← Back to Patent Explorer
US3925577A Expired / Lapsed US ⏱️ 0.0 years remaining

Silicon carbide coated graphite members and process for producing the same

Assignee: Westinghouse Electric Corp
•
Filing: 1972-11-24
•
Granted: 1975-12-09
•
Expires: 1992-11-24
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract A preferred process for producing coated isotropic graphite members comprises: A. HEAT TREATING THE ISOTROPIC GRAPHITE MEMBER TO A TEMPERATURE FROM ABOUT 1700*C to 2400*C in a halogen atmosphere comprising chlorine or fluorine to reduce the impurity ash content to the range of the order to 2 to 10 ppm, B. MACHINING THE HEAT TREATED ISOTROPIC GRAPHITE MEMBER TO A PREDETERMINED SHAPE AND SURFACE CONDITION, C. ULTRASONICALLY CLEANING THE MACHINED GRAPHITE BODY IN A LIQUID CLEANING FLUID TO REMOVE LOOSE SURFACE PARTICLES, D. DEPOSITING A LAYER OF SILICON ON THE CLEAN GRAPHITE BODY BY A GAS PHASE REACTION AT A TEMPERATURE ABOVE 1000*C but below the melting point of silicon, E. HEATING THE GRAPHITE MEMBER WITH THE APPLIED LAYER OF SILICON TO A TEMPERATURE TO CAUSE THE SILICON TO MELT AND PENETRATE THE PORES OF THE GRAPHITE AND CAUSE THE SILICON TO REACT COMPLETELY IN SITU WITH THE GRAPHITE TO FORM A LAYER OF SILICON CARBIDE PENETRATING TO A DEPTH OF AT LEAST ABOUT 5 MILS, AND F. DEPOSITING BY A GAS PHASE REACTION A SEALING LAYER OF SILICON CARBIDE OVER THE UNDERLYING, PREVIOUSLY REACTED SILICON CARBIDE LAYER.

Inventors

  • 👤 Elmer G Fatzer
  • 👤 Edgar L Kochka

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 06:56
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/515; C04B35/52; C04B35/522; C04B41/00; C04B41/009; C04B41/45; C04B41/50; C04B41/5053; C04B41/5057; C04B41/5059; C04B41/80; C04B41/81; C04B41/85; C04B41/87; C23; C23C; C23C16/00; C23C16/22; C23C16/30; C23C16/32; C23C16/325; H; H01; H01J; H01J35/00; H01J35/02; H01J35/04; H01J35/08; H01J35/10; H01J35/108; H01J2235/00; H01J2235/08; H01J2235/083; H01J2235/084; Y; Y10; Y10S; Y10S148/00; Y10S148/025; Y10S148/073; Y10S148/134; Y10S148/148; Y10T; Y10T428/00; Y10T428/30

Claims Analysis

Total Claims: 7
Claim 1
Independent Claim 317 words
IN THE PROCESS OF APPLYING A SILICON CARBIDE COATING TO A GRAPHITE MEMBER TO PRODUCE A COMPOSITE STRUCTURE, THE STEPS COMPRISING: A. HEAT TREATING AT A TEMPERATURE OF FROM ABOUT 1700*C TO 2400*C AN ISOTROPIC GRAPHITE BODY COMPRISING FINE GRAINED ISOTROPIC GRAPHITE OF A DENSITY OF AT LEAST 1.75 GM/CC AND HAVING A COEFFICIENT OF THERMAL EXPANSION OF ABOUT 7.5 TO 8.3 INCH PER INCH PER DEGREE CENTIGRADE X 10-6, THE GRAPHITE GRAINS BEING OF A MAXIMUM PARTICLE SIZE OF LESS THAN 0.001 INCH, AND CHARACTERIZED BY A RELATIVELY UNIFORM DISTRIBUTION OF MANY INTERCONNECTED FINE PORES OF AN AVERAGE DIAMETER OF ABOUT 5 MICRONS AND LESS, THE PORES EXTENDING TO THE SURFACE OF THE BODY, THE HEAT TREATING BEING APPLIED FOR AT LEAST AN HOUR IN A HALOGEN ATMOSPHERE, THE HALOGEN COMPRISING AT LEAST ONE OF THE GROUP CONSISTING OF CHLORINE AND FLUORINE, THE HEAT-TREATMENT PURIFYING THE BODY TO REDUCE THE ASH IMPURITIES TO A RANGE OF THE ORDER OF 2 TO 10 PPM, B. MACHINING THE HEAT TREATED ISOTROPIC GRAPHITE BODY TO A MEMBER OF PREDETERMINED SHAPE AND SURFACE CONDITION, C. ULTRASONICALLY CLEANING THE MACHINED BODY IN A LIQUID CLEANING THE FLUID TO REMOVE LOOSE SURFACE PARTICLES, D. DEPOSITING SILICON BY A GAS PHASE REACTION ON THE SURFACES OF THE CLEANED ISOTROPIC GRAPHITE MEMBER WHILE AT A TEMPERATURE OF AT LEAST 1000*C BUT BELOW THE MELTING POINT OF SILICON, TO PROVIDE AN INFILTRATABLE LAYER OF SILICON ON THE SURFACES, E. HEATING THE SILICON COATED ISOTROPIC GRAPHITE MEMBER TO A TEMPERATURE AND FOR A PERIOD OF TIME TO CUASE THE SILICON TO MELT AND PENETRATE THE PORES AND CREVICES OF THE GRAPHITE MEMBER AND TO REACT COMPLETELY IN SITU WITH THE GRAPHITE TO FORM A LAYER OF SILICON CARBIDE TO A DEPTH OF AT LEAST ABOUT 5 MILS, AND F. DEPOSITING THEREOVER BY A GAS PHASE REACTION A SEALING LAYER OF SILICON CARBIDE ON THE GRAPHITE MEMBER.
Claim 2
Dependent Claim 317 words
IN THE PROCESS OF APPLYING A SILICON CARBIDE COATING TO A GRAPHITE MEMBER TO PRODUCE A COMPOSITE STRUCTURE, THE STEPS COMPRISING: A. HEAT TREATING AT A TEMPERATURE OF FROM ABOUT 1700*C TO 2400*C AN ISOTROPIC GRAPHITE BODY COMPRISING FINE GRAINED ISOTROPIC GRAPHITE OF A DENSITY OF AT LEAST 1.75 GM/CC AND HAVING A COEFFICIENT OF THERMAL EXPANSION OF ABOUT 7.5 TO 8.3 INCH PER INCH PER DEGREE CENTIGRADE X 10-6, THE GRAPHITE GRAINS BEING OF A MAXIMUM PARTICLE SIZE OF LESS THAN 0.001 INCH, AND CHARACTERIZED BY A RELATIVELY UNIFORM DISTRIBUTION OF MANY INTERCONNECTED FINE PORES OF AN AVERAGE DIAMETER OF ABOUT 5 MICRONS AND LESS, THE PORES EXTENDING TO THE SURFACE OF THE BODY, THE HEAT TREATING BEING APPLIED FOR AT LEAST AN HOUR IN A HALOGEN ATMOSPHERE, THE HALOGEN COMPRISING AT LEAST ONE OF THE GROUP CONSISTING OF CHLORINE AND FLUORINE, THE HEAT-TREATMENT PURIFYING THE BODY TO REDUCE THE ASH IMPURITIES TO A RANGE OF THE ORDER OF 2 TO 10 PPM, B. MACHINING THE HEAT TREATED ISOTROPIC GRAPHITE BODY TO A MEMBER OF PREDETERMINED SHAPE AND SURFACE CONDITION, C. ULTRASONICALLY CLEANING THE MACHINED BODY IN A LIQUID CLEANING THE FLUID TO REMOVE LOOSE SURFACE PARTICLES, D. DEPOSITING SILICON BY A GAS PHASE REACTION ON THE SURFACES OF THE CLEANED ISOTROPIC GRAPHITE MEMBER WHILE AT A TEMPERATURE OF AT LEAST 1000*C BUT BELOW THE MELTING POINT OF SILICON, TO PROVIDE AN INFILTRATABLE LAYER OF SILICON ON THE SURFACES, E. HEATING THE SILICON COATED ISOTROPIC GRAPHITE MEMBER TO A TEMPERATURE AND FOR A PERIOD OF TIME TO CUASE THE SILICON TO MELT AND PENETRATE THE PORES AND CREVICES OF THE GRAPHITE MEMBER AND TO REACT COMPLETELY IN SITU WITH THE GRAPHITE TO FORM A LAYER OF SILICON CARBIDE TO A DEPTH OF AT LEAST ABOUT 5 MILS, AND F. DEPOSITING THEREOVER BY A GAS PHASE REACTION A SEALING LAYER OF SILICON CARBIDE ON THE GRAPHITE MEMBER.
Claim 3
Dependent Claim 144 words
The process of claim 1 wherein the silicon deposition step (d) comprises passing a reactive gas mixture of silicon halide vapor, hydrogen, and an inert gas over the graphite member while the graphite member is at a temperature of at least about 1000*C, but below the melting temperature of the silicon whereby silicon is deposited on the graphite member from contact of the gas mixture therewith, the deposited silicon and the graphite being thereafter heated above the melting temperature of silicon for a period of time to cause it to infiltrate the pores of the graphite and thereafter to react completely in situ to form silicon carbide and the silicon carbide deposition step (f) comprises passing a reactive gas mixture of silicon halide vapor, a hydrocarbon gas, hydrogen and an inert gas, over the graphite member, to deposit a sealing layer of silicon carbide.
Claim 4
Dependent Claim 56 words
The process of claim 1, wherein the silicon carbide coating step (f) comprises heating the coated isotropic graphite member to at least about 1000*C and passing over the heated member a reactive gas mixture comprising a silicon halide, hydrogen and a hydrocarbon, whereby sealing coating of the refractory silicon carbide is deposited on the graphite member.
Claim 5
Dependent Claim 161 words
A composite structure comprising a. a substrate comprising a fine grained isotropic graphite member of a density of at least about 1.75 gm/cc, of a coefficient of thermal expansion of the order of 7.5 to 8.3 inch per inch per degrees Centigrade X 10 6, in which the grains are of a maximum particle size of less than 0.001 inch, and characterized by a relatively uniform distribution of many interconnected fine pores of an average diameter of about 5 microns and less, the pores extending to the surface of the member, and b. an all silicon carbide coating firmly bonded to and conforming to the surface of the isotropic member, the silicon carbide coating comprising a first portion infiltrated to a depth of at least about 5 mils into the pores of the surface of the isotropic graphite member and a superimposed sealing surface layer composed of silicon carbide, the composite structure having been produced by the process of claim 1.
Claim 6
Dependent Claim 25 words
The composite structure of claim 4, wherein the superimposed sealing surface layer portion of the silicon carbide coating is at least 0.3 mil in thickness.
Claim 7
Dependent Claim 232 words
A member suitable for use in chemical and metallurgical apparatus at temperatures of up to 3000*F and in contact with various chemicals and oxidizing and reducing gases comprising a shaped body having the structure and dimensions for such use thereof, the body comprising a. a substrate comprising a fine grained isotropic graphite member of a density of at least about 1.75 grams per Cc, and a coefficient of thermal expansion of the order of 7.5 to 8.3 inch per inch per degrees Centigrade X 10 6, in which the grains are of a maximum particle size of less than 0.001 inch, and characterized by a relatively uniform distribution of many interconnected fine pores of an average diameter of about 5 microns and less, the pores extending to the surface of the member, a surface of the substrate being subject to the chemicals and gases while at the high temperatures when in use, and b. the said surface of the substrate having applied thereto an all silicon carbide coating firmly bonded and conforming to said surface, said silicon carbide coating comprising a first underlying portion infiltrated to a depth of at least about 15 mils into the pores of the said surface of the isotropic graphite member and a superimposed sealing surface layer portion of a thickness of at least 0.5 mil, the member having been produced by the process of claim 1.

References Cited (Backward Citations)

US2677627A Cited
US2828231A Cited
US3019128A Cited
US2992127A Cited
US3095316A Cited
US3140193A Cited
US3164489A Cited
US3393085A Cited
US3329527A Cited
US3493423A Cited
US3385723A Cited
US3406044A Cited
US3459504A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1978-12-08 1979-06-09 1979-12-09 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1982-12-08 1983-06-09 1983-12-09 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1986-12-08 1987-06-09 1987-12-09 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag