Fiber reinforced glass matrix composites

Claim 1

A method of perparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with resin sol, which resin sol is selected from the group consisting essentially of (i) a sol of an organosilsesquioxane having the average formula [C.sub.6 H.sub.5 SiO.sub.3/2 ][RSiO.sub.3/2 ] wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 5 to 100 percent by weight and RSiO 3/2 is present in the amount of 0 to 95 percent by weight based on the total weight of organosilsesquioxane present, and where R is an alkyl radical containing from 1 to 4 carbon atoms; (ii) a mixture of a sol of the organosilsesquioxane from (i) and a colloidal metal oxide, or a mixture of colloidal metal oxides, selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , SnO 2 , ZrSiO 4 , B 2 O 3 , La 2 O 3 , Sb 2 O 5 ; wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 5 to 90 percent by weight and RSiO 3/2 is present in the amount of 10 to 95 percent by weight based on the total weight of organosilsesquioxane present; and (iii) a mixture of a sol of the organosilsesquioxane from (i) and a metal alkoxide, or a mixture of metal alkoxides, having the general formula M(OR').sub.x wherein M is a metal atom, R' is an alkyl radical containing from 1 to 4 carbon atoms, and x is 3 or 4, which metal alkoxide is capable of hydrolyzing and condensing in water; wherein C 6 H 5 SiO 3/2 is present in the amount of 5 to 90 percent by weight and RSiO 3/2 is present in the amount of 10 to 95 percent by weight based on the total weight of organosilsesquioxane present; (B) forming a prepreg by drying the product from (A); (C) heating the prepreg of (B) at an elevated temperature for a time sufficient to effect partial curing but to avoid excessive curing of the resin; (D) pressing the prepreg from (C) at a temperature not greater than about 300° C.; (E) curing the pressed prepreg from (D) at a temperature not greater than about 300° C. for a time sufficient to insure complete or nearly complete cross-linking in the prepreg; (F) slowly firing the pressed and cured prepreg from (E) to a temperature of at least 1000° C. in an inert atmosphere or vacuum until a fiber reinforced glass composite is obtained; and (G) cooling the fiber reinforced glass composite.

Claim 2

A method of perparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with resin sol, which resin sol is selected from the group consisting essentially of (i) a sol of an organosilsesquioxane having the average formula [C.sub.6 H.sub.5 SiO.sub.3/2 ][RSiO.sub.3/2 ] wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 5 to 100 percent by weight and RSiO 3/2 is present in the amount of 0 to 95 percent by weight based on the total weight of organosilsesquioxane present, and where R is an alkyl radical containing from 1 to 4 carbon atoms; (ii) a mixture of a sol of the organosilsesquioxane from (i) and a colloidal metal oxide, or a mixture of colloidal metal oxides, selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , SnO 2 , ZrSiO 4 , B 2 O 3 , La 2 O 3 , Sb 2 O 5 ; wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 5 to 90 percent by weight and RSiO 3/2 is present in the amount of 10 to 95 percent by weight based on the total weight of organosilsesquioxane present; and (iii) a mixture of a sol of the organosilsesquioxane from (i) and a metal alkoxide, or a mixture of metal alkoxides, having the general formula M(OR').sub.x wherein M is a metal atom, R' is an alkyl radical containing from 1 to 4 carbon atoms, and x is 3 or 4, which metal alkoxide is capable of hydrolyzing and condensing in water; wherein C 6 H 5 SiO 3/2 is present in the amount of 5 to 90 percent by weight and RSiO 3/2 is present in the amount of 10 to 95 percent by weight based on the total weight of organosilsesquioxane present; (B) forming a prepreg by drying the product from (A); (C) heating the prepreg of (B) at an elevated temperature for a time sufficient to effect partial curing but to avoid excessive curing of the resin; (D) pressing the prepreg from (C) at a temperature not greater than about 300° C.; (E) curing the pressed prepreg from (D) at a temperature not greater than about 300° C. for a time sufficient to insure complete or nearly complete cross-linking in the prepreg; (F) slowly firing the pressed and cured prepreg from (E) to a temperature of at least 1000° C. in an inert atmosphere or vacuum until a fiber reinforced glass composite is obtained; and (G) cooling the fiber reinforced glass composite.

Claim 38

A method of preparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with a resin sol, which high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and which resin sol is selected from the group consisting essentially of (i) a sol of an organosilsesquioxane having the average formula [C.sub.6 H.sub.5 SiO.sub.3/2 ][CH.sub.3 SiO.sub.3/2 ] wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 30 to 60 percent by weight and CH 3 SiO 3/2 is present in the amount of 30 to 60 percent by weight based on the total weight of organosilsesquioxane present; (ii) a mixture of a sol of the organosilsesquioxane from (i) and a colloidal metal oxide, or a mixture of colloidal metal oxides, selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and ZrSiO 4 ; (iii) a mixture of a sol of the organosilsesquioxane from (i) and a metal alkoxide, or mixture of metal alkoxides, selected from the group consisting of Si(OR') 4 , Ti(OR') 4 , Al(OR') 3 , Zr(OR') 4 , and Sn(OR') 4 ; (B) forming a prepreg by drying the product from (A); (C) heating the prepreg of (B) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the resin; (D) pressing the prepreg from (C) at a temperature of 100° to 300° C.; (E) curing the pressed prepreg from (D) at a temperature not greater than about 300° C. for a time sufficient to insure complete or nearly complete cross-linking in the prepreg; (F) slowing firing the pressed and cured prepreg from (E) to a temperature of at least 1000° C. in an inert atmospheric or vacuum until a fiber reinforced glass composite is obtained; and (G) cooling the fiber reinforced glass composite.

Claim 39

A method of preparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with a resin sol, which high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and which resin sol is selected from the group consisting essentially of (i) a sol of an organosilsesquioxane having the average formula [C.sub.6 H.sub.5 SiO.sub.3/2 ][CH.sub.3 SiO.sub.3/2 ] wherein C 6 H 5 SiO 3/2 is present in said organosilsesquioxane in the amount of 30 to 60 percent by weight and CH 3 SiO 3/2 is present in the amount of 30 to 60 percent by weight based on the total weight of organosilsesquioxane present; (ii) a mixture of a sol of the organosilsesquioxane from (i) and a colloidal metal oxide, or a mixture of colloidal metal oxides, selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and ZrSiO 4 ; (iii) a mixture of a sol of the organosilsesquioxane from (i) and a metal alkoxide, or mixture of metal alkoxides, selected from the group consisting of Si(OR') 4 , Ti(OR') 4 , Al(OR') 3 , Zr(OR') 4 , and Sn(OR') 4 ; (B) forming a prepreg by drying the product from (A); (C) heating the prepreg of (B) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the resin; (D) pressing the prepreg from (C) at a temperature of 100° to 300° C.; (E) curing the pressed prepreg from (D) at a temperature not greater than about 300° C. for a time sufficient to insure complete or nearly complete cross-linking in the prepreg; (F) slowing firing the pressed and cured prepreg from (E) to a temperature of at least 1000° C. in an inert atmospheric or vacuum until a fiber reinforced glass composite is obtained; and (G) cooling the fiber reinforced glass composite.