Stock material or miscellaneous articles – Composite – Of silicon containing
Reexamination Certificate
2002-03-14
2004-09-07
Robertson, Jeffrey B. (Department: 1712)
Stock material or miscellaneous articles
Composite
Of silicon containing
C427S387000, C525S478000, C525S479000, C528S025000, C528S031000, C528S032000
Reexamination Certificate
active
06787241
ABSTRACT:
BACKGROUND OF THE INVENTION
This invention relates to a film obtained from a heat resisting silsesquioxane polymer and a cured film thereof. The present invention is also directed to a method of preparing the film. The present invention is further directed to a composite material having the above film or cured film.
The present inventors disclose in Japanese patents Nos. 2,884,073, 2884074 and 3,020,164 a hydrosilylated polymer obtained by reacting octakis(hydridosilsesquioxane), namely pentacyclo-[9.5.1.1
3,9
.1
5,15
.1
7,13
]-ocatasiloxane, which is one of a cage-type hydridosilsesquioxanes, with a monoyne or diyne compound. In the hydrosilylated polymer, part of the hydrogen atoms bonded to the silicon atoms thereof may be substituted by an alkyl group or an aralkyl group. This polymer, which is soluble in organic solvents, is highly thermally stable. Japanese patent No. 2,884,073 also disclose the formation of a film by applying an organic solution of the hydrosilylated polymer to a glass substrate. The coating is dried at room temperature in a nitrogen gas flow and then in vacuum. The resulting film, however, has been found to form cracks and is relatively easily delaminated from the substrate.
SUMMARY OF THE INVENTION
It is, therefore, an object of the present invention to provide a film of a hydrosilylated polymer which is free of defects such as cracks and which can be tightly adhered to a substrate.
Another object of the present invention is to provide a film of the above-mentioned type which does not absorb moisture and which has high water resistance, high resistance to chemicals, good weatherability, good electric insulation properties and high mechanical strengths.
In accordance with one aspect of the present invention, there is provided a film obtained by heating a coating of a resin composition at a temperature lower than 300° C. but not lower than 40° C. in air or in an inert atmosphere, said resin composition comprising a hydrosilylated polymer obtained by reacting at least one hydridosilsesquioxane compound of the following formula (1):
(HSiO
3/2
)
n
(1)
wherein n is an integer of 4-1000, with at least one compound of the following formula (2)
R
1
—C≡C—R
2
(2)
wherein R
1
represents a hydrogen atom, a monovalent organic group or a monovalent organosilicon group and R
2
represents a hydrogen atom or a group of the formula:
—(R′)
q
—C≡C—R
where R′ represents a divalent organic group or a divalent organometallic group, R represents a monovalent organic group or a monovalent organosilicon group and q is 0 or 1
with the proviso that when R
1
is a hydrogen atom R
2
is a hydrogen atom.
In another aspect, the present invention provides a method of preparing a film, comprising applying a coating of a composition to a substrate, and heating said coating at a temperature lower than 300° C. but not lower than 40° C. in air or in an inert atmosphere for a period of time sufficient to form a film on said substrate, said composition comprising a hydrosilylated polymer obtained by reacting at least one hydridosilsesquioxane compound of the following formula (1):
(HSiO
3/2
)
n
(1)
wherein n is an integer of 4-1000, with at least one compound of the following formula (2)
R
1
—C≡C—R
2
(2)
wherein R
1
represents a hydrogen atom, a monovalent organic group or a monovalent organosilicon group and R
2
represents a hydrogen atom or a group of the formula:
—(R′)
q
—C≡C—R
where R′ represents a divalent organic group or a divalent organometallic group, R represents a monovalent organic group or a monovalent organosilicon group and q is 0 or 1
with the proviso that when R
1
is a hydrogen atom R
2
is a hydrogen atom.
The present invention also provides a cured film obtained by heating the above film at a temperature of 300-1500° C. in an inert atmosphere.
The present invention further provides a method of preparing a cured film, comprising heating the above film at a temperature of 300-1500° C. in an inert atmosphere for a period of at least 1 minute.
The present invention further provides a composite material comprising a substrate, and the above film or cured film provided on said substrate.
The present invention further provides a semiconductor device having the above film or cured film.
The above film or cured film according to the present invention is suitably used for various applications such as a protecting film (e.g. a passivation film of a semiconductor), a barrier coat film, a resist film, an insulation film (e.g. an interlayer insulation film of a semiconductor) and a heat resisting film.
REFERENCES:
patent: 4847162 (1989-07-01), Haluska et al.
patent: 5336532 (1994-08-01), Haluska et al.
patent: 5506177 (1996-04-01), Kishimoto et al.
patent: 5899751 (1999-05-01), Chang et al.
patent: 5942638 (1999-08-01), Lichtenhan et al.
patent: 6143360 (2000-11-01), Zhong
patent: 6175031 (2001-01-01), Tachikawa
patent: 6410772 (2002-06-01), Okuyama et al.
English Translation of JP 09-296044, Kobayashi et al, Nov. 1997, from JPO web-site.*
English Translation of JP 2000-212285, Kobayashi et al, Aug. 2000, from JPO web-site.*
English Translation of JP 2001-343631, Katsuragawa, Dec. 2001, from JPO web-site.*
N. Auner et al, “Chemistry of Hydrogen-Octasilsesquioxane . . . ” Chem. Mater., vol. 12, pp. 3402-3418.
Kobayashi et al, “Synthesis of Highly Heat-Resistant Soluble . . . ” Chemistry Letters, 1998, pp. 763,764.
Patent Abstracts of Japan, vol. 1998, No. 3, Feb. 27, 1998 & JP 09 296044.
Patent Abstracts of Japan, vol. 1998, No. 3, Feb. 27, 1998 & JP 09 296043.
Hayashi Teruyuki
Kobayashi Toshi-aki
Tanaka Masato
Yamaguchi Kouichi
Lorusso, Loud & Kelly
National Institute of Advanced Industrial Science and Technology
Robertson Jeffrey B.
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