US4460640A — Fiber reinforced glass matrix composites

Claim 1

Independent Claim 149 words

A method of preparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with a thermosetting organosilicone resin dissolved in an organic solvent; (B) forming a prepreg by drying the product from (A); (C) heating the dried product of (B) at an elevated temperature for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone 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

Independent Claim 149 words

A method of preparing fiber reinforced glass composites which method comprises (A) impregnating high modulus fibers with a thermosetting organosilicone resin dissolved in an organic solvent; (B) forming a prepreg by drying the product from (A); (C) heating the dried product of (B) at an elevated temperature for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone 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 3

Dependent Claim 156 words

A method as defined in claim 1 wherein said organosilicone resin is a composition containing (a) an organopolysiloxane containing from 75 to 85 mol percent C 6 H 5 SiO 3/2 units and 15 to 25 mol percent of CH 2 ═CH(CH 3 ) 2 SiO 1/2 units, said organopolysiloxane having an average of at least 8 silicon atoms per molecule; (b) a silicon hydride containing polysiloxane cross-linker for (a), said (b) being present in an amount sufficient to provide about 0.9 to 1.1 mol of silicon hydride per mol of CH 2 ═CHSi.tbd. present in (a); wherein, in said organosilicone resin, there is also present a platinum catalyst in an amount sufficient to catalyze the reaction of the silicon hydride with the CH 2 ═CHSi.tbd.; and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers are essentially undirectional and continuous.

Claim 4

Dependent Claim 155 words

A method as defined in claim 1 wherein said organosilicone resin is a composition containing (a) an organopolysiloxane containing from 75 to 85 mol percent C 6 H 5 SiO 3/2 units and 15 to 25 mol percent of CH 2 ═CH(CH 3 ) 2 SiO 1/2 units, said organopolysiloxane having an average of at least 8 silicon atoms per molecule; (b) a silicon hydride containing polysiloxane cross-linker for (a), said (b) being present in an amount sufficient to provide about 0.9 to 1.1 mol of silicon hydride per mol of CH 2 ═CHSi.tbd. present in (a); wherein, in said organosilicone resin, there is also present a platinum catalyst in an amount sufficient to catalyze the reaction of the silicon hydride with the CH 2 ═CHSi.tbd.; and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers form a woven fabric.

Claim 5

Dependent Claim 182 words

A method as defined in claim 1 wherein said organosilicone resin is a composition containing (a) an organopolysiloxane containing from 67 to 85 mol percent C 6 H 5 SiO 3/2 units and 33 to 15 mol percent of CH 2 ═CH(CH 3 ) 2 SiO 1/2 units, said organopolysiloxane having an average of at least 8 silicon atoms per molecule; (b) a silicon hydride containing polysiloxane cross-linker for (a), said (b) being present in an amount sufficient to provide about 0.9 to 1.1 mol of silicon hydride per mol of CH 2 ═CHSi.tbd. present in (a); and (c) a reactive diluent having the formula [CH.sub.2 ═CH(CH.sub.3).sub.2 SiO].sub.2 Si(C.sub.6 H.sub.5).sub.2 in a ratio of 1:4 to 1:1 of component (c) to component (a); wherein, in said organosilicone resin, there is also present a platinum catalyst in an amount sufficient to catalyze the reaction of the silicon hydride with the CH 2 ═CHSi.tbd.; and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers are essentially undirectional and continuous.

Claim 6

Dependent Claim 181 words

A method as defined in claim 1 wherein said organosilicone resin is a composition containing (a) an organopolysiloxane containing from 67 to 85 mol percent C 6 H 5 SiO 3/2 units and 33 to 15 mol percent of CH 2 ═CH(CH 3 ) 2 SiO 1/2 units, said organopolysiloxane having an average of at least 8 silicon atoms per molecule; (b) a silicon hydride containing polysiloxane cross-linker for (a), said (b) being present in an amount sufficient to provide about 0.9 to 1.1 mol of silicon hydride per mol of CH 2 ═CHSi.tbd. present in (a); and (c) a reactive diluent having the formula [CH.sub.2 ═CH(CH.sub.3).sub.2 SiO].sub.2 Si(C.sub.6 H.sub.5).sub.2 in a ratio of 1:4 to 1:1 of component (c) to component (a); wherein, in said organosilicone resin, there is also present a platinum catalyst in an amount sufficient to catalyze the reaction of the silicon hydride with the CH 2 ═CHSi.tbd.; and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers form a woven fabric.

Claim 7

Dependent Claim 67 words

A method as defined in claim 2 wherein, in said organosilicone resin, component (b) is present in an amount sufficient to provide about 1.0 mole of silicon hydride per mole of CH 2 ═CHSi.tbd. in said organosilicon resin; and wherein said platinum catalyst is present in an amount sufficient to provide at least 0.1 parts by weight platinum per million parts by weight of said organosilicone resin.

Claim 8

Dependent Claim 67 words

A method as defined in claim 3 wherein, in said organosilicone resin, component (b) is present in an amount sufficient to provide about 1.0 mole of silicon hydride per mole of CH 2 ═CHSi.tbd. in said organosilicon resin; and wherein said platinum catalyst is present in an amount sufficient to provide at least 0.1 parts by weight platinum per million parts by weight of said organosilicone resin.

Claim 9

Dependent Claim 67 words

A method as defined in claim 4 wherein, in said organosilicone resin, component (b) is present in an amount sufficient to provide about 1.0 mole of silicon hydride per mole of CH 2 ═CHSi.tbd. in said organosilicon resin; and wherein said platinum catalyst is present in an amount sufficient to provide at least 0.1 parts by weight platinum per million parts by weight of said organosilicone resin.

Claim 10

Dependent Claim 67 words

A method as defined in claim 5 wherein, in said organosilicone resin, component (b) is present in an amount sufficient to provide about 1.0 mole of silicon hydride per mole of CH 2 ═CHSi.tbd. in said organosilicon resin; and wherein said platinum catalyst is present in an amount sufficient to provide at least 0.1 parts by weight platinum per million parts by weight of said organosilicone resin.

Claim 11

Dependent Claim 62 words

A method as defined in claim 6 wherein said platinum catalyst is [R 3 PPtCl 2 ] 2 where R is selected from the group consisting of methyl, ethyl, propyl and butyl radicals and wherein said platinum catalyst is present in an amount sufficient to provide from about 1 to 20 parts by weight platinum per million parts of said organosilicone resin.

Claim 12

Dependent Claim 62 words

A method as defined in claim 7 wherein said platinum catalyst is [R 3 PPtCl 2 ] 2 where R is selected from the group consisting of methyl, ethyl, propyl and butyl radicals and wherein said platinum catalyst is present in an amount sufficient to provide from about 1 to 20 parts by weight platinum per million parts of said organosilicone resin.

Claim 13

Dependent Claim 62 words

A method as defined in claim 8 wherein said platinum catalyst is [R 3 PPtCl 2 ] 2 where R is selected from the group consisting of methyl, ethyl, propyl and butyl radicals and wherein said platinum catalyst is present in an amount sufficient to provide from about 1 to 20 parts by weight platinum per million parts of said organosilicone resin.

Claim 14

Dependent Claim 62 words

A method as defined in claim 9 wherein said platinum catalyst is [R 3 PPtCl 2 ] 2 where R is selected from the group consisting of methyl, ethyl, propyl and butyl radicals and wherein said platinum catalyst is present in an amount sufficient to provide from about 1 to 20 parts by weight platinum per million parts of said organosilicone resin.

Claim 15

Dependent Claim 87 words

A method as defined in claim 1 wherein said organosilicone resin contains at least 0.25 percent by weight silicon-bonded hydroxyl groups and contains, on the average, 0.9 to 1.8 monovalent hydrocarbon radicals per silicon and wherein said organosilicone resin contains sufficient phenyl groups bonded directly to silicon to insure flowability of said organosilicone resin in step (D); and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers are essentially undirectional and continuous.

Claim 16

Dependent Claim 86 words

A method as defined in claim 1 wherein said organosilicone resin contains at least 0.25 percent by weight silicon-bonded hydroxyl groups and contains, on the average, 0.9 to 1.8 monovalent hydrocarbon radicals per silicon and wherein said organosilicone resin contains sufficient phenyl groups bonded directly to silicon to insure flowability of said organosilicone resin in step (D); and wherein said high modulus fibers are selected from the group consisting of carbon fibers and silicon carbide fibers and wherein said high modulus fibers form a woven fabric.

Claim 17

Dependent Claim 59 words

A method as defined in claim 14 wherein said organosilicone resin is a copolymer which contains at least one of the units of structure SiO 2 , ZSiO 3/2 , Z 2 SiO, and Z 3 SiO 1/2 where Z is a monovalent hydrocarbon radical and where at least 5 percent by weight of the Z groups are phenyl.

Claim 18

Dependent Claim 59 words

A method as defined in claim 15 wherein said organosilicone resin is a copolymer which contains at least one of the units of structure SiO 2 , ZSiO 3/2 , Z 2 SiO, and Z 3 SiO 1/2 where Z is a monovalent hydrocarbon radical and where at least 5 percent by weight of the Z groups are phenyl.

Claim 19

Dependent Claim 39 words

A method as defined in claim 14 wherein, in said organosilicone resin, there is present a silanol condensation catalyst at a level of about 0.005 to 5 percent by weight based on the total weight of said organosilicone resin.

Claim 20

Dependent Claim 39 words

A method as defined in claim 15 wherein, in said organosilicone resin, there is present a silanol condensation catalyst at a level of about 0.005 to 5 percent by weight based on the total weight of said organosilicone resin.

Claim 21

Dependent Claim 63 words

A method as defined in claim 18 wherein said organosilicone resin is a phenylmethylsiloxane wherein the C 6 H 5 :Si ratio is in the range of 0.5:1 to 0.7:1, wherein the CH 3 :Si ratio is in the range of 0.5:1 to 1.0:1, and wherein the (C 6 H 5 +CH 3 ):Si ratio is in the range of 1.1:1 to 1.6:1.

Claim 22

Dependent Claim 63 words

A method as defined in claim 19 wherein said organosilicone resin is a phenylmethylsiloxane wherein the C 6 H 5 :Si ratio is in the range of 0.5:1 to 0.7:1, wherein the CH 3 :Si ratio is in the range of 0.5:1 to 1.0:1, and wherein the (C 6 H 5 +CH 3 ):Si ratio is in the range of 1.1:1 to 1.6:1.

Claim 23

Dependent Claim 62 words

A method as defined in claim 20 wherein said organosilicone resin is a phenylmethylsiloxane resin which contains about 45 mol percent CH 3 SiO 3/2 units, about 40 mol percent C 6 H 5 SiO 3/2 units, about 5 mol percent C 6 H 5 (CH 3 )SiO units, and about 10 mol percent (C 6 H 5 ) 2 SiO units.

Claim 24

Dependent Claim 62 words

A method as defined in claim 21 wherein said organosilicone resin is a phenylmethylsiloxane resin which contains about 45 mol percent CH 3 SiO 3/2 units, about 40 mol percent C 6 H 5 SiO 3/2 units, about 5 mol percent C 6 H 5 (CH 3 )SiO units, and about 10 mol percent (C 6 H 5 ) 2 SiO units.

Claim 25

Dependent Claim 62 words

A method as defined in claim 2 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 26

Dependent Claim 62 words

A method as defined in claim 3 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 27

Dependent Claim 62 words

A method as defined in claim 4 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 28

Dependent Claim 62 words

A method as defined in claim 5 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 29

Dependent Claim 62 words

A method as defined in claim 10 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 30

Dependent Claim 62 words

A method as defined in claim 11 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 31

Dependent Claim 62 words

A method as defined in claim 12 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 32

Dependent Claim 62 words

A method as defined in claim 13 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 33

Dependent Claim 62 words

A method as defined in claim 14 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 34

Dependent Claim 62 words

A method as defined in claim 15 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 35

Dependent Claim 62 words

A method as defined in claim 20 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 36

Dependent Claim 62 words

A method as defined in claim 21 wherein the prepreg of step (B) is heated in step (C) at a temperature of 50° to 150° C. for a time sufficient to effect partial curing but to avoid excessive curing of the organosilicone resin; and wherein the prepreg from (C) is pressed in step (D) at a temperature of 100° to 300° C.

Claim 37

Dependent Claim 28 words

A method as defined in claim 24 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 38

Dependent Claim 28 words

A method as defined in claim 25 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 39

Dependent Claim 28 words

A method as defined in claim 26 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 40

Dependent Claim 28 words

A method as defined in claim 27 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 41

Dependent Claim 28 words

A method as defined in claim 32 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 42

Dependent Claim 28 words

A method as defined in claim 33 wherein the pressed and cured prepreg from (E) is slowly fired to a temperature of about 1200° C. in step (F).

Claim 43

Dependent Claim 30 words

A method as defined in claim 2 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 44

Dependent Claim 30 words

A method as defined in claim 3 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 45

Dependent Claim 30 words

A method as defined in claim 4 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 46

Dependent Claim 30 words

A method as defined in claim 5 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 47

Dependent Claim 30 words

A method as defined in claim 14 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 48

Dependent Claim 30 words

A method as defined in claim 15 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 49

Dependent Claim 30 words

A method as defined in claim 28 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 50

Dependent Claim 30 words

A method as defined in claim 29 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 51

Dependent Claim 30 words

A method as defined in claim 30 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 52

Dependent Claim 30 words

A method as defined in claim 31 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 53

Dependent Claim 30 words

A method as defined in claim 34 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 54

Dependent Claim 30 words

A method as defined in claim 35 wherein the fiber reinforced glass composite of step (G) is subjected to steps (A), (B), (E), (F), and (G) one or more times.

Claim 55

Dependent Claim 114 words

A method as defined in claim 2, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 56

Dependent Claim 114 words

A method as defined in claim 3, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 57

Dependent Claim 114 words

A method as defined in claim 4, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 58

Dependent Claim 114 words

A method as defined in claim 5, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 59

Dependent Claim 114 words

A method as defined in claim 14, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 60

Dependent Claim 114 words

A method as defined in claim 15, which method further comprises (H) impregnating the fiber reinforced glass composite of step (G) with a colloidal metal oxide solution where said metal oxide is selected from the group consisting of SiO 2 , Al 2 O 3 , ZrO 2 , TiO 2 , and SnO 2 ; (I) drying the fiber reinforced glass composite of step (H); (J) slowing firing the fiber reinforced glass composite of step (I) to a temperature of at least 1100° C. in an inert atmosphere or vacuum; and (K) cooling the fiber reinforced glass composite of step (J); wherein steps (H) through (K) can be repeated one or more times.

Claim 61

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 2.

Claim 62

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 3.

Claim 63

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 4.

Claim 64

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 5.

Claim 65

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 10.

Claim 66

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 11.

Claim 67

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 12.

Claim 68

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 13.

Claim 69

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 14.

Claim 70

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 15.

Claim 71

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 20.

Claim 72

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 21.

Claim 73

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 42.

Claim 74

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 43.

Claim 75

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 44.

Claim 76

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 45.

Claim 77

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 46.

Claim 78

Dependent Claim 13 words

A fiber reinforced glass composite as prepared by the method of claim 47.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1987-07-17	1988-01-16	1988-07-17	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1991-07-17	1992-01-16	1992-07-17	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1995-07-17	1996-01-16	1996-07-17	$7700.00	Window Closed / Lapsed

Fiber reinforced glass matrix composites

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