, potassium hydride or the like.
[0107] At the production, the purification conforms to the method
in the field of organic metal compound synthesis. That is, it is
preferred to perform the purification in a dehydrated and
deoxidized nitrogen or argon atmosphere and previously subject the
employed solvent, column packing material for purification, and the
like to a dehydration operation. Furthermore, impurities such as
metal residue and particles are preferably removed in advance.
[0108] Specific examples of the silane compound represented by
formula (2) include monosilanes such as isopropylsilane,
isopropylmethylsilane, isopropylethylsilane,
isopropyl-n-propylsilane, isopropyl-n-butylsilane,
isopropylisobutylsilane, isopropyl-sec-butylsilane,
isopropyl-sec-butylsilane, isopropyl-n-hexylsilane,
isopropylcyclohexylsilane, isopropylcyclopentylsilane,
isopropylcyclopentadienylsilane, isopropylphenylsilane,
[0109] isopropyldimethylsilane, isopropyldiethylsilane,
isopropyldiethylsilane, isopropyl-di-n-propylsilane,
isopropyl-di-n-butylsilane, isopropyldiisobutylsilane,
isopropyl-di-sec-butylsilane, isopropyl-di-n-hexylsilane,
isopropyldicyclohexylsilane, isopropyldicyclopentylsilane,
isopropyldicyclopentadienylsilane, isopropyldiphenylsilane,
[0110] diisopropylsilane, diisopropylmethylsilane,
diisopropylethylsilane, diisopropyl-n-propylsilane,
diisopropyl-n-butylsilane, diisopropyl-sec-butylsilane,
diisopropyl-sec-butylsilane, diisopropyl-n-hexylsilane,
diisopropylcyclohexylsilane, diisopropylcyclopentylsilane,
diisopropylcyclopentadienylsilane, diisopropylphenylsilane,
[0111] triisopropylsilane, triisopropylmethylsilane,
triisopropylethylsilane, triisopropyl-n-propylsilane,
triisopropyl-n-butylsilane, triisopropylisobutylsilane,
triisopropyl-sec-butylsilane, triisopropyl-n-hexylsilane,
triisopropylcyclohexylsilane, triisopropylcyclopentylsilane,
triisopropylcyclopentadienylsilane, triisopropylphenylsilane,
tetraisopropylsilane,
[0112] sec-butylsilane, sec-butylmethylsilane,
sec-butylethylsilane, sec-butyl-n-propylsilane,
sec-butyl-n-butylsilane, sec-butylisobutylsilane,
sec-butyl-sec-butylsilane, sec-butyl-sec-butylsilane,
sec-butyl-n-hexylsilane, sec-butylcyclohexylsilane,
sec-butylcyclopentylsilane, sec-butylcyclopentadienylsilane,
sec-butylphenylsilane,
[0113] sec-butyldimethylsilane, sec-butyldiethylsilane,
sec-butyldiethylsilane, sec-butyl-di-n-propylsilane,
sec-butyl-di-n-butylsilane, sec-butyldiisobutylsilane,
sec-butyl-di-sec-butylsilane, sec-butyl-di-n-hexylsilane,
sec-butyldicyclohexylsilane, sec-butyldicyclopentylsilane,
sec-butyldicyclopentadienylsilane, sec-butyldiphenylsilane,
[0114] di-sec-butylsilane, di-sec-butylmethylsilane,
di-sec-butylethylsilane, di-sec-butyl-n-propylsilane,
di-sec-butyl-n-butylsilane, di-sec-butylisobutylsilane,
di-sec-butyl-sec-butylsilane, di-sec-butyl-n-hexylsilane,
di-sec-butylcyclohexylsilane, di-sec-butylcyclopentylsilane,
di-sec-butylcyclopentadienylsilane, di-sec-butylphenylsilane,
[0115] tri-sec-butylsilane, tri-sec-butylmethylsilane,
tri-sec-butylethylsilane, tri-sec-butyl-n-propylsilane,
tri-sec-butyl-n-butylsilane, tri-sec-butylisobutylsilane,
tri-sec-butyl-n-hexylsilane, tri-sec-butylcyclohexylsilane,
tri-sec-butylcyclopentylsilane,
tri-sec-butylcyclopentadienylsilane, tri-sec-butylphenylsilane,
tetra-sec-butylsilane,
[0116] cyclopentylsilane, cyclopentylmethylsilane,
cyclopentylethylsilane, cyclopentyl-n-propylsilane,
cyclopentyl-n-butylsilane, cyclopentylisobutylsilane,
cyclopentyl-sec-butylsilane, cyclopentyl-sec-butylsilane,
cyclopentyl-n-hexylsilane, cyclopentylcyclohexylsilane,
cyclopentylcyclopentadienylsilane, cyclopentylphenylsilane,
[0117] cyclopentyldimethylsilane, cyclopentyldiethylsilane,
cyclopentyldiethylsilane, cyclopentyl-di-n-propylsilane,
cyclopentyl-di-n-butylsilane, cyclopentyldiisobutylsilane,
cyclopentyl-di-sec-butylsilane, cyclopentyl-di-n-hexylsilane,
cyclopentyldicyclohexylsilane, cyclopentyldicyclopentylsilane,
cyclopentyldicyclopentadienylsilane, cyclopentyldiphenylsilane,
[0118] dicyclopentylsilane, dicyclopentylmethylsilane,
dicyclopentylethylsilane, dicyclopentyl-n-propylsilane,
dicyclopentyl-n-butylsilane, dicyclopentylisobutylsilane,
dicyclopentyl-sec-butylsilane, dicyclopentyl-sec-butylsilane,
dicyclopentyl-n-hexylsilane, dicyclopentylcyclohexylsilane,
dicyclopentylcyclopentadienylsilane, dicyclopentylphenylsilane,
[0119] tricyclopentylsilane, tricyclopentylmethylsilane,
tricyclopentylethylsilane, tricyclopentyl-n-propylsilane,
tricyclopentyl-n-butylsilane, tricyclopentylisobutylsilane,
tricyclopentyl-sec-butylsilane, tricyclopentyl-n-hexylsilane,
tricyclopentylcyclohexylsilane,
tricyclopentylcyclopentadienylsilane, tricyclopentylphenylsilane,
tetracyclopentylsilane,
[0120] cyclopentadienylsilane, cyclopentadienylmethylsilane,
cyclopentadienylethylsilane, cyclopentadienyl-n-propylsilane,
cyclopentadienyl-n-butylsilane, cyclopentadienylisobutylsilane,
cyclopentadienyl-sec-butylsilane, cyclopentadienyl-sec-butylsilane,
cyclopentadienyl-n-hexylsilane, cyclopentadienylcyclohexylsilane,
cyclopentadienylcyclopentylsilane,
cyclopentadienylphenylsilane,
[0121] cyclopentadienyldimethylsilane,
cyclopentadienyldiethylsilane, cyclopentadienyldiethylsilane,
cyclopentadienyl-di-n-propylsilane,
cyclopentadienyl-di-n-butylsilane,
cyclopentadienyldiisobutylsilane,
cyclopentadienyl-di-sec-butylsilane,
cyclopentadienyl-di-n-hexylsilane,
cyclopentadienyldicyclohexylsilane,
cyclopentadienyldicyclopentylsilane,
cyclopentadienyldiphenylsilane,
[0122] dicyclopentadienylsilane, dicyclopentadienylmethylsilane,
dicyclopentadienylethylsilane, dicyclopentadienyl-n-propylsilane,
dicyclopentadienyl-n-butylsilane, dicyclopentadienylisobutylsilane,
dicyclopentadienyl-sec-butylsilane,
dicyclopentadienyl-sec-butylsilane,
dicyclopentadienyl-n-hexylsilane,
dicyclopentadienylcyclohexylsilane,
dicyclopentadienylcyclopentylsilane,
dicyclopentadienylphenylsilane,
[0123] tricyclopentadienylsilane, tricyclopentadienylmethylsilane,
tricyclopentadienylethylsilane, tricyclopentadienyl-n-propylsilane,
tricyclopentadienyl-n-butylsilane,
tricyclopentadienylisobutylsilane,
tricyclopentadienyl-sec-butylsilane,
tricyclopentadienyl-n-hexylsilane,
tricyclopentadienylcyclohexylsilane,
tricyclopentadienylcyclopentylsilane,
tricyclopentadienylphenylsilane,
[0124] tetracyclopentadienylsilane,
[0125] cyclohexylsilane, cyclohexylmethylsilane,
cyclohexylethylsilane, cyclohexyl-n-propylsilane,
cyclohexyl-n-butylsilane, cyclohexylisobutylsilane,
cyclohexyl-sec-butylsilane, cyclohexyl-sec-butylsilane,
cyclohexyl-n-hexylsilane, cyclohexylcyclohexylsilane,
cyclohexylcyclopentylsilane, cyclohexylcyclopentadienylsilane,
cyclohexylphenylsilane,
[0126] cyclohexyldimethylsilane, cyclohexyldiethylsilane,
cyclohexyldiethylsilane, cyclohexyldi-n-propylsilane,
cyclohexyl-di-n-butylsilane, cyclohexyldiisobutylsilane,
cyclohexyl-di-sec-butylsilane, cyclohexyl-di-n-hexylsilane,
cyclohexyldicyclopentylsilane, cyclohexyldicyclopentadienylsilane,
cyclohexyldiphenylsilane,
[0127] dicyclohexylsilane, dicyclohexylmethylsilane,
dicyclohexylethylsilane, dicyclohexyl-n-propylsilane,
dicyclohexyl-n-butylsilane, dicyclohexyldiisobutylsilane,
dicyclohexyl-sec-butylsilane, dicyclohexyl-n-hexylsilane,
dicyclohexylcyclopentylsilane, dicyclohexylcyclopentadienylsilane,
dicyclohexylphenylsilane,
[0128] tricyclohexylsilane, tricyclohexylmethylsilane,
tricyclohexylethylsilane, tricyclohexyl-n-propylsilane,
tricyclohexyl-n-butylsilane, tricyclohexylisobutylsilane,
tricyclohexyl-sec-butylsilane, tricyclohexyl-n-hexylsilane,
tricyclohexylcyclopentylsilane,
tricyclohexylcyclopentadienylsilane, tricyclohexylphenylsilane,
and
[0129] tetracyclohexylsilane;
and
[0130] disilanes such as
[0131] 1,3-diisopropyldisilane,
[0132] 1,3-diisopropyl-1,3-dimethyldisilane,
1,3-diisopropyl-1,3-diethyldisilane,
1,3-diisopropyl-1,3-divinyldisilane,
1,3-diisopropyl-1,3-di-n-propyldisilane,
1,1,3,3-tetraisopropyldisilane,
1,3-diisopropyl-1,3-di-n-butyldisilane,
1,3-diisopropyl-1,3-diisobutyldisilane,
1,3-diisopropyl-1,3-di-sec-butyldisilane,
1,3-diisopropyl-1,3-diphenyldislane,
[0133] 1,3-diisopropyl-1,1,3,3-tetramethyldisilane,
1,3-diisopropyl-1,1,3,3-tetraethyldisilane,
1,3-diisopropyl-1,1,3,3-tetravinyldisilane,
1,3-diisopropyl-1,1,3,3-tetra-n-propyldisilane,
1,3-diisopropyl-1,1,3,3-tetra-n-butyldisilane,
1,3-diisopropyl-1,1,3,3-tetraisobutyldisilane,
1,3-diisopropyl-1,1,3,3-tetra-sec-butyldisilane,
1,3-diisopropyl-1,1,3,3-tetraphenyldislane,
[0134] 1,1,3,3-tetraisopropyl-1,3-dimethyldisilane,
1,1,3,3-tetraisopropyl-1,3-diethyldisilane,
1,1,3,3-tetraisopropyl-1,3-divinyldisilane,
1,1,3,3-tetraisopropyl-1,3-di-n-propyldisilane,
1,1,3,3-tetraisopropyl-1,3-di-n-propyldisilane,
1,1,3,3-tetraisopropyl-1,3-di-n-butyldisilane,
1,1,3,3-tetraisopropyl-1,3-diisobutyldisilane,
1,1,3,3-tetraisopropyl-1,3-di-sec-butyldisilane,
1,1,3,3-tetraisopropyl-1,3-diphenyldislane,
1,1,1,3,3,3-hexaisopropyldisilane,
[0135] 1,3-di-sec-butyldisilane,
[0136] 1,3-di-sec-butyl-1,3-dimethyldisilane,
1,3-di-sec-butyl-1,3-diethyldisilane,
1,3-di-sec-butyl-1,3-divinyldisilane,
1,3-di-sec-butyl-1,3-di-n-propyldisilane,
1,1,3,3-tetra-sec-butyldisilane,
1,3-di-sec-butyl-1,3-di-n-butyldisilane,
1,3-di-sec-butyl-1,3-diisobutyldisilane,
1,3-di-sec-butyl-1,3-di-sec-butyldisilane,
1,3-di-sec-butyl-1,3-diphenyldislane,
[0137] 1,3-di-sec-butyl-1,1,3,3-tetramethyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetraethyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetravinyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetra-n-propyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetra-n-butyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetraisobutyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetra-sec-butyldisilane,
1,3-di-sec-butyl-1,1,3,3-tetraphenyldislane,
[0138] 1,1,3,3-tetra-sec-butyl-1,3-dimethyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-diethyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-divinyldisilane,
1,1,3,3-tetra-sec-butylisopropyl-1,3-di-n-propyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-di-n-propyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-di-n-butyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-diisobutyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-di-sec-butyldisilane,
1,1,3,3-tetra-sec-butyl-1,3-diphenyldislane,
1,1,1,3,3,3-hexa-sec-butyldisilane,
[0139] 1,3-dicyclopentyldisilane,
[0140] 1,3-dicyclopentyl-1,3-dimethyldisilane,
1,3-dicyclopentyl-1,3-diethyldisilane,
1,3-dicyclopentyl-1,3-divinyldisilane,
1,3-dicyclopentyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentyldisilane,
1,3-dicyclopentyl-1,3-di-n-butyldisilane,
1,3-dicyclopentyl-1,3-diisobutyldisilane,
1,3-dicyclopentyl-1,3-di-sec-butyldisilane,
1,3-dicyclopentyl-1,3-diphenyldislane,
[0141] 1,3-dicyclopentyl-1,1,3,3-tetramethyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetraethyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetravinyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetra-n-propyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetra-n-butyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetraisobutyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetra-sec-butyldisilane,
1,3-dicyclopentyl-1,1,3,3-tetraphenyldislane,
[0142] 1,1,3,3-tetracyclopentyl-1,3-dimethyldisilane,
1,1,3,3-tetracyclopentyl-1,3-diethyldisilane,
1,1,3,3-tetracyclopentyl-1,3-divinyldisilane,
1,1,3,3-tetracyclopentyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentyl-1,3-di-n-butyldisilane,
1,1,3,3-tetracyclopentyl-1,3-diisobutyldisilane,
1,1,3,3-tetracyclopentyl-1,3-di-sec-butyldisilane,
1,1,3,3-tetracyclopentyl-1,3-diphenyldislane,
1,1,1,3,3,3-hexacyclopentyldislane,
[0143] 1,3-dicyclopentadienyldisilane,
[0144] 1,3-dicyclopentadienyl-1,3-dimethyldisilane,
1,3-dicyclopentadienyl-1,3-diethyldisilane,
1,3-dicyclopentadienyl-1,3-divinyldisilane,
1,3-dicyclopentadienyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentadienyldisilane,
1,3-dicyclopentadienyl-1,3-di-n-butyldisilane,
1,3-dicyclopentadienyl-1,3-diisobutyldisilane,
1,3-dicyclopentadienyl-1,3-di-sec-butyldisilane,
1,3-dicyclopentadienyl-1,3-diphenyldislane,
[0145] 1,3-dicyclopentadienyl-1,1,3,3-tetramethyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetraethyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetravinyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-n-propyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-n-butyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetraisobutyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetra-sec-butyldisilane,
1,3-dicyclopentadienyl-1,1,3,3-tetraphenyldislane,
[0146] 1,1,3,3-tetracyclopentadienyl-1,3-dimethyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-diethyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-divinyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-di-n-butyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-diisobutyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-di-sec-butyldisilane,
1,1,3,3-tetracyclopentadienyl-1,3-diphenyldislane,
1,1,1,3,3,3-hexacyclopentadienyldisilane,
[0147] 1,3-dicyclohexyldisilane,
[0148] 1,3-dicyclohexyl-1,3-dimethyldisilane,
1,3-dicyclohexyl-1,3-diethyldisilane,
1,3-dicyclohexyl-1,3-divinyldisilane,
1,3-dicyclohexyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclohexyldisilane,
1,3-dicyclohexyl-1,3-di-n-butyldisilane,
1,3-dicyclohexyl-1,3-diisobutyldisilane,
1,3-dicyclohexyl-1,3-di-sec-butyldisilane,
1,3-dicyclohexyl-1,3-diphenyldislane,
[0149] 1,3-dicyclohexyl-1,1,3,3-tetramethyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetraethyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetravinyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetra-n-propyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetra-n-butyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetraisobutyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetra-sec-butyldisilane,
1,3-dicyclohexyl-1,1,3,3-tetraphenyldislane,
[0150] 1,1,3,3-tetracyclohexyl-1,3-dimethyldisilane,
1,1,3,3-tetracyclohexyl-1,3-diethyldisilane,
1,1,3,3-tetracyclohexyl-1,3-divinyldisilane,
1,1,3,3-tetracyclohexyl-1,3-di-n-propyl disilane,
1,1,3,3-tetracyclohexyl-1,3-di-n-propyldisilane,
1,1,3,3-tetracyclohexyl-1,3-di-n-butyldisilane,
1,1,3,3-tetracyclohexyl-1,3-diisobutyldisilane,
1,1,3,3-tetracyclohexyl-1,3-di-sec-butyldisilane,
1,1,3,3-tetracyclohexyl-1,3-diisobutyldisilane,
1,1,3,3-tetracyclohexyl-1,3-diphenyldislane, and
1,1,1,3,3,3-hexacyclohexyldisilane.
[0151] Other examples include chain polysilanes such as
[0152] 1,2,3-triisopropyltrisilane,
1,1,2,2,3,3-hexaisopropyltrisilane,
1,2,3-hexaisopropyl-1,2,3-trimethyltrisilane,
1,2,3-hexaisopropyl-1,1,2,3,3-pentamethyltrisilane,
1,2,3,4-tetraisopropyltetrasilane,
1,1,2,2,3,3,4,4-octaisopropyltetrasilane,
1,2,3,4,5-pentaisopropylpentasilane,
1,1,2,2,3,3,4,4,5,5-decaisopropylpentasilane,
[0153] 1,2,3-tri-sec-butyltri silane, 1,1,2,2,3,3-hexa-sec-butyltri
silane, 1,2,3,4-tetra-sec-butyltetrasilane,
1,1,2,2,3,3,4,4-octa-sec-butyltetrasilane,
1,2,3,4,5-penta-sec-butylpentasilane, and
1,1,2,2,3,3,4,4,5,5-deca-sec-butylpentasilane,
[0154] Among others, isopropylsilane, isopropylmethylsilane,
isopropyldimethylsilane, diisopropylsilane,
diisopropylmethylsilane, triisopropylsilane, sec-butylsilane,
sec-butylmethylsilane, sec-butyldimethylsilane, di-sec-butylsilane,
di-sec-butylmethylsilane, tri-sec-butylsilane and the like are
preferred.
[0155] Specific examples of the cyclic silane compound represented
by formula (3) include cyclic polysilanes such as
[0156] 1,2,3,4-tetraisopropylcyclotetrasilane,
1,2,3,4,5-pentaisopropylcyclopentasilane,
1,2,3,4,5,6-hexaisopropylcyclohexasilane,
1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decaisopropylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undecaisopropylcyclohexasilane,
1,2,3,4-tetraisopropyl-1,2,3,4-tetramethylcyclotetrasilane,
1,2,3,4-tetraisopropyl-1,2,3,4-tetraethylcyclotetrasilane,
1,2,3,4-tetraisopropyl-1,2,3,4-tetraphenylcyclotetrasilane,
1,2,3,4,5-pentaisopropyl-1,2,3,4,5-pentamethylcyclopentasilane,
1,2,3,4,5-pentaisopropyl-1,2,3,4,5-pentaethylcyclopentasilane,
1,2,3,4,5-pentaisopropyl-1,2,3,4,5-pentaphenylcyclopentasilane,
1,2,3,4,5,6-hexaisopropyl-1,2,3,4,5,6-hexamethylcyclohexasilane,
1,2,3,4,5,6-hexaisopropyl-1,2,3,4,5,6-hexaethylcyclohexasilane,
1,2,3,4,5,6-hexaisopropyl-1,2,3,4,5,6-hexaphenylcyclohexasilane,
[0157] 1,2,3,4-tetra-sec-butylcyclotetrasilane,
1,2,3,4,5-penta-sec-butylcyclopentasilane,
1,2,3,4,5,6-hexa-sec-butylcyclohexasilane,
1,1,2,2,3,3,4,4-octa-sec-butylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-deca-sec-butylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undeca-sec-butylcyclohexasilane,
1,2,3,4-tetra-sec-butyl-1,2,3,4-tetramethylcyclotetrasilane,
1,2,3,4-tetra-sec-butyl-1,2,3,4-tetraethylcyclotetrasilane,
1,2,3,4-tetra-sec-butyl-1,2,3,4-tetraphenylcyclotetrasilane,
1,2,3,4,5-penta-sec-butyl-1,2,3,4,5-pentamethylcyclopentasilane,
1,2,3,4,5-penta-sec-butyl-1,2,3,4,5-pentaethylcyclopentasilane,
1,2,3,4,5-penta-sec-butyl-1,2,3,4,5-pentaphenylcyclopentasilane,
1,2,3,4,5,6-hexa-sec-butyl-1,2,3,4,5,6-hexamethylcyclohexasilane,
1,2,3,4,5,6-hexa-sec-butyl-1,2,3,4,5,6-hexaethylcyclohexasilane,
1,2,3,4,5,6-hexa-sec-butyl-1,2,3,4,5,6-hexaphenylcyclohexasilane,
[0158] 1,2,3,4-tetracyclopentylcyclotetrasilane,
1,2,3,4,5-pentacyclopentylcyclopentasilane,
1,2,3,4,5,6-hexacyclopentylcyclopentylcyclohexasilane,
1,1,2,2,3,3,4,4-octacyclopentylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decacyclopentylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undecacyclopentylcyclohexasilane,
1,2,3,4-tetracyclopentyl-1,2,3,4-tetramethylcyclotetrasilane,
1,2,3,4-tetracyclopentyl-1,2,3,4-tetraethylcyclotetrasilane,
1,2,3,4-tetracyclopentyl-1,2,3,4-tetraphenylcyclotetrasilane,
1,2,3,4,5-pentacyclopentyl-1,2,3,4,5-pentamethylcyclopentasilane,
1,2,3,4,5-pentacyclopentyl-1,2,3,4,5-pentaethylcyclopentasilane,
1,2,3,4,5-pentacyclopentyl-1,2,3,4,5-pentaphenylcyclopentasilane,
1,2,3,4,5,6-hexacyclopentyl-1,2,3,4,5,6-hexamethylcyclohexasilane,
1,2,3,4,5,6-hexacyclopentyl-1,2,3,4,5,6-hexaethylcyclohexasilane,
1,2,3,4,5,6-hexacyclopentyl-1,2,3,4,5,6-hexaphenylcyclohexasilane,
[0159] 1,2,3,4-tetracyclopentadienylcyclotetrasilane,
1,2,3,4,5-pentacyclopentadienylcyclopentasilane,
1,2,3,4,5,6-hexacyclopentylcyclopentadienylcyclohexasilane,
1,1,2,2,3,3,4,4-octacyclopentadienylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decacyclopentadienylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undecacyclopentadienylcyclohexasilane,
1,2,3,4-tetracyclopentadienyl-1,2,3,4-tetramethylcyclotetrasilane,
1,2,3,4-tetracyclopentadienyl-1,2,3,4-tetraethylcyclotetrasilane,
1,2,3,4-tetracyclopentadienyl-1,2,3,4-tetraphenylcyclotetrasilane,
1,2,3,4,5-pentacyclopentadienyl-1,2,3,4,5-pentamethylcyclopentasilane,
1,2,3,4,5-pentacyclopentadienyl-1,2,3,4,5-pentaethylcyclopentasilane,
1,2,3,4,5-pentacyclopentadienyl-1,2,3,4,5-pentaphenylcyclopentasilane,
1,2,3,4,5,6-hexacyclopentadienyl-1,2,3,4,5,6-hexamethylcyclohexasilane,
1,2,3,4,5,6-hexacyclopentadienyl-1,2,3,4,5,6-hexaethylcyclohexasilane,
1,2,3,4,5,6-hexacyclopentadienyl-1,2,3,4,5,6-hexaphenylcyclohexasilane,
[0160] 1,2,3,4-tetracyclohexylcyclotetrasilane,
1,2,3,4,5-hexycyclopentylcyclopentasilane,
1,2,3,4,5,6-hexacyclohexylcyclopentylcyclohexasilane,
1,1,2,2,3,3,4,4-octacyclohexylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decacyclohexylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undecacyclohexylcyclohexasilane,
1,2,3,4-tetracyclohexyl-1,2,3,4-tetramethylcyclotetrasilane,
1,2,3,4-tetracyclohexyl-1,2,3,4-tetraethylcyclotetrasilane,
1,2,3,4-tetracyclohexyl-1,2,3,4-tetraphenylcyclotetrasilane,
1,2,3,4,5-pentacyclohexyl-1,2,3,4,5-pentamethylcyclopentasilane,
1,2,3,4,5-pentacyclohexyl-1,2,3,4,5-pentaethylcyclopentasilane,
1,2,3,4,5-pentacyclohexyl-1,2,3,4,5-pentaphenylcyclopentasilane,
1,2,3,4,5,6-hexacyclohexyl-1,2,3,4,5,6-hexamethylcyclohexasilane,
1,2,3,4,5,6-hexacyclohexyl-1,2,3,4,5,6-hexaethylcyclohexasilane,
and
1,2,3,4,5,6-hexacyclohexyl-1,2,3,4,5,6-hexaphenylcyclohexasilane.
[0161] Among others, 1,2,3,4-tetraisopropylcyclotetrasilane,
1,2,3,4,5-pentaisopropylcyclopentasilane,
1,2,3,4,5,6-hexaisopropylcyclohexasilane,
1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane,
1,1,2,2,3,3,4,4,5,5-decaisopropylcyclopentasilane,
1,1,2,2,3,3,4,4,5,5,6,6-undecaisopropylcyclohexasilane, and the
like are preferred.
[0162] The production method for the silane compound and cyclic
silane compound of formulae (2) and (3) is not particularly
limited, but each compound can be produced by reacting an organic
compound represented by the following formula (8):
##STR00010##
(wherein R.sup.5, R.sup.6 and R.sup.9 are the same as respective
members in formula (2), and each X represents a hydrogen atom, a
chlorine atom, a bromine atom or an iodine atom) or represented by
the following formula (9):
##STR00011##
(wherein R.sup.10, R.sup.11 and R.sup.12 are the same as respective
members in formula (3), and each X represents a hydrogen atom, a
chlorine atom, a bromine atom or an iodine atom) with a metal
lithium particle.
[0163] In the case where an unreacted halogen substituent remains,
the unreacted halogen substituent may be alkylated by the reaction
with a lithium or magnesium compound obtained from formula (5) or
may be hydrogenated by the reaction with lithium aluminum hydride
or sodium borate.
[0164] The production conditions for the silane compound and cyclic
silane compound of formulae (2) and (3) are not particularly
limited, but the production conditions for the disiloxane compound
of formula (1) may be employed.
[0165] The organosilicon compound having, as in formulae (1) to (3)
of the present invention, a secondary hydrocarbon group directly
bonded to at least one silicon atom and having an atomic ratio of
0.5 or less oxygen atom with respect to 1 silicon atom can form a
carbon-containing silicon oxide film through deposition by CVD, and
the film can be used as a sealing film. CVD includes, for example,
PECVD and a catalytic chemical vapor deposition method. The kind of
PECVD and the apparatus used therefor are not particularly limited,
but PECVD generally employed in this technical field such as
semiconductor production field, liquid display production field and
surface treatment field of roll-to-roll polymer film is used.
[0166] In the PECVD set up, the organosilicon compound of the
present invention is vaporized by a vaporizer and introduced into a
deposition chamber, and a voltage is applied to an electrode in the
deposition chamber by means of a high-frequency power source to
generate plasma, whereby a plasma CVD thin film can be formed on a
silicon substrate or the like in the deposition chamber. At this
time, introducing an inert gas, such as helium, argon, krypton,
neon and xenon, together with the organosilicon compound so as to
generate plasma is also encompassed by the scope of the present
invention.
[0167] The plasma generation method of the PECVD set up is not
particularly limited, and inductively coupled plasma, capacitively
coupled plasma, ECR plasma and the like, which are used in this
art, can be used. As the plasma generation source, various types
such as parallel plate type and antenna type can be used, and PECVD
under any pressure condition such as atmospheric-pressure PECVD,
reduced-pressure PECVD or compressive PECVD can be used.
[0168] At this time, the PECVD conditions are not particularly
limited, but the chemical vapor deposition is preferably performed
at 1.0 to 10,000 W, more preferably from 1.0 to 2,000 W.
[0169] Also, a film densified or increased in the mechanical
strength can be sometimes obtained by subjecting a sealing film
composed of the above-described carbon-containing silicon oxide
film to a heat treatment, an ultraviolet irradiation treatment
and/or an electron beam treatment, and the film obtained after such
a treatment may be suitable as a gas barrier film.
[0170] The sealing film of the present invention can be used for an
FPD device, a semiconductor device and the like.
[0171] As the PECVD set up, FIG. 1 specifically depicts a parallel
plate capacitively coupled PECVD apparatus 1. The parallel plate
capacitively coupled PECVD apparatus shown in FIG. 1 has a shower
head upper electrode, a lower electrode capable of controlling the
temperature of a substrate, which are provided in a PECVD apparatus
chamber, a vaporization device for vaporizing the raw material
compound and feeding the vapor to the chamber, a plasma generation
device composed of a high-frequency power source and a matching
circuit, and an evacuation system composed of a vacuum pump.
[0172] The PECVD apparatus 1 consists of a PECVD chamber 2, an
upper electrode 3 having a shower head for uniformly feeding the
raw material compound into the chamber, a lower electrode 4 having
a temperature control device 8 and allowing a thin film-forming
substrate 5 such as Si substrate to be placed thereon, vaporization
devices 9 to 15 for vaporizing the raw material compound, a plasma
generation source, that is, a matching circuit 6 and an RF power
source 7, and an evacuation device 16 for discharging unreacted
materials and by-products from the chamber. Each of 17 and 18 is a
ground wire.
[0173] The matching circuit 6 and RF power source 7, which are a
plasma generation source, are connected to the upper electrode 3,
and plasma is generated by a discharge. The standards of the RF
power source 7 are not particularly limited, but an RF power source
employed in this technical field, having an electric power of 1 to
2,000 W, preferably from 10 to 1,000 W, and a frequency of 50 kHz
to 2.5 GHz, preferably from 100 kHz to 100 MHz, more preferably
from 200 kHz to 50 MHz, may be used.
[0174] The control of substrate temperature is not particularly
limited, but the temperature is from -90 to 1,000.degree. C.,
preferably from 0.degree. C. to 500.degree. C.
[0175] The vaporization device consists of a container 12 filled
with the raw material compound 13 that is a liquid at ordinary
temperature and atmospheric pressure, and equipped with a dip pipe
and a pipe 15 for applying a pressure from the above-described
insert gas, a liquid flow rate control device 10 for controlling
the flow rate of the raw material compound 13 in a liquid state, a
vaporizer 9 for vaporizing the liquid-state raw material compound
13, a pipe 14 for feeding the inert gas into the PECVD apparatus
chamber via the vaporizer, and a gas flow rate control device 11
for controlling the flow rate of the insert gas. The vaporization
device is pipe-connected from the vaporizer 9 to the upper
electrode 3 having a shower head.
[0176] The vapor feed rate of the raw material compound into the
chamber is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm. Also, the feed rate of the inert
gas is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm.
[0177] As the PECVD apparatus, FIG. 2 specifically depicts an
inductively coupled remote PECVD apparatus 19. The inductively
coupled remote PECVD apparatus shown in FIG. 2 has a plasma
generation part wound like a coil around quartz on the top of a
PECVD apparatus chamber, a temperature-controllable substrate
setting part, a vaporizer device for vaporizing the raw material
compound and feeding the vapor to the chamber, a plasma generation
device composed of a high-frequency power source and a matching
circuit, and an evacuation system composed of a vacuum pump.
[0178] The PECVD apparatus 19 consists of a PECVD chamber 20, a
plasma generation part, that is, a coil 21 and a quartz tube 22, a
heater part 23 for placing a thin film-forming substrate 24 such as
Si substrate thereon, a temperature control device 27, vaporization
devices 28 to 35 for vaporizing the raw material compound, a plasma
generation source, that is, a matching circuit 25 and an RF power
source 26, and an evacuation device 36 for discharging unreacted
materials and by-products from the chamber. Also, 37 is a ground
wire.
[0179] The coil around the quartz as a plasma generation part is
connected to the matching circuit 25, and a discharge is caused to
occur in the quartz tube by an antenna current magnetic field from
RF current. The standards of the RF power source 26 are not
particularly limited, but an RF power source employed in this
technical field, having an electric power of 1 to 2,000 W,
preferably from 10 to 1,000 W, and a frequency of 50 kHz to 2.5
GHz, preferably from 100 kHz to 100 MHz, more preferably from 200
kHz to 50 MHz, may be used.
[0180] The control of substrate temperature is not particularly
limited, but the temperature is from -90 to 1,000.degree. C.,
preferably from 0.degree. C. to 500.degree. C.
[0181] The vaporization device consists of a container 32 filled
with the raw material compound 33 that is a liquid at ordinary
temperature and atmospheric pressure, and equipped with a dip pipe
and a pipe 35 for applying a pressure from the above-described
insert gas, a liquid flow rate control device 29 for controlling
the flow rate of the raw material compound 33 in a liquid state, a
vaporizer 28 for vaporizing the liquid-state raw material compound
33, a pipe 34 for feeding the inert gas into the PECVD apparatus
chamber via the vaporizer, a gas flow rate control device 30 for
controlling the flow rate of the insert gas, and a shower head 31
for uniformly feeding the inert gas and the gasified raw material
compound 33 into the chamber.
[0182] The vapor feed rate of the raw material compound into the
chamber is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm. Also, the feed rate of the inert
gas is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm.
[0183] The raw material compound is gasified using the PECVD
apparatus illustrated above and after feeding the inert gas and the
gasified raw material compound or feeding the gasified raw material
into the chamber, plasma is generated by a discharge using an RF
power source to deposit a film on a temperature-controlled
substrate. At this time, the pressure in the chamber is not
particularly limited but is from 0.1 to 10,000 Pa, preferably from
1 to 5,000 Pa.
[0184] As the PECVD apparatus, FIG. 3 specifically depicts a
microwave PECVD apparatus 38. This apparatus consists of a
quartz-made chamber 39, a heater part 41 for placing a thin
film-forming substrate 40 such as Si substrate thereon, a
temperature control device 42, vaporization devices 43 to 50 for
vaporizing the raw material compound, a microwave generation
source, that is, a matching circuit 51 and a microwave transmitter
52, a microwave reflector 53, and an evacuation device 54 for
discharging unreacted materials and byproducts from the
chamber.
[0185] The matching circuit 51 and microwave transmitter 52, which
are a microwave generation source, are connected to the quartz
chamber, and the inside of the quartz chamber is irradiated with
microwave to generate plasma. The microwave frequency is not
particularly limited, but a microwave employed in this technical
field, having a frequency of 1 MHz to 50 GHz, preferably from 0.5
to 10 GHz, more preferably from 1 to 5 GHz, may be used. As for the
microwave output, a microwave of 0.1 to 20,000 W, preferably from 1
to 10,000 W, may be used.
[0186] The control of substrate temperature is not particularly
limited, but the temperature is from -90 to 1,000.degree. C.,
preferably from 0.degree. C. to 500.degree. C.
[0187] The vaporization device consists of a container 47 filled
with the raw material compound 48 that is a liquid at ordinary
temperature and atmospheric pressure, and equipped with a dip pipe
and a pipe 50 for applying a pressure from the above-described
insert gas, a liquid flow rate control device 44 for controlling
the flow rate of the raw material compound 48 in a liquid state, a
vaporizer 43 for vaporizing the liquid-state raw material compound
48, a pipe 49 for feeding the inert gas into the PECVD apparatus
chamber via the vaporizer, a gas flow rate control device 45 for
controlling the flow rate of the insert gas, and a shower head 46
for uniformly feeding the inert gas and the gasified raw material
compound 48 into the chamber.
[0188] The feed rate of the raw material compound vapor into the
chamber is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm. Also, the feed rate of the inert
gas is not particularly limited but is from 0.1 to 10,000 sccm,
preferably from 10 to 5,000 sccm.
[0189] The raw material compound is gasified using the PECVD
apparatus illustrated above and after feeding the inert gas and the
gasified raw material compound or feeding the gasified raw material
into the chamber, plasma is generated by microwave irradiation to
deposit a film on a temperature-controlled substrate. At this time,
the pressure in the chamber is not particularly limited but is from
0.1 to 10,000 Pa, preferably from 1 to 5,000 Pa.
EXAMPLES
[0190] Working examples are described below, but the present
invention is not limited to these Examples.
[0191] The film thickness was measured using a stylus surface
profile meter, Dektak 6M, manufactured by ULVAC. The composition of
the film produced was measured using ESCA5400MC manufactured by
Perkin Elmer. The oxygen permeability was measured in conformity
with JIS K 7126-1, and the water permeability was measured in
conformity with Appendix C of JIS K 7129. The total light
transmittance was measured by the method of JIS K 7361-1. The
linear expansion coefficient was calculated by heating a film
sample in a no-load state at 5 deg./min from room temperature to
240.degree. C. in an oven and measuring the change in the film
thickness during the temperature rise by a CCD camera. The surface
roughness was measured using a scanning probe microscope, NanoScope
Ma, manufactured by Veecoo by tapping mode AFM.
Example 1
Deposition of a Gas Barrier Layer by Using
1,3-Diisopropyl-1,3-Dimethyldisiloxane (Compound Represented by
Formula (1) where Oxygen/Silicon=0.5) in a Capacitively Coupled
PECVD Apparatus
[0192] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
1,3-diisopropyl-1,3-dimethyldisiloxane flow rate of 50 sccm, a
helium gas flow rate of 50 sccm, an oxygen gas flow rate of 50
sccm, an in-chamber pressure of 10 Pa, a substrate temperature of
room temperature, an RF source power of 500 W, an RF source
frequency of 13.56 MHz, and a deposition time of 10 minutes.
[0193] As a result, the film thickness was 2,570 nm. The
composition of the carbon-containing silicon oxide sealing film was
Si=24 atom %, C=20 atom % and O=56 atom %. When the gas
permeability was measured, the oxygen permeability was less than
0.01 cc/m.sup.2day (not more than detection limit), and the water
permeability was 4.0.times.10.sup.-3 g/m.sup.2day. Also, the total
light transmittance was 91.7%, the linear expansion coefficient was
12 ppm/deg., and the surface roughness was 0.25 nm.
Example 2
Deposition of a Gas Barrier Layer by Using
1,3-Diisopropyl-1,3-Dimethyldisiloxane (Compound Represented by
Formula (1) where Oxygen/Silicon=0.5) in a Capacitively Coupled
PECVD Apparatus
[0194] A sealing film was deposited in the same manner as in
Example 1 except that in Example 1, the flow rate was changed to 50
sccm for helium and to 100 sccm for oxygen.
[0195] As a result, the film thickness was 1,421 nm. When the gas
permeability was measured, the oxygen permeability was less than
0.01 cc/m.sup.2day (not more than detection limit), and the water
permeability was 2.5.times.10.sup.-3 g/m.sup.2day. Also, the total
light transmittance was 91.6%, the linear expansion coefficient was
11 ppm/deg., and the surface roughness was 0.27 nm.
Example 3
Deposition of a Gas Barrier Layer by Using
1,3-Diisopropyl-1,3-Dimethyldisiloxane (Compound Represented by
Formula (1) where Oxygen/Silicon=0.5) in a Capacitively Coupled
PECVD Apparatus
[0196] A sealing film was deposited in the same manner as in
Example 1 except that in Example 1, the flow rate was changed to 50
sccm for helium and to 500 sccm for oxygen.
[0197] As a result, the film thickness was 1,050 nm. When the gas
permeability was measured, the oxygen permeability was less than
0.01 cc/m.sup.2day (not more than detection limit), and the water
permeability was 1.1.times.10.sup.-3 g/m.sup.2day. Also, the total
light transmittance was 91.7%, the linear expansion coefficient was
12 ppm/deg., and the surface roughness was 0.25 nm.
Example 4
Deposition of a Gas Barrier Layer by Using Diisopropylmethylsilane
(Compound Represented by Formula (2) where Oxygen/Silicon=0) in a
Capacitively Coupled PECVD Apparatus
[0198] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
vaporized diisopropylmethylsilane flow rate of 50 sccm, a helium
gas flow rate of 50 sccm, an oxygen gas flow rate of 50 sccm, an
in-chamber pressure of 10 Pa, a substrate temperature of room
temperature, an RF source power of 500 W, an RF source frequency of
13.56 MHz, and a deposition time of 10 minutes.
[0199] As a result, the film thickness was 2,180 nm. The
composition of the carbon-containing silicon oxide sealing film was
Si=25 atom %, C=16 atom % and O=59 atom %. When the gas
permeability was measured, the oxygen permeability was less than
0.01 cc/m.sup.2day (not more than detection limit), and the water
permeability was 3.5.times.10.sup.-3 g/m.sup.2day. Also, the total
light transmittance was 91.7%, the linear expansion coefficient was
11 ppm/deg., and the surface roughness was 0.26 nm.
Example 5
Deposition of a Gas Barrier Layer by Using
1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane (Compound Represented
by Formula (3) where Oxygen/Silicon=0) in a Capacitively Coupled
PECVD Apparatus
[0200] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
vaporized 1,1,2,2,3,3,4,4-octaisopropylcyclotetrasilane flow rate
of 50 sccm, a helium gas flow rate of 50 sccm, an oxygen gas flow
rate of 100 sccm, an in-chamber pressure of 10 Pa, a substrate
temperature of room temperature, an RF source power of 500 W, an RF
source frequency of 13.56 MHz, and a deposition time of 10
minutes.
[0201] As a result, the film thickness was 2,830 nm. The
composition of the carbon-containing silicon oxide sealing film was
Si=27 atom %, C=17 atom % and O=56 atom %. When the gas
permeability was measured, the oxygen permeability was less than
0.01 cc/m.sup.2day (not more than detection limit), and the water
permeability was 2.4.times.10.sup.-3 g/m.sup.2day. Also, the total
light transmittance was 91.6%, the linear expansion coefficient was
11 ppm/deg., and the surface roughness was 0.28 nm.
Comparative Example 1
Deposition of a Carbon-Containing Silicon Oxide Sealing Film by
Using Vinyltrimethoxysilane (Oxygen/Silicon=3.0) in a Capacitively
Coupled PECVD Apparatus
[0202] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
vaporized vinyltrimethoxysilane flow rate of 50 sccm, a helium gas
flow rate of 50 sccm, an in-chamber pressure of 133 Pa, a substrate
temperature of room temperature, an RF source power of 200 W, an RF
source frequency of 13.56 MHz, and a deposition time of 10 minutes.
As a result, the film thickness was 470 nm. The composition of the
carbon-containing silicon oxide sealing film was Si=31 atom %, C=20
atom % and O=49 atom %. When the gas permeability was measured, the
oxygen permeability was less than 1.44 cc/m.sup.2day, and the water
permeability was 1.67 g/m.sup.2day. Also, the total light
transmittance was 86.5%, the linear expansion coefficient was 30
ppm/deg., and the surface roughness was 10 nm.
[0203] An organosilicon compound having an atomic ratio of 0.5 or
less oxygen atom with respect to 1 silicon atom was not used and
therefore, the obtained thin film was unsuited for a gas barrier
layer.
Comparative Example 2
Deposition of a Carbon-Containing Silicon Oxide Sealing Film by
Using Tetramethoxysilane (Oxygen/Silicon=4.0) in a Capacitively
Coupled PECVD Apparatus
[0204] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
vaporized tetramethoxysilane flow rate of 50 sccm, a helium gas
flow rate of 50 sccm, an in-chamber pressure of 133 Pa, a substrate
temperature of room temperature, an RF source power of 200 W, an RF
source frequency of 13.56 MHz, and a deposition time of 10
minutes.
[0205] As a result, the film thickness was 136 nm. The composition
of the carbon-containing silicon oxide sealing film was Si=35 atom
%, C=13 atom % and O=52 atom %. When the gas permeability was
measured, the oxygen permeability was less than 1.75 cc/m.sup.2day,
and the water permeability was 1.67 g/m.sup.2day. Also, the total
light transmittance was 86.4%, the linear expansion coefficient was
32 ppm/deg., and the surface roughness was 26 nm.
[0206] An organosilicon compound having an atomic ratio of 0.5 or
less oxygen atom with respect to 1 silicon atom was not used and
therefore, the obtained thin film was unsuited for a gas barrier
layer.
Comparative Example 3
[0207] The gas permeability, total light transmittance, linear
expansion coefficient and surface roughness of the polyethylene
naphthalate film substrate used were measured, as a result, the
oxygen permeability was 21.0 cc/m.sup.2day, and the water
permeability was 6.70 g/m.sup.2day. Also, the total light
transmittance was 86.9%, the linear expansion coefficient was 35
ppm/deg., and the surface roughness was 1.4 nm.
Example 6
Deposition of a Gas Barrier Layer by Using Diisopropylmethylsilane
(Compound Represented by Formula (2) where Oxygen/Silicon=0) in a
Capacitively Coupled PECVD Apparatus
[0208] A film was deposited on a polyethylene naphthalate film
substrate by using a parallel plate capacitively coupled PECVD
apparatus shown in FIG. 1. The deposition conditions were a
vaporized diisopropylmethylsilane flow rate of 50 sccm, a helium
gas flow rate of 50 sccm, an oxygen gas flow rate of 500 sccm, an
in-chamber pressure of 100 Pa, a substrate temperature of room
temperature, an RF source power of 1,000 W, an RF source frequency
of 13.56 MHz, and a deposition time of 10 minutes.
[0209] As a result, the film thickness was 858 nm. The composition
of the carbon-containing silicon oxide sealing film was Si=31 atom
%, C=9 atom % and O=60 atom %. When the gas permeability was
measured, the oxygen permeability was less than 0.01 cc/m.sup.2day
(not more than detection limit), and the water permeability was
2.1.times.10.sup.-4 g/m.sup.2day. Also, the total light
transmittance was 91.8%, the linear expansion coefficient was 11
ppm/deg., and the surface roughness was 0.21 nm.
[0210] While the invention has been described in detail and with
reference to specific embodiments thereof, it will be apparent to
one skilled in the art that various changes and modifications can
be made therein without departing from the spirit and scope of the
invention.
[0211] This application is based on Japanese Patent Application
(Patent Application No. 2011-192741) filed on Sep. 5, 2011 and
Japanese Patent Application (Patent Application No. 2012-176433)
filed on Aug. 8, 2012, the contents of which are incorporated
herein by way of reference.
INDUSTRIAL APPLICABILITY
[0212] According to the present invention, a film deposition
material containing an organosilicon compound having a secondary
hydrocarbon group directly bonded to at least one silicon atom and
having an atomic ratio of 0.5 or less oxygen atom with respect to 1
silicon atom can be deposited by CVD to form a carbon-containing
silicon oxide film, and the film can be used as a sealing film.
Above all, this sealing film is very useful as a gas barrier film
or a gas barrier layer for a gas barrier substrate. Hence, the
industrial value of the present invention is remarkable.
EXPLANATIONS OF REFERENCE SIGNS
[0213] 1: Parallel plate capacitively coupled PECVD apparatus
[0214] 2: PECVD Chamber [0215] 3: Upper electrode having a shower
head [0216] 4: Lower Electrode [0217] 5: Thin film-forming
substrate [0218] 6: Matching circuit [0219] 7: RF Power source
[0220] 8: Temperature control device [0221] 9: Vaporizer [0222] 10:
Liquid flow rate control device [0223] 11: Gas flow rate control
device [0224] 12: Container [0225] 13: Raw material compound [0226]
14: Pipe for feeding an inert gas into PECVD apparatus chamber via
vaporizer [0227] 15: Pipe for applying a pressure from an insert
gas [0228] 16: Evacuation device [0229] 17: Ground wire [0230] 18:
Ground wire [0231] 19: Inductively coupled remote PECVD apparatus
[0232] 20: PECVD Chamber [0233] 21: Coil [0234] 22: Quartz tube
[0235] 23: Heater part [0236] 24: Thin film-forming substrate
[0237] 25: Matching circuit [0238] 26: RF Power source [0239] 27:
Temperature control device [0240] 28: Vaporizer [0241] 29: Liquid
flow rate control device [0242] 30: Gas flow rate control device
[0243] 31: Shower head [0244] 32: Container [0245] 33: Raw material
compound [0246] 34: Pipe for feeding an inert gas into PECVD
apparatus chamber via vaporizer [0247] 35: Pipe for applying a
pressure from an insert gas [0248] 36: Evacuation device [0249] 37:
Ground wire [0250] 38: Microwave PECVD apparatus [0251] 39:
Quartz-made chamber [0252] 40: Thin film-forming substrate [0253]
41: Heater part [0254] 42: Temperature control device [0255] 43:
Vaporizer [0256] 44: Liquid flow rate control device [0257] 45: Gas
flow rate control device [0258] 46: Shower head [0259] 47:
Container [0260] 48: Raw material compound [0261] 49: Pipe for
feeding an inert gas into PECVD apparatus chamber via vaporizer
[0262] 50: Pipe for applying a pressure from an insert gas [0263]
51: Matching circuit [0264] 52: Microwave transmitter [0265] 53:
Microwave reflector [0266] 54: Evacuation device
* * * * *