Stock material or miscellaneous articles – Composite – Of silicon containing
Reexamination Certificate
2001-02-26
2002-07-02
Dawson, Robert (Department: 1712)
Stock material or miscellaneous articles
Composite
Of silicon containing
C525S100000, C525S102000, C525S474000, C524S588000, C524S858000, C528S021000
Reexamination Certificate
active
06413647
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to a composition for film formation. More particularly, the invention relates to a composition for film formation which, when used as an interlayer insulating film material in the production of semiconductor devices and the like, can give a silica-based film excellent in dielectric constant characteristics and mechanical strength.
BACKGROUND OF THE INVENTION
Silica (SiO
2
) films formed by vacuum processes such as the CVD method have hitherto been used frequently as interlayer insulating films in semiconductor devices and other devices. In recent years, an insulating coating film which comprises a tetraalkoxysilane hydrolyzate as the main component and is called an SOG (spin on glass) film has come to be used for the purpose of forming a more even interlayer insulating film. Furthermore, as a result of the trend toward higher degree of integration in semiconductor devices and the like, an interlayer insulating film called an organic SOG film has been developed which comprises a polyorganosiloxane as the main component and has a low dielectric constant.
However, with further progress in the degree of integration or multilayer constitution in semiconductor devices and the like, better electrical insulation between conductors has come to be required and, hence, an interlayer insulating film material having a lower dielectric constant and excellent cracking resistance has come to be desired.
Proposed as materials having a low dielectric constant are a composition comprising a mixture of fine particles obtained by condensing an alkoxysilane in the presence of ammonia and a basic product of partial hydrolysis of an alkoxysilane (see JP-A-5-263045 (the term “JP-A” as used herein means an “unexamined published Japanese patent application”) and JP-A-5-315319) and a coating fluid obtained by condensing a basic hydrolyzate of a polyalkoxysilane in the presence of ammonia (see JP-A-11-340219 and JP-A-11-340220). However, the materials obtained by these methods each has a dielectric constant exceeding 2.5 and has hence been insufficient for the progress of the degree of integration or multilayer constitution in semiconductor devices and the like.
SUMMARY OF THE INVENTION
One object of the invention is to provide a composition for film formation which eliminates the problem described above. More particularly, the object is to provide a composition for film formation which is capable of giving a silica-based coating film having an exceeding low dielectric constant and improved mechanical strength and useful as an interlayer insulating film in semiconductor devices and the like.
Another object of the invention is to provide a process for producing the composition.
Still another object of the invention is to provide a silica-based film obtained from the composition.
The invention provides a composition for film formation which comprises:
(A) a product of hydrolysis and condensation (hereinafter referred to also as “product of hydrolysis and condensation (A)”) obtained by hydrolyzing and condensing one or more silane compounds selected from the group consisting of compounds represented by the following formula (1) (hereinafter referred to also as “compounds (1)”), compounds represented by the following formula (2) (hereinafter referred to also as “compounds (2)”), and compounds represented by the following formula (3) (hereinafter referred to also as “compounds (3)”) in the presence of 0.2 mol or more of an alkaline compound per mol of the silane compounds,
R
a
Si(OR
1
)
4−a
(1)
wherein R represents a hydrogen atom, a fluorine atom, or a monovalent organic group; R
1
represents a monovalent organic group; and a is an integer of 1 or 2;
Si(OR
2
)
4
(2)
wherein R
2
represents a monovalent organic group;
R
3
b
(R
4
O)
3−b
Si—(R
7
)
d
—Si(OR
5
)
3−c
R
6
c
(3)
wherein R
3
to R
6
may be the same or different and each represents a monovalent organic group; b and c may be the same or different and each is a number of 0 to 2; R
7
represents an oxygen atom, a phenylene group, or a group represented by —(CH
2
)
n
—, wherein n is an integer of 1 to 6; and d is 0 or 1; and
(B) an organic solvent.
The invention further provides a method of film formation which comprises applying the composition for film formation described above to a substrate and then heating the resultant coating.
The invention furthermore provides a silica-based film obtained by the method of film formation described film.
DETAILED DESCRIPTION OF THE INVENTION
The product of hydrolysis and condensation (A) in the invention means a mixture of a hydrolyzate of at least one member selected from the group consisting of the compounds (1) to (3) and a condensate of the hydrolyzate, or means either of the hydrolyzate and the condensate.
In the hydrolyzate in ingredient (A) all the R
1
O—, R
2
O—, R
4
O—, and R
5
O— groups contained in compounds (1) to (3) to constitute ingredient (A) need not have been hydrolyzed. For example, the hydrolyzate may be one in which only one of those groups has been hydrolyzed or two or more thereof have been hydrolyzed or may be a mixture of these.
The condensate in ingredient (A) means a product formed from the hydrolyzate of compounds (1) to (3) to constitute ingredient (A) by condensing silanol groups of the hydrolyzate to form Si—O—Si bonds. In the invention, however, all the silanol groups need not have undergone condensation. Namely, the term “condensate” as used herein means a concept which includes, for example, a condensate in which a slight proportion of the silanol groups have been condensed and a mixture of condensates which differ in the degree of condensation.
Product of Hydrolysis and Condensation (A)
The product of hydrolysis and condensation (A) is obtained by hydrolyzing and condensing, in the presence of a specific amount of an alkaline compound, at least one silane compound selected from the group consisting of compounds (1) to (3).
Compounds (1)
Examples of the monovalent organic groups represented by R and R
1
in formula (1) include alkyl, aryl, allyl, and glycidyl groups. In formula (1), R is preferably a monovalent organic group, more preferably an alkyl or phenyl group.
The alkyl group preferably has 1 to 5 carbon atoms, and examples thereof include methyl, ethyl, propyl, and butyl. These alkyl groups may be linear or branched, and may be ones in which one or more of the hydrogen atoms have been replaced, for example, with fluorine atoms.
In formula (1), examples of the aryl group include phenyl, naphthyl, methylphenyl, ethylphenyl, chlorophenyl, bromophenyl, and fluorophenyl.
Specific examples of the compounds (1) include: trimethoxysilane, triethoxysilane, tri-n-propoxysilane, triisopropoxysilane, tri-n-butoxysilane, tri-sec-butoxysilane, tri-tert-butoxysilane, triphenoxysilane, fluorotrimethoxysilane, fluorotriethoxysilane, fluorotri-n-propoxysilane, fluorotriisopropoxysilane, fluorotri-n-butoxysilane, fluorotri-sec-butoxysilane, fluorotri-tert-butoxysilane, and fluorotriphenoxysilane; methyltrimethoxysilane, methyltriethoxysilane, methyltri-n-propoxysilane, methyltri-iso-propoxysilane, methyltri-n-butoxysilane, methyltri-sec-butoxysilane, methyltri-tert-butoxysilane, methyltriphenoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, ethyltri-n-propoxysilane, ethyltri-iso-propoxysilane, ethyltri-n-butoxysilane, ethyltri-sec-butoxysilane, ethyltri-tert-butoxysilane, ethyltriphenoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltri-n-propoxysilane, vinyltri-iso-propoxysilane, vinyltri-n-butoxysilane, vinyltri-sec-butoxysilane, vinyltri-tert-butoxysilane, vinyltriphenoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, n-propyltri-n-propoxysilane, n-propyltriisopropoxysilane, n-propyltri-n-butoxysilane, n-propyltri-sec-butoxysilane, n-propyltri-tert-butoxysilane, n-propyltriphenoxysilane, isopropyltrimethoxysilane, isopropyltriethoxysilane, isopropyltri-n-propoxysilane, isopropyltriisopropoxysilane, isopropyltri-n-butoxysilane, isopropyltri-sec-butoxysilane, isopropyl
Hasegawa Kouichi
Hayashi Eiji
Youngsoo Seo
Dawson Robert
JSR Corporation
Keehan Christopher M.
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
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