US3713865A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Composite product and method of making same
Assignee: Goodrich Corp
•
Filing: 1968-07-05
•
Granted: 1973-01-30
•
Expires: 1988-07-05
Abstract
Abstract A composite product and method of producing same having a substrate or matrix comprising carbonized fibers in which a metallic salt solution consisting of a soluble metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb, which form either carbides which are refractory or oxides which melt and are capable of forming a liquid surface (which will slow the diffusion of oxygen to the graphite surface causing either C + 1/202 -> CO or C + O2 -> CO2, depending upon the pressure and temperatures used in the end use). Said metallic salt when dissolved in a solvent of water or a solvent containing acetone, alcohol, ether or the like, is introduced into the interstices of the substrate and which after drying is left in fine particles. The composite is then heated to a temperature in the range of 1,500* to 2,500* F. with or without hydrogen atmosphere to effect partial reduction of the metallic salt. Almost simultaneously, carbon is infiltrated into the substrate to enclose the fibers and the metal particles. Subsequently the substrate is raised to a temperature of between approximately 1,400* C. and approximately 2,800* C. to anneal the pyrocarbon and convert the reduced metallic salt into carbide, thus producing a composition product having the substrate fibers surrounded by dead soft annealed graphite intimately mixed with hard carbide particles of very high melting point. The metal salt impregnated matrix, the reduced and/or not pyrocarbon coated metal salt in the matrix and the reduced, pyrocarbon coated, carbide converted metal salt or oxidized variations thereof are all referred to hereafter as alloys of the matrix.
Inventors
- 👤 D Leeds
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 11:43
CPC Classifications
H; H01; H01M; H01M4/00; H01M4/86; C; C22; C22C; C22C49/00; C22C49/14; D; D01; D01F; D01F11/00; D01F11/10; D01F11/12; D01F11/123; Y; Y02; Y02E; Y02E60/00; Y02E60/30; Y02E60/50; Y10; Y10S; Y10S264/00; Y10S264/19; Y10T; Y10T428/00; Y10T428/29; Y10T428/2913; Y10T428/2918; Y10T428/292; Y10T428/2933; Y10T428/2971
Claims Analysis
Total Claims: 51
Claim 1
Independent Claim
31 words
A composite product comprising: a. a carbonized fibrous substrate; and b. small particles of carbide in the interstices between said carbonized fibers and around the juncture of two or more fibers.
Claim 2
Dependent Claim
31 words
A composite product comprising: a. a carbonized fibrous substrate; and b. small particles of carbide in the interstices between said carbonized fibers and around the juncture of two or more fibers.
Claim 3
Dependent Claim
39 words
A composite product as defined in claim 1 in which the small particles of carbide are formed from a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, and B.
Claim 4
Dependent Claim
24 words
A composite product as defined in claim 1 in which dead soft annealed pyrolytic carbon surrounds said carbonized fibers and said particles of carbide.
Claim 5
Independent Claim
67 words
A method of forming a composite product comprising: a. introducing a metallic salt solution between carbonized fibers of a substrate; b. drying out said solution to leave alloy particles in the interstices between the carbonized fibers and around the juncture of two or more fibers; and c. heating the substrate in a reducing atmosphere to temperatures of between approximately 1,000* and 2,500*F. to reduce said alloy particles.
Claim 6
Independent Claim
67 words
A method of forming a composite product comprising: a. introducing a metallic salt solution between carbonized fibers of a substrate; b. drying out said solution to leave alloy particles in the interstices between the carbonized fibers and around the juncture of two or more fibers; and c. heating the substrate in a reducing atmosphere to temperatures of between approximately 1,000* and 2,500*F. to reduce said alloy particles.
Claim 7
Dependent Claim
46 words
A method as defined in claim 4 in which after the reducing step the substrate and its impregnate is infiltrated with pyrolytic carbon and then is heated to a temperature of between 1,400* to 2,800* in an inert atmosphere to convert the alloy particles into carbide.
Claim 8
Dependent Claim
17 words
A method as defined in claim 5 in which said metallic salt solution is a metallic sulfate.
Claim 9
Dependent Claim
59 words
A method of forming a composite product as defined in claim 4 in which the metal salt solution consists of a metal selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Si, and B, and a solvent from the group consisting of water, acetone, ethyl and methyl alcohol, ether and equivalent volatile solvent liquids.
Claim 10
Dependent Claim
89 words
A method of forming a composite product as defined in claim 4 in which the metal salt solution consists of a metal salt selected from a group of meTal salts and a solvent having the properties of forming refractory carbides or oxides which are refractory or melt and are capable of forming a liquid surface which will slow the diffusion of oxygen to the carbon surface, said metal salt selected from a group consisting of Hf. Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P And Pb.
Claim 11
Dependent Claim
17 words
A method as defined in claim 4 in which said metallic salt solution is a metallic sulfate.
Claim 12
Dependent Claim
14 words
A method as defined in claim 4 in which said reducing atmosphere is hydrogen.
Claim 13
Dependent Claim
14 words
A method as defined in claim 4 in which said reducing atmosphere is methane.
Claim 14
Dependent Claim
40 words
The method as defined in claim 4 in which the carbonized fibers of the substrate are converted into graphite before impregnation with the salt, and thereafter the salt is reduced to the metal and pyrocarbon is infiltrated into the composite.
Claim 15
Dependent Claim
32 words
A method of forming a composite product as defined in claim 4 in which the carbonized fibers and metal salt are surrounded with pyrocarbon prior to converting the metal salts into carbide.
Claim 16
Dependent Claim
57 words
A method of forming a composite product as defined in claim 4 in which the substrate is heated in an atmosphere containing methane or the equivalent to a temperature of between 1,500* and 2,500*F. in order to infiltrate pyrocarbon into the substrate around the carbonized fibers and metal salt particles before the alloy is converted into carbide.
Claim 17
Dependent Claim
78 words
A method of forming a composite product as defined in claim 4 in which the metal salt solution consists of a metal salt selected from a group of metal salts and a solvent having the properties of forming refractory carbides or oxides which are refractory or melt and are capable of forming a liquid surface which will slow the diffusion of oxygen to the carbon surface which yields either C +1/202 -> CO or C +O2 -> CO2.
Claim 18
Dependent Claim
46 words
A method of forming a composite product as defined in claim 4 in which the metal salt solution consisting of a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, and B, and a solvent including acetone.
Claim 19
Dependent Claim
49 words
A method of forming a composite produce as defined in claim 4 in which the metal salt solution consisting of a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W Mo, Ti, V, Cr, Si, and B, and a solvent including ethyl or methyl alcohol.
Claim 20
Dependent Claim
45 words
A method of forming a composite product as defined in claim 4 which the metal salt solution consisting of a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, and B, and a solvent including water.
Claim 21
Dependent Claim
59 words
A method of forming a composite product as defined in claim 4 in which the metal salt solution consisting of a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, and B, and a solvent elected from a group consisting of water, acetone, alcohols, ether and equivalent volatile solvent liquids.
Claim 22
Dependent Claim
40 words
A method of forming a composite product as defined in claim 4 in which the substrate consists of fibers of rayon and in which the fibers are either carbonized before impregnation by the metal salt solution or are carbonized afterwards.
Claim 23
Dependent Claim
62 words
A method of forming a composite product as defined in claim 4 in which the substrate consists of fibers selected from a group consisting of rayon, cotton, wool or other fibrous material, which is either inorganic and will remain without decomposition to a temperature where carbon infiltration is accomplished, or is organic and forms, without deforming or melting a suitable carbon char.
Claim 24
Dependent Claim
15 words
A composite product as defined in claim 2 in which the metal salt is Ta.
Claim 25
Dependent Claim
15 words
A composite product as defined in claim 2 in which the metal salt is Cb.
Claim 26
Dependent Claim
15 words
A composite product as defined in claim 2 in which the metal salt is Zr.
Claim 27
Dependent Claim
15 words
A composite product as defined in claim 2 in which the metal salt is Si.
Claim 28
Independent Claim
70 words
A method of forming a composite prodUct comprising: a. introducing a metallic salt solution between carbonized fibers of a substrate; b. drying out said solution to leave small alloy particles in the interstices of the carbonized fiber; c. heating the substrate and its impregnant to temperatures of 1,500* to 2,500*F. in hydrogen; and d. depositing pyrolytic carbon around said fibrous substrate and impregnant particles without converting them significantly to carbide.
Claim 29
Independent Claim
70 words
A method of forming a composite prodUct comprising: a. introducing a metallic salt solution between carbonized fibers of a substrate; b. drying out said solution to leave small alloy particles in the interstices of the carbonized fiber; c. heating the substrate and its impregnant to temperatures of 1,500* to 2,500*F. in hydrogen; and d. depositing pyrolytic carbon around said fibrous substrate and impregnant particles without converting them significantly to carbide.
Claim 30
Independent Claim
54 words
A method of impregnating a carbonized fibrous substrate comprising: a. forming a metal salt solution from a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb, and a solvent; and b. introducing the solution into the interstices the carbonized fibrous substrate.
Claim 31
Independent Claim
54 words
A method of impregnating a carbonized fibrous substrate comprising: a. forming a metal salt solution from a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb, and a solvent; and b. introducing the solution into the interstices the carbonized fibrous substrate.
Claim 32
Independent Claim
68 words
A method of impregnating a carbonized fibrous substrate comprising: a. forming a metal salt solution from a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb, and a solvent selected from a group consisting of water, acetone, alcohols, ether and equivalent liquids; and b. introducing the solution into the interstices between the carbonized fibrous substrate.
Claim 33
Independent Claim
68 words
A method of impregnating a carbonized fibrous substrate comprising: a. forming a metal salt solution from a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb, and a solvent selected from a group consisting of water, acetone, alcohols, ether and equivalent liquids; and b. introducing the solution into the interstices between the carbonized fibrous substrate.
Claim 34
Independent Claim
84 words
A method of increasing the impregnant solute solution system liquid wettability of carbon or graphite fibrous matrices comprising; a. colloidally impregnating the matrix with a compound which will chemically react with the carbon or graphite matrix at elevated temperatures to form a solvent soluble compound, such as LiF in carbon or graphite heated to 750*; and b. additions to the solvent-solute system of miscible liquids which wet the graphite or carbon surface, such as the addition of acetone to a water zirconium sulfate solution.
Claim 35
Independent Claim
84 words
A method of increasing the impregnant solute solution system liquid wettability of carbon or graphite fibrous matrices comprising; a. colloidally impregnating the matrix with a compound which will chemically react with the carbon or graphite matrix at elevated temperatures to form a solvent soluble compound, such as LiF in carbon or graphite heated to 750*; and b. additions to the solvent-solute system of miscible liquids which wet the graphite or carbon surface, such as the addition of acetone to a water zirconium sulfate solution.
Claim 36
Dependent Claim
51 words
A composite product comprising: a. a substrate having carbonized fibers; b. metal alloy particles in the interstices of said fibers, said metal alloy being formed of a metal salt selected from a group consisting of Ta, Cb, Zr, Si an Pb; and c. pyrolytic carbon surrounding said particles and said fibers.
Claim 37
Dependent Claim
51 words
A composite product comprising: a. a substrate having carbonized fibers; b. metal alloy particles in the interstices of said fibers, said metal alloy being formed of a metal salt selected from a group consisting of Ta, Cb, Zr, Si an Pb; and c. pyrolytic carbon surrounding said particles and said fibers.
Claim 38
Dependent Claim
68 words
A composite product as defined in claim 30 in which the fibers of said substrate are graphite. 32 A composite product comprising: a. a substrate having carbonized fibers; b. carbide particles in the interstices of said carbonized fibers, said carbide being formed of a metal salt selected from a group consisting of Ta, Cb, Zr, and Si; and c. pyrolytic carbon surrounding said particles and said carbonized fibers.
Claim 39
Dependent Claim
33 words
A composite product comprising: a. a substrate having carbonized fibers; b. particles of carbide in the interstices of said carbonized fibers; and c. pyrolytic carbon surrounding said carbonized fibers and said carbide particles.
Claim 40
Dependent Claim
33 words
A composite product comprising: a. a substrate having carbonized fibers; b. particles of carbide in the interstices of said carbonized fibers; and c. pyrolytic carbon surrounding said carbonized fibers and said carbide particles.
Claim 41
Dependent Claim
54 words
A composite product comprising: a. a substrate having carbonized fibers infiltrated with pyrocarbon; and b. small particles of metal salt distributed throughout the substrate between the fibers of the substrate, said metal salt being selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb.
Claim 42
Dependent Claim
54 words
A composite product comprising: a. a substrate having carbonized fibers infiltrated with pyrocarbon; and b. small particles of metal salt distributed throughout the substrate between the fibers of the substrate, said metal salt being selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb.
Claim 43
Dependent Claim
58 words
A composite product comprising: a. a substrate having carbonized fibers infiltrated with pyrocarbon which has subsequently been graphitized; and b. particles of metal salt distributed throughout the substrate between the fibers of the substrate said metal salt being selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb.
Claim 44
Dependent Claim
58 words
A composite product comprising: a. a substrate having carbonized fibers infiltrated with pyrocarbon which has subsequently been graphitized; and b. particles of metal salt distributed throughout the substrate between the fibers of the substrate said metal salt being selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb.
Claim 45
Independent Claim
105 words
A method of forming a composite product comprising: a. heating a substrate having carbonized fibers to temperatures of 1,500* to 2,500*F; b. infiltrating hydrocarbon gas into said substrate to coat said carbonized fibers with pyrolytic carbon; c. introducing a metallic salt solution between the fibers of said substrate, said metallic salt solution consisting of a solvent and a metAl salt selected from a group consisting of Hf, Zr, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb; and d. drying out said metallic salt solution at a temperature of about 60*C to 100*C to leave alloy particles in the interstices of the fibers.
Claim 46
Independent Claim
105 words
A method of forming a composite product comprising: a. heating a substrate having carbonized fibers to temperatures of 1,500* to 2,500*F; b. infiltrating hydrocarbon gas into said substrate to coat said carbonized fibers with pyrolytic carbon; c. introducing a metallic salt solution between the fibers of said substrate, said metallic salt solution consisting of a solvent and a metAl salt selected from a group consisting of Hf, Zr, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb; and d. drying out said metallic salt solution at a temperature of about 60*C to 100*C to leave alloy particles in the interstices of the fibers.
Claim 47
Independent Claim
123 words
A method of forming a composite product comprising: a. heating a substrate having carbonized fibers to temperatures of 1,500* to 2,500*F; b. infiltrating hydrocarbon gas into said substrate to coat said carbonized fibers with pyrolytic carbon; c. annealing the infiltrated substrate to convert the carbonized fibers and the pyrolytic carbon coating to graphite; d. introducing a metallic salt solution between the fibers of said substrate, said metallic salt solution consisting of a solvent and a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb; and e. drying out said metallic salt solution at a temperature of about 60*C to 110*C to leave alloy particles in the interstices of the fibers.
Claim 48
Independent Claim
123 words
A method of forming a composite product comprising: a. heating a substrate having carbonized fibers to temperatures of 1,500* to 2,500*F; b. infiltrating hydrocarbon gas into said substrate to coat said carbonized fibers with pyrolytic carbon; c. annealing the infiltrated substrate to convert the carbonized fibers and the pyrolytic carbon coating to graphite; d. introducing a metallic salt solution between the fibers of said substrate, said metallic salt solution consisting of a solvent and a metal salt selected from a group consisting of Hf, Zr, Ta, Cb, W, Mo, Ti, V, Cr, Si, B, P and Pb; and e. drying out said metallic salt solution at a temperature of about 60*C to 110*C to leave alloy particles in the interstices of the fibers.
Claim 49
Independent Claim
58 words
A method of forming a composite product comprising: a. introducing a metallic particle suspension solution between carbonized fibers of a substrate; b. drying out said solution to leave small metal particles in the interstices of the carbonized fibers; and c. infiltrating the substrate with pyrolytic carbon to encapsulate the metal particles and tie them to the fibrous substrate.
Claim 50
Independent Claim
58 words
A method of forming a composite product comprising: a. introducing a metallic particle suspension solution between carbonized fibers of a substrate; b. drying out said solution to leave small metal particles in the interstices of the carbonized fibers; and c. infiltrating the substrate with pyrolytic carbon to encapsulate the metal particles and tie them to the fibrous substrate.
Claim 51
Dependent Claim
25 words
A method as defined in claim 38 in which after the infiltration step the substrate is heat treated to convert the metal particles to carbide.
References Cited (Backward Citations)
US3208872A
Cited
US3187502A
Cited
US3271181A
Cited
US3281261A
Cited
US3432336A
Cited
US3369920A
Cited
US3447952A
Cited
US3301763A
Cited
US3385915A
Cited
US3403008A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1976-01-30 | 1976-07-31 | 1977-01-30 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1980-01-30 | 1980-07-31 | 1981-01-30 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1984-01-30 | 1984-07-31 | 1985-01-30 | $7700.00 | Window Closed / Lapsed |