US4298558A
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High yield silicon carbide pre-ceramic polymers
Assignee: Dow Silicones Corp
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Filing: 1980-07-23
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Granted: 1981-11-03
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Expires: 2000-07-23
Abstract
Abstract Pre-polymers which are alkoxylated or phenoxylated methylpolysilanes are useful for the preparation of fine grained silicon carbide ceramic materials and silicon carbide-containing ceramics. The pre-polymers exhibit ease of handling and their use to obtain silicon carbide ceramic materials results in high yields.
Inventors
- 👤 Ronald H. Baney
- 👤 John H. Gaul, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 15:00
CPC Classifications
C; C04; C04B; C04B41/00; C04B41/009; C01; C01B; C01B32/00; C01B32/90; C01B32/914; C01B32/956; C01B32/963; C01B32/977; C04B35/00; C04B35/515; C04B35/56; C04B35/565; C04B35/571; C04B35/622; C04B35/626; C04B35/63; C04B35/6303; C04B35/6316; C04B41/45; C04B41/50; C04B41/5053; C04B41/5057; C04B41/5059; C04B41/80; C04B41/81; C04B41/85; C04B41/87; C08; C08G; C08G77/00; C08G77/60; C01P; C01P2002/00; C01P2002/80; C01P2002/86; C01P2006/00; C01P2006/80; Y; Y10; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31551; Y10T428/31609; Y10T428/31612; Y10T428/31678; Y10T428/31714
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
328 words
A method of preparing a polysilane having the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} (I) in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane which method consists of (A) reacting under anhydrous conditions a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} (II) in which there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein the remaining bonds on the silicon atoms are attached to either another silicon atom, a chlorine atom or a bromine atom such that the polysilane contains from 10-43 weight percent, based on the weight of the polysilane, of hydrolyzable chlorine or 21-62 weight percent based on the weight of the polysilane of hydrolyzable bromine, with a reagent selected from the group consisting of (i) carbinols having the general formula ROH (ii) alcoholates having the general formula ROM and (iii) alkyl orthoformates having the general formula (R'O) 3 CH wherein R is the same as above, R' is an alkyl group of 1-4 carbon atoms, and M is sodium, potassium or lithium, at a temperature of from 0° to 110° C. for a period of from 1.5 to 65 hours, in a suitable solvent, and (B) thereafter recovering the polysilane (I).
Claim 2
Independent Claim
328 words
A method of preparing a polysilane having the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} (I) in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane which method consists of (A) reacting under anhydrous conditions a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} (II) in which there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein the remaining bonds on the silicon atoms are attached to either another silicon atom, a chlorine atom or a bromine atom such that the polysilane contains from 10-43 weight percent, based on the weight of the polysilane, of hydrolyzable chlorine or 21-62 weight percent based on the weight of the polysilane of hydrolyzable bromine, with a reagent selected from the group consisting of (i) carbinols having the general formula ROH (ii) alcoholates having the general formula ROM and (iii) alkyl orthoformates having the general formula (R'O) 3 CH wherein R is the same as above, R' is an alkyl group of 1-4 carbon atoms, and M is sodium, potassium or lithium, at a temperature of from 0° to 110° C. for a period of from 1.5 to 65 hours, in a suitable solvent, and (B) thereafter recovering the polysilane (I).
Claim 3
Dependent Claim
33 words
A method of preparing a polysilane as claimed in claim 1 wherein there is present at least a stoichiometric quantity of a carbinol based on the amount of halogen in the polysilane (II).
Claim 4
Dependent Claim
33 words
A method of preparing a polysilane as claimed in claim 1 wherein there is present at least a stoichiometric quantity of an alcoholate based on the amount of halogen in the polysilane (II).
Claim 5
Dependent Claim
34 words
A method of preparing a polysilane as claimed in claim 1 wherein there is present at least a stoichiometric quantity of an alkyl orthoformate based on the amount of halogen in the polysilane (II).
Claim 6
Dependent Claim
144 words
A composition of matter consisting essentially of a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane.
Claim 7
Dependent Claim
144 words
A composition of matter consisting essentially of a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane.
Claim 8
Independent Claim
149 words
A method of preparing silicon carbide ceramic materials which consists of heating a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane.
Claim 9
Independent Claim
149 words
A method of preparing silicon carbide ceramic materials which consists of heating a polysilane having the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane.
Claim 10
Dependent Claim
13 words
Silicon carbide ceramic material prepared by the method as claimed in claim 6.
Claim 11
Independent Claim
197 words
A method of preparing a silicon carbide-containing ceramic article which consists of (A) forming an article of the desired shape from a polysilane having the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane; and (B) heating the article formed in (A) in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the polysilane is converted to a silicon carbide-containing ceramic article.
Claim 12
Independent Claim
197 words
A method of preparing a silicon carbide-containing ceramic article which consists of (A) forming an article of the desired shape from a polysilane having the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane; and (B) heating the article formed in (A) in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the polysilane is converted to a silicon carbide-containing ceramic article.
Claim 13
Dependent Claim
12 words
The silicon carbide-containing ceramic article prepared by the method of claim 8.
Claim 14
Independent Claim
214 words
A method of preparing a filled silicon carbide-containing ceramic article which consists of (A) mixing a polysilane with at least one conventional ceramic filler which polysilane has the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane, (B) forming an article of the desired shape from the mixture of polysilane and fillers and, (C) heating the article formed in (B) in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the polysilane is converted to a silicon carbide-containing ceramic.
Claim 15
Independent Claim
214 words
A method of preparing a filled silicon carbide-containing ceramic article which consists of (A) mixing a polysilane with at least one conventional ceramic filler which polysilane has the average formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical, and either 0 to 25 weight percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane, (B) forming an article of the desired shape from the mixture of polysilane and fillers and, (C) heating the article formed in (B) in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the polysilane is converted to a silicon carbide-containing ceramic.
Claim 16
Dependent Claim
9 words
An article prepared by the method of claim 10.
Claim 17
Independent Claim
216 words
A method of preparing an article coated with ceramic which consists of (A) mixing a polysilane with at least one conventional ceramic filler which polysilane has the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 35 percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane; (B) coating a substrate with the mixture of polysilane and fillers and, (C) heating the coated substrate in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the coating is converted to a silicon carbide ceramic, whereby a silicon carbide-containing ceramic coated article is obtained.
Claim 18
Independent Claim
216 words
A method of preparing an article coated with ceramic which consists of (A) mixing a polysilane with at least one conventional ceramic filler which polysilane has the average unit formula {(CH.sub.3).sub.2 Si}{CH.sub.3 Si} in which polysilane there is from 0 to 60 mole percent (CH 3 ) 2 Si═ units and 40 to 100 mole percent CH 3 Si.tbd. units, wherein there is also bonded to the silicon atoms other silicon atoms and radicals having the formula RO-- wherein R is an alkyl radical of 1 to 4 carbon atoms or phenyl wherein essentially all the remaining bonds on silicon are attached to chlorine or bromine atoms such that the polysilane contains from 24 to 61 weight percent of RO-- when R is an alkyl radical, 26 to 66 weight percent of RO-- when R is a phenyl radical and either 0 to 35 percent chlorine or 0-35 weight percent bromine, all based on the weight of the polysilane; (B) coating a substrate with the mixture of polysilane and fillers and, (C) heating the coated substrate in an inert atmosphere or in a vacuum to an elevated temperature in the range of 1200° C. to 1600° C. until the coating is converted to a silicon carbide ceramic, whereby a silicon carbide-containing ceramic coated article is obtained.
Claim 19
Dependent Claim
9 words
An article prepared by the method of claim 12.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1984-11-02 | 1985-05-04 | 1985-11-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-11-02 | 1989-05-04 | 1989-11-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-11-02 | 1993-05-04 | 1993-11-03 | $7700.00 | Window Closed / Lapsed |