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US4535007A
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Silicon nitride-containing ceramics
Assignee: Dow Silicones Corp
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Filing: 1984-07-02
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Granted: 1985-08-13
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Expires: 2004-07-02
Abstract
Abstract What is disclosed is a process for preparing a silicon nitride-containing ceramic material from a R 3 SiNH-containing silazane polymer, which has been rendered infusible by treatment with certain reactive metal halides, by heating the infusible silazane polymer to an elevated temperature under an inert atmosphere. Suitable reactive metal halides are of the general formula MX n or R b SiX.sub.(4-b) where M is a metal atom of valence n, X is chlorine or bromine, R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms, and b has a value of 0, 1, or 2. Preferred reactive metal halides are SiCl 4 and HSiCl 3 .
Inventors
- 👤 John P. Cannady
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 16:59
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/60; C08G77/62; C04; C04B; C04B35/00; C04B35/515; C04B35/58; C04B35/584; C04B35/589
Claims Analysis
Total Claims: 54
Claim 1
Independent Claim
175 words
A method of preparing a silicon nitride-containing ceramic material, which method comprises (1) treating a R 3 SiNH-containing silazane polymer with a reactive metal halide of general formula MX n or R b SiX.sub.(4-b) at a temperature below the softening point of the R 3 SiNH-containing silazane polymer for a time sufficient to render the silazane polymer infusible where R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; M is a metal atom of valence n; X is a halide atom selected from the group consisting of chlorine and bromine; and b has a value of 0, 1, or 2; where said reactive metal halide has fewer carbon atoms than the R 3 SiNH-endblocking group; and where said reactive metal halide has at least two halide atoms; and (2) heating the infusible silazane polymer of step (1) in an inert atmosphere or vacuum to a temperature of at least 750° C. until said infusible silazane polymer is converted to a silicon nitride-containing ceramic material.
Claim 2
Independent Claim
175 words
A method of preparing a silicon nitride-containing ceramic material, which method comprises (1) treating a R 3 SiNH-containing silazane polymer with a reactive metal halide of general formula MX n or R b SiX.sub.(4-b) at a temperature below the softening point of the R 3 SiNH-containing silazane polymer for a time sufficient to render the silazane polymer infusible where R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; M is a metal atom of valence n; X is a halide atom selected from the group consisting of chlorine and bromine; and b has a value of 0, 1, or 2; where said reactive metal halide has fewer carbon atoms than the R 3 SiNH-endblocking group; and where said reactive metal halide has at least two halide atoms; and (2) heating the infusible silazane polymer of step (1) in an inert atmosphere or vacuum to a temperature of at least 750° C. until said infusible silazane polymer is converted to a silicon nitride-containing ceramic material.
Claim 3
Dependent Claim
113 words
A method as defined in claim 1 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, an organochlorosilane or a mixture of organochlorosilanes of general formula R'.sub.c SiCl.sub.(4-c) with a disilazane of general formula (R.sub.3 Si).sub.2 NH at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein R' is selected from the group consisting of vinyl, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; and c has a value of 1 or 2.
Claim 4
Dependent Claim
132 words
A method as defined in claim 1 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, a chlorine-containing disilane or a mixture of chlorine-containing disilazanes, of general formula (Cl.sub.d R'.sub.e Si).sub.2 with a disilazane of general formula (R.sub.3 Si).sub.2 NH at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein R' is selected from the group consisting of vinyl, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; d has a value of 0.5 to 3; e has a value of 0 to 2.5; and the sum of (d+e) is equal to 3.
Claim 5
Dependent Claim
78 words
A method as defined in claim 1 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, trichlorosilane with a disilazane at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein said disilazane has the general formula (R.sub.3 Si).sub.2 NH where R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms.
Claim 6
Dependent Claim
19 words
A method as defined in claim 1 wherein said reactive metal halide is of general formula MX n .
Claim 7
Dependent Claim
19 words
A method as defined in claim 2 wherein said reactive metal halide is of general formula MX n .
Claim 8
Dependent Claim
19 words
A method as defined in claim 3 wherein said reactive metal halide is of general formula MX n .
Claim 9
Dependent Claim
19 words
A method as defined in claim 4 wherein said reactive metal halide is of general formula MX n .
Claim 10
Dependent Claim
38 words
A method as defined in claim 5 whereas said reactive metal halide is selected from the group consisting of BCl 3 , BBr 3 , PCl 3 , PBr 3 , ZrCl 4 , and SnCl 4 .
Claim 11
Dependent Claim
38 words
A method as defined in claim 6 whereas said reactive metal halide is selected from the group consisting of BCl 3 , BBr 3 , PCl 3 , PBr 3 , ZrCl 4 , and SnCl 4 .
Claim 12
Dependent Claim
38 words
A method as defined in claim 7 whereas said reactive metal halide is selected from the group consisting of BCl 3 , BBr 3 , PCl 3 , PBr 3 , ZrCl 4 , and SnCl 4 .
Claim 13
Dependent Claim
38 words
A method as defined in claim 8 whereas said reactive metal halide is selected from the group consisting of BCl 3 , BBr 3 , PCl 3 , PBr 3 , ZrCl 4 , and SnCl 4 .
Claim 14
Dependent Claim
20 words
A method as defined in claim 1 wherein said reactive metal halide is of the general formula R b SiX.sub.(4-b).
Claim 15
Dependent Claim
20 words
A method as defined in claim 2 wherein said reactive metal halide is of the general formula R b SiX.sub.(4-b).
Claim 16
Dependent Claim
20 words
A method as defined in claim 3 wherein said reactive metal halide is of the general formula R b SiX.sub.(4-b).
Claim 17
Dependent Claim
20 words
A method as defined in claim 4 wherein said reactive metal halide is of the general formula R b SiX.sub.(4-b).
Claim 18
Dependent Claim
59 words
A method as defined in claim 13 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 , SiCl 4 , CH 3 SiCl 3 , CH 3 CH 2 SiCl 3 , C 6 H 5 SiCl 3 , CH 2 ═CH 2 SiCl 3 , and (CH 3 ) 2 SiCl 2 .
Claim 19
Dependent Claim
59 words
A method as defined in claim 14 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 , SiCl 4 , CH 3 SiCl 3 , CH 3 CH 2 SiCl 3 , C 6 H 5 SiCl 3 , CH 2 ═CH 2 SiCl 3 , and (CH 3 ) 2 SiCl 2 .
Claim 20
Dependent Claim
59 words
A method as defined in claim 15 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 , SiCl 4 , CH 3 SiCl 3 , CH 3 CH 2 SiCl 3 , C 6 H 5 SiCl 3 , CH 2 ═CH 2 SiCl 3 , and (CH 3 ) 2 SiCl 2 .
Claim 21
Dependent Claim
59 words
A method as defined in claim 16 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 , SiCl 4 , CH 3 SiCl 3 , CH 3 CH 2 SiCl 3 , C 6 H 5 SiCl 3 , CH 2 ═CH 2 SiCl 3 , and (CH 3 ) 2 SiCl 2 .
Claim 22
Dependent Claim
25 words
A method as defined in claim 17 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 and SiCl 4 .
Claim 23
Dependent Claim
25 words
A method as defined in claim 18 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 and SiCl 4 .
Claim 24
Dependent Claim
25 words
A method as defined in claim 19 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 and SiCl 4 .
Claim 25
Dependent Claim
25 words
A method as defined in claim 20 wherein said reactive metal halide is selected from the group consisting of HSiCl 3 and SiCl 4 .
Claim 26
Dependent Claim
23 words
A method as defined in claim 1 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in solution.
Claim 27
Dependent Claim
23 words
A method as defined in claim 2 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in solution.
Claim 28
Dependent Claim
23 words
A method as defined in claim 3 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in solution.
Claim 29
Dependent Claim
23 words
A method as defined in claim 4 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in solution.
Claim 30
Dependent Claim
24 words
A method as defined in claim 1 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 31
Dependent Claim
24 words
A method as defined in claim 2 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 32
Dependent Claim
24 words
A method as defined in claim 3 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 33
Dependent Claim
24 words
A method as defined in claim 4 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 34
Dependent Claim
24 words
A method as defined in claim 21 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 35
Dependent Claim
24 words
A method as defined in claim 22 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 36
Dependent Claim
24 words
A method as defined in claim 23 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 37
Dependent Claim
24 words
A method as defined in claim 24 wherein said R 3 SiNH-containing silazane polymer is treated with said reactive metal halide in vapor phase.
Claim 38
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 1.
Claim 39
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 2.
Claim 40
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 3.
Claim 41
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 4.
Claim 42
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 21.
Claim 43
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 22.
Claim 44
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 23.
Claim 45
Dependent Claim
14 words
A silicon nitride containing ceramic material as prepared by the method of claim 24.
Claim 46
Independent Claim
136 words
A method of preparing an infusible silazane polymer, which method comprises treating a R 3 SiNH-containing silazane polymer with a reactive metal halide of general formula MX n or R b SiX.sub.(4-b) at a temperature below the softening point of the R 3 SiNH-containing silazane polymer for a time sufficient to render the silazane polymer infusible when R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms, M is a metal atom of valence n, X is a halide atom selected from the group consisting of chlorine and bromine, and b has a value of 0, 1, or 2, where said reactive metal halide has fewer carbon atoms than the R 3 SiNH-endblocking group, and where said reactive metal halide has at least two halide atoms.
Claim 47
Independent Claim
136 words
A method of preparing an infusible silazane polymer, which method comprises treating a R 3 SiNH-containing silazane polymer with a reactive metal halide of general formula MX n or R b SiX.sub.(4-b) at a temperature below the softening point of the R 3 SiNH-containing silazane polymer for a time sufficient to render the silazane polymer infusible when R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms, M is a metal atom of valence n, X is a halide atom selected from the group consisting of chlorine and bromine, and b has a value of 0, 1, or 2, where said reactive metal halide has fewer carbon atoms than the R 3 SiNH-endblocking group, and where said reactive metal halide has at least two halide atoms.
Claim 48
Dependent Claim
113 words
A method as defined in claim 45 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, an organochlorosilane or a mixture of organochlorosilanes of general formula R'.sub.c SiCl.sub.(4-c) with a disilazane of general formula (R.sub.3 Si).sub.2 NH at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein R' is selected from the group consisting of vinyl, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; and c has a value of 1 or 2.
Claim 49
Dependent Claim
132 words
A method as defined in claim 45 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, a chlorine-containing disilane or a mixture of chlorine-containing disilazane, of general formula (Cl.sub.d R'.sub.e Si).sub.2 with a disilazane of general formula (R.sub.3 Si).sub.2 NH at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein R' is selected from the group consisting of vinyl, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms; d has a value of 0.5 to 3; e has a value of 0 to 2.5; and the sum of (d+e) is equal to 3.
Claim 50
Dependent Claim
78 words
A method as defined in claim 45 wherein said R 3 SiNH-containing silazane polymer is prepared by contacting and reacting in an inert, essentially anhydrous atmosphere, trichlorosilane with a disilazane at a temperature in the range of 25° C. to 300° C. while removing byproduced volatile products, wherein said disilazane has the general formula (R.sub.3 Si).sub.2 NH where R is selected from the group consisting of vinyl, hydrogen, phenyl, and alkyl radicals containing 1 to 3 carbon atoms.
Claim 51
Dependent Claim
19 words
A method as defined in claim 45 wherein said reactive metal halide is HSiCl 3 or SiCl 4 .
Claim 52
Dependent Claim
19 words
A method as defined in claim 46 wherein said reactive metal halide is HSiCl 3 or SiCl 4 .
Claim 53
Dependent Claim
19 words
A method as defined in claim 47 wherein said reactive metal halide is HSiCl 3 or SiCl 4 .
Claim 54
Dependent Claim
19 words
A method as defined in claim 48 wherein said reactive metal halide is HSiCl 3 or SiCl 4 .
References Cited (Backward Citations)
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| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1988-08-12 | 1989-02-11 | 1989-08-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-08-12 | 1993-02-11 | 1993-08-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-08-12 | 1997-02-11 | 1997-08-13 | $7700.00 | Window Closed / Lapsed |