Carbon-containing monolithic glasses and ceramics prepared by a sol-gel process
First Claim
Patent Images
1. A method of preparing a carbon-containing, monolithic glassy ceramic which comprises drying and pyrolyzing at a temperature of 500°
- C. to 1500°
C. in an inert atmosphere, or a vacuum, until a carbon-containing, monolithic glassy ceramic is obtained, a product comprising a stable gel selected from a group consisting essentially of(A) a gel obtained from a sol of an organosilsesquioxane having the unit formula
space="preserve" listing-type="equation">RSiO.sub.3/2wherein R is selected from a group consisting essentially of(a) CH2 ═
CH--;
(b) CH2 ═
CHCH2 --;
(c) C6 H5 --;
(d) alkyl radicals of 1 to 4 carbon atoms;
(e) substituted monovalent organic radicals selected from the group consisting of CH2 ═
CHC(CH3)COO(CH2)3 --, ##STR2## HS(CH2)3 --, Cl(CH2)3 --, and NH2 (CH2)2 NH(CH2)3 --; and
(f) mixtures of (a), (b), (c), (d), and (e);
(B) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A), and a colloidal metal oxide or a mixture of colloidal metal oxides selected from a group consisting essentially of(i) SiO2(ii) Al2 O3(iii) ZrO2(iv) TiO2(v) SnO2(vi) ZrSiO4(vii) B2 O3(viii) La2 O3 and(ix) Sb2 O5wherein said gel contains at least 10 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal oxide;
(C) a gel obtained from a mixture of a sol of an .[.organosilsesquioxanes.]. .Iadd.organosilsesquioxane .Iaddend.from (A), and a metal alkoxide, or a mixture of metal alkoxides having the general formula
space="preserve" listing-type="equation">M(OR'"'"').sub.xwherein M is any metal from a metal alkoxide which hydrolyzes and polymerizes in the presence of water, R'"'"' is an alkyl radical of 1 to 4 carbon atoms and x has a value equivalent to the metal ion valence wherein said gel contains at least about 50 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal M in said gel.
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Abstract
What is disclosed is a method of preparing carbon-containing monolithic glassy ceramics from organosilsesquioxanes, metal oxides and metal alkoxides through pyrolysis of their gels. Also disclosed are certain gel compositions used in the method and the glassy ceramics.
72 Citations
89 Claims
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1. A method of preparing a carbon-containing, monolithic glassy ceramic which comprises drying and pyrolyzing at a temperature of 500°
- C. to 1500°
C. in an inert atmosphere, or a vacuum, until a carbon-containing, monolithic glassy ceramic is obtained, a product comprising a stable gel selected from a group consisting essentially of(A) a gel obtained from a sol of an organosilsesquioxane having the unit formula
space="preserve" listing-type="equation">RSiO.sub.3/2wherein R is selected from a group consisting essentially of (a) CH2 ═
CH--;(b) CH2 ═
CHCH2 --;(c) C6 H5 --; (d) alkyl radicals of 1 to 4 carbon atoms; (e) substituted monovalent organic radicals selected from the group consisting of CH2 ═
CHC(CH3)COO(CH2)3 --, ##STR2## HS(CH2)3 --, Cl(CH2)3 --, and NH2 (CH2)2 NH(CH2)3 --; and(f) mixtures of (a), (b), (c), (d), and (e); (B) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A), and a colloidal metal oxide or a mixture of colloidal metal oxides selected from a group consisting essentially of (i) SiO2 (ii) Al2 O3 (iii) ZrO2 (iv) TiO2 (v) SnO2 (vi) ZrSiO4 (vii) B2 O3 (viii) La2 O3 and (ix) Sb2 O5 wherein said gel contains at least 10 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal oxide; (C) a gel obtained from a mixture of a sol of an .[.organosilsesquioxanes.]. .Iadd.organosilsesquioxane .Iaddend.from (A), and a metal alkoxide, or a mixture of metal alkoxides having the general formula
space="preserve" listing-type="equation">M(OR'"'"').sub.xwherein M is any metal from a metal alkoxide which hydrolyzes and polymerizes in the presence of water, R'"'"' is an alkyl radical of 1 to 4 carbon atoms and x has a value equivalent to the metal ion valence wherein said gel contains at least about 50 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal M in said gel. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 85)
- C. to 1500°
- 41. A method of forming a carbon-containing, monolithic glassy ceramic coating on a solid substrate which comprises
(I) coating a solid substrate with a sol selected from a group consisting essentially of (A) a sol of organosilsesquioxane having the unit formula - space="preserve" listing-type="equation">RSiO.sub.3/2
wherein R is selected from a group consisting essentially of (a) CH2 ═
CH--;(b) CH2 ═
CHCH2 --;(c) C6 H5 --; (d) alkyl radicals of 1 to 4 carbon atoms; (e) substituted monovalent organic radicals selected from the group consisting of CH2 ═
CHC(CH3)COO(CH2)3 --, ##STR3## HS(CH2)3 --, Cl(CH2)3 --, and NH2 (CH2)2 NH(CH2)3 --; and(f) mixtures of (a), (b), (c), (d), and (e); (B) a mixture of a sol of an organosilsesquioxane from (A), and a colloidal metal oxide or a mixture of colloidal metal oxides selected from a group consisting essentially of (i) SiO2 (ii) Al2 O3 (iii) ZrO2 (iv) TiO2 (v) SnO2 (vi) ZrSiO4 (vii) B2 O3 (viii) La2 O3 and (ix) Sb2 O5 wherein said gel contains at least 10 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal oxide; (C) a mixture of a sol of an organosilsesquioxane from (A), and a metal alkoxide, or a mixture of metal alkoxides having the general formula
space="preserve" listing-type="equation">M(OR'"'"').sub.xwherein M is any metal from a metal alkoxide which hydrolyzes and polymerizes in the presence of water, R'"'"' is an alkyl radical of 1 to 4 carbon atoms and x has a value equivalent to the metal ion valence wherein said gel contains at least about 50 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal M in said gel; (II) gelling the sol while the sol is on the solid substrate; (III) drying the gel to remove volatile materials; (IV) heat treating the gel to remove higher boiling volatiles; and (V) pyrolyzing the dried and heat treated gel at a temperature of 500°
C. to 1500°
C. in an inert atmosphere or a vacuum until a carbon-containing, monolithic glassy ceramic coated substrate is obtained.- View Dependent Claims (42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76)
- 77. A method of forming a carbon-containing, monolithic glassy ceramic coating on a solid substrate which comprises
(I) coating a solid substrate with a stable gel selected from a group consisting essentially of (A) a gel obtained from a sol of an organosilsesquioxane having the unit formula - space="preserve" listing-type="equation">RSiO.sub.3/2
wherein R is selected from a group consisting essentially of (a) CH2 ═
CH--;(b) CH2 ═
CHCH2 --;(c) C6 H5 --; (d) alkyl radicals of 1 to 4 carbon atoms; (e) substituted monovalent organic radicals selected from the group consisting of CH2 ═
CHC(CH3)COO(CH2)3 --, ##STR4## HS(CH2)3 --, Cl(CH2)3 --, and NH2 (CH2)2 NH(CH2)3 --; and(f) mixtures of (a), (b), (c), (d), and (e); (B) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A), and a colloidal metal oxide or a mixture of colloidal metal oxides selected from a group consisting essentially of (i) SiO2 (ii) Al2 O3 (iii) ZrO2 (vi) ZrSiO4 (vii) B2 O3 (viii) La2 O3 and (iv) TiO2 (v) SnO2 (ix) Sb2 O5 wherein said gel contains at least 10 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal oxide; (C) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A), and a metal alkoxide, or a mixture of metal alkoxides having the general formula
space="preserve" listing-type="equation">M(OR'"'"').sub.xwherein M is any metal from a metal alkoxide which hydrolyzes and polymerizes in the presence of water, R'"'"' is an alkyl radical of 1 to 4 carbon atoms and x has a value equivalent to the metal ion valence wherein said gel contains at least about 50 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal M in said gel; (II) drying the gel to remove volatile materials; (III) het treating the gel to remove higher boiling volatiles; and (IV) pyrolyzing the dried and heat treated gel at a temperature of 500°
C. to 1500°
C. in an insert atmosphere or a vacuum until a carbon-containing, monolithic glassy ceramic coated substrate is obtained.- View Dependent Claims (78, 79, 80, 81, 82, 83, 84)
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86. organosilsesquioxane and said metal M in said gel. 87. A method as claimed in claim 86 wherein M(OR'"'"'")y is Ti(OC3 H7)4 and the
- 87. colloidal metal oxide is SiO2. 88. A method as claimed in claim 87
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89. and C6 H5 SiO3/2. .Iadd.90. A composition of matter which is a monolithic glassy ceramic prepared by the method which comprises drying and pyrolyzing at a temperature of 500°
- C. to 1500°
C. in an inert atmosphere or a vacuum, until a carbon-containing, monolithic glassy ceramic is obtained, a product comprising a stable gel selected from a group consisting essentially of(A) a gel obtained from a sol of an organosilsesquioxane having the unit formula
space="preserve" listing-type="equation">RSiO.sub.3/2wherein R is selected from a group consisting essentially of (a) CH2 ═
CH--;(b) CH2 ═
CHCH2 --;(c) C6 H5 --; (d) alkyl radicals of 1 to 4 carbon atoms; (e) substituted monovalent organic radicals selected from the group consisting of CH2 ═
CHC(CH3)COO(CH2)3 --, ##STR6## HS(CH2)3 --; and
(f) mixtures of (a), (b), (c), (d), and (e);(B) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A) and a colloidal metal oxide or a mixture of colloidal metal oxides selected from a group consisting essentially of (i) SiO2, (ii) Al2 O3, (iii) ZrO2, (iv) SnO2, (v) ZrSiO4, (vi) B2 O3, (vii) La2 O3, and (viii) Sb2 O5 wherein said gel contains at least 10 weight percent of said organosilsesquioxane from (A) based on the metal weight of said organosilsesquioxane and said metal oxide; and (C) a gel obtained from a mixture of a sol of an organosilsesquioxane from (A) and a metal alkoxide or a mixture of metal alkoxides having the general formula
space="preserve" listing-type="equation">M(OR'"'"').sub.xwherein M is a metal selected from the group consisting of aluminum, zirconium, and tin, wherein said metal alkoxide hydrolyzes and polymerizes in the presence of water, R'"'"' is an alkyl radical of 1 to 4 carbon atoms and x has a value equivalent to the valence of M wherein said gel contains at least about 50 weight percent of said organosilsesquioxane from (A) based on the total weight of said organosilsesquioxane and said metal M in said gel. .Iaddend.
- C. to 1500°
Specification
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Current AssigneeDow, Inc.
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Original AssigneeDow, Inc.
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InventorsJanuary, James R.
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Primary Examiner(s)McCarthy, Helen M.
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Application NumberUS06/682,739Time in Patent Office477 DaysField of Search501/12, 501/32, 501/55, 501/87, 501/95, 501/128, 501/35, 501/38, 65/17, 65/18.1, 65/18.2, 65/134, 428/412, 428/428, 428/446, 428/447US Class Current501/12CPC Class CodesC03C 1/006 to produce glass through we...C03C 10/0009 containing silica as main c...
