US3065088A - Oxidation-resistant graphite article and method - Google Patents

Oxidation-resistant graphite article and method Download PDF

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US3065088A
US3065088A US843364A US84336459A US3065088A US 3065088 A US3065088 A US 3065088A US 843364 A US843364 A US 843364A US 84336459 A US84336459 A US 84336459A US 3065088 A US3065088 A US 3065088A
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article
carbide
oxidation
silicon
percent
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Janes Milton
Sheldon A Taylor
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Union Carbide Corp
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Union Carbide Corp
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
    • C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B7/00—Heating by electric discharge
    • H05B7/02—Details
    • H05B7/06—Electrodes
    • H05B7/08—Electrodes non-consumable
    • H05B7/085—Electrodes non-consumable mainly consisting of carbon

Definitions

  • This invention relates to oxidation-resistant articles and it more particularly refers to such articles which are basically graphitic in nature.
  • this invention broadly comprises an oxidation-resistant article comprising graphite having silicon carbide and either titanium carbide, boron carbide or mixtures thereof substantially uniformly distributed throughout said article.
  • An article according to this invention may be produced by mixing some form of comminuted carbon, such as petroleum coke for example, with a carbonizable binder, suitably coal tar pitch, and either boron carbide, titanium carbide or mixtures thereof. After thorough mixing, these materials are formed into the desired shape by molding, extruding or other suitable means, and then the formed article is packed in a protective covering, preferably coke, and baked to approximately 850 C. according to the usual practice in the carbon industry. This baking carbonizes the binder thus curing the article and making it dimensionally stable. After the article is cured, the protective covering is removed and replaced with a siliconcontaining packing.
  • comminuted carbon such as petroleum coke for example
  • the thus-packed article is placed in a suitable graphitizing furnace and heated to a graphitizing temperature, suitably higher than 25 C., in a conventional manner. After a suitable time at the graphitizing temperature, which time depends upon the size of the article being produced, the graphitized article is cooled and removed from the furnace.
  • the article thus produced is basically graphitic in nature having either boron carbide, titanium carbide, or mixtures thereof and silicon carbide substantially uniformly distributed throughout the article.
  • the article according to this invention initially should suitably contain to 50 weight percent boron carbide, titanium carbide or mixtures thereof and should preferably contain 15 to 35 weight percent of such carbide after the initial baking step.
  • a thus-constituted article when properly graphitized according to the method described above, will pick up between and 70 percent silicon from the graphitization packing. The silicon picked up reacts to form silicon carbide inside the graphitized article. The amount of silicon pick-up and the amount of other carbide present in the article is determinative of the oxidation resistance of the finished graphitized article.
  • the proportions of each constituent in the finally graphitized article based upon the total weight of the final article are about 30 to weight percent graphite, about 15 to 60 weight percent silicon carhide, and about 10 to 30' weight percent in the aggregate of boron carbide, titanium carbide or mixtures thereof. It is preferred to have a silicon carbide concentration of from 30 to 50 weight percent.
  • the amount of silicon picked up to form silicon carbide from the silicon-containing packing during the graphitization step described above is a function of the graphitizing time and temperature and is also proportional to the amount and nature of the other carbides introduced into the mix from which the article is made.
  • Table I below is a compilation of data comparing the silicon pick up for articles /2 inch by /2 inch by 4% inches containing 18 weight percent boron carbide which were graphitized at temperatures from 2500 C. to 2900 C. for 30 minutes.
  • Table II below is a compilation of data comparing the silicon pick up, for articles /2 inch by /2 inch by 4% inches which have been graphitized at 2700 C. to 2800" C. for 30 minutes, to the amount of boron or titanium carbide initially added to the mix from which the article was made.
  • a formed graphite oxidation-resistant article having silicon carbide and at least one member of the group con sisting of boron carbide and titanium carbide substantially uniformly distributed therethrough.
  • a formed oxidation-resistant article consisting essentially of 10 to 30 percent by weight in the aggregate of at least one member of the group consisting of boron carbide and titanium carbide and the remainder graphite which additionally contains silicon carbide in a proportion of 15 to 60 percent by weight of said graphite and said aggregate; said carbides being substantially uniformly distributed throughout said article.
  • a formed oxidation-resistant article consisting essentially of 10 to percent by weight in the aggregate of at least one member of the group consisting of boron carbide and titanium carbide and the remainder graphite 'which additionally contains silicon carbide in a proportion of 30 to 50 percent by Weight of said graphite and said aggregate; said carbides being substantially uniformly distributed throughout said article,
  • a formed oxidation-resistant article which comprises mixing at least one member of the group consisting of titanium carbide and boron carbide with carbon and a carbonizable binder; forming said mixture into at least one shaped article; baking said formed article, thereby carbonizing said binder and curing said article, in a non-oxidizing atmosphere; covering said baked article with a silicon-containing packing; and graphitizing said article at 2500" C. to 2900 C.
  • the method of making a formed oxidation-resistant article which comprises mixing at least one member of the group consisting of titanium carbide and boron carbide with comminuted petroleum coke and coal tar pitch; forming said mixture into at least one shaped article; baking said formed article to about 850 C., thereby carbonizing said pitch and curing said article, in a protective coke covering; replacing at least part of said coke covering with sand; and graphitizing said article at about 2700 C. to about 2800 C. for about 30 minutes.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Ceramic Products (AREA)

Description

United States Patent ()fitice Fates-lied Nov. 20, 1962 3,065,088 @XEDA'llON-RESESTANT GRAPHITE ARTICLE AND METHOD Milton Janes, Lakewood, and Sheldon A. Taylor, Berea,
Ohio, assignors to Union Carbide Corperation, a corporation of New York No Drawing. Filed Sept. 30, 1959, Ser. No. 843,364 5 Claims. (Cl. 10644) This invention relates to oxidation-resistant articles and it more particularly refers to such articles which are basically graphitic in nature.
Recent developments in the field of aerodynamics have revealed a need for materials which will endure under conditions of high heat flux, with consequent high surface temperatures, and high velocity oxidizing gas flow relative to the material. It has been discovered that such a material must also be resistant to thermal shock since the conditions encountered lead to very rapid temperature rise. Graphite is one of the best refractory materials known today which is adapted to fulfill the requirements above set forth. However, graphite suffers from the fault of being subject to rapid oxidation and consequent erosion under the action of high velocity oxidizing gas streams.
It is therefore the principal object of this invention to provide graphitic articles which are relatively oxidation resistant.
It is another object of this invention to provide a method of producing such articles.
Fulfilling these objects this invention broadly comprises an oxidation-resistant article comprising graphite having silicon carbide and either titanium carbide, boron carbide or mixtures thereof substantially uniformly distributed throughout said article.
An article according to this invention may be produced by mixing some form of comminuted carbon, such as petroleum coke for example, with a carbonizable binder, suitably coal tar pitch, and either boron carbide, titanium carbide or mixtures thereof. After thorough mixing, these materials are formed into the desired shape by molding, extruding or other suitable means, and then the formed article is packed in a protective covering, preferably coke, and baked to approximately 850 C. according to the usual practice in the carbon industry. This baking carbonizes the binder thus curing the article and making it dimensionally stable. After the article is cured, the protective covering is removed and replaced with a siliconcontaining packing. The thus-packed article is placed in a suitable graphitizing furnace and heated to a graphitizing temperature, suitably higher than 25 C., in a conventional manner. After a suitable time at the graphitizing temperature, which time depends upon the size of the article being produced, the graphitized article is cooled and removed from the furnace. The article thus produced is basically graphitic in nature having either boron carbide, titanium carbide, or mixtures thereof and silicon carbide substantially uniformly distributed throughout the article.
The article according to this invention initially should suitably contain to 50 weight percent boron carbide, titanium carbide or mixtures thereof and should preferably contain 15 to 35 weight percent of such carbide after the initial baking step. A thus-constituted article, when properly graphitized according to the method described above, will pick up between and 70 percent silicon from the graphitization packing. The silicon picked up reacts to form silicon carbide inside the graphitized article. The amount of silicon pick-up and the amount of other carbide present in the article is determinative of the oxidation resistance of the finished graphitized article. The proportions of each constituent in the finally graphitized article based upon the total weight of the final article are about 30 to weight percent graphite, about 15 to 60 weight percent silicon carhide, and about 10 to 30' weight percent in the aggregate of boron carbide, titanium carbide or mixtures thereof. It is preferred to have a silicon carbide concentration of from 30 to 50 weight percent.
It has been determined that the amount of silicon picked up to form silicon carbide from the silicon-containing packing during the graphitization step described above is a function of the graphitizing time and temperature and is also proportional to the amount and nature of the other carbides introduced into the mix from which the article is made. Table I below is a compilation of data comparing the silicon pick up for articles /2 inch by /2 inch by 4% inches containing 18 weight percent boron carbide which were graphitized at temperatures from 2500 C. to 2900 C. for 30 minutes.
Table II below is a compilation of data comparing the silicon pick up, for articles /2 inch by /2 inch by 4% inches which have been graphitized at 2700 C. to 2800" C. for 30 minutes, to the amount of boron or titanium carbide initially added to the mix from which the article was made.
Table II Boron carbide in original mix (percent) 7 11 17 29 0 14 Titanium carbide nal mix (percent) 0 0 0 0 29 14 Silicon weight gain (Dercent of sample weight850 C. bake) 30. 2 36.1 40. 5 46. 5 12. 5 47. 3
From a consideration of Table I and II, it may be seen that while silicon vapor is picked up from the packing during graphitization at any temperature up to 2900 C., an optimum graphitization temperature is 2700" C. to 2800 C. Similarly, the incorporation of amounts of boron or titanium carbide up to 50 Weight percent induce silicon pick-up from the packing. However the best results are obtained when 15 to 35 weight percent boron or titanium carbide or mixtures thereof is present in the body which is baked to 850 C.
Many articles have been made according to the practice of this invention and tested to determine the amount of resistance to oxidation imparted by the method disclosed herein. This testing consisted of resistance heating a test article to a given temperature by passing an electric current therethrough and directing a stream of air, initially at room temperature, at the heated article. Table III below is a compilation of data taken from the various tests run. The measure of oxidation resistance in these tests is the time it takes for a sample article to burn through thereby interrupting the current flow. Each of the articles tested was Mr inch in diameter and 4 inches long.
aeeacas 3 Table III Composition of Article Final Composition baked to 850 C. Graphiti- Percent Failure zation GraphitiZawt. gain Test Temp. time Tempera tion packing from (minutes) Percent Percent Percent ture, C. packing Percent Percent Percent Percent B40 TiO 0 B40 TiG S10 M 1 100 2, 800 coke 0 100 4,800 Watts 099.
input. 2 81.9 18.1 2, 500 d0 0 84. S 14.6 0.6 do 0.86. 3 81.9 18.1 2, 500 SiO+coke 7. 37 76.1 13. 10.4 d0 0.92. 4 81.9 18.1 2, 800 do 3S. 2 40.6 10. 0 39.8 do 15.9. 5 81.9 18.1 2, 800 coke 0 84. 8 14. 6 0.6 3,600 watts 0.83.
' input. 81. 9 18.1 2,700 SiO+c0ke 52. 0 41. 2 9.6 341), 81.9 18.1 2800 .do 45.0 45.2 10.1 88.3 12.7 1, 2, 900 do 22. 7 65. 8 7. 4 81. 9 18.1 2, 725 do 47.1 43. 0 10.0 60. 4 30.6 2, 700 do 40. 5 36.3 18. 4
30. 6 2, 800 coke 0 30. 6 2,800 SiC+eoke 26. b 30.6 2,700 do 14.0 15. 3 2, 800 coke 0 15. 3 2,800 SiO-l-coke 58.0
An analysis of the data presented in this table reveals that the oxidation resistance of an article which is basically graphitic in composition is increased provided the proper carbide in the proper proportions is incorporated into the mix from which the article is formed and that such formed, cured article is graphitized at the proper temperature while it is protected by a silicon-containing pack. A comparison of runs 5 vs. 7, 6 vs. 7, 7 vs. 8, and 10 vs. 13 points up the value of having all the variables noted above at their optimum in order to insure oxidation resistance.
What is claimed is:
l. A formed graphite oxidation-resistant article having silicon carbide and at least one member of the group con sisting of boron carbide and titanium carbide substantially uniformly distributed therethrough.
2. A formed oxidation-resistant article consisting essentially of 10 to 30 percent by weight in the aggregate of at least one member of the group consisting of boron carbide and titanium carbide and the remainder graphite which additionally contains silicon carbide in a proportion of 15 to 60 percent by weight of said graphite and said aggregate; said carbides being substantially uniformly distributed throughout said article.
3. A formed oxidation-resistant article consisting essentially of 10 to percent by weight in the aggregate of at least one member of the group consisting of boron carbide and titanium carbide and the remainder graphite 'which additionally contains silicon carbide in a proportion of 30 to 50 percent by Weight of said graphite and said aggregate; said carbides being substantially uniformly distributed throughout said article,
4. The method of making a formed oxidation-resistant article which comprises mixing at least one member of the group consisting of titanium carbide and boron carbide with carbon and a carbonizable binder; forming said mixture into at least one shaped article; baking said formed article, thereby carbonizing said binder and curing said article, in a non-oxidizing atmosphere; covering said baked article with a silicon-containing packing; and graphitizing said article at 2500" C. to 2900 C.
5. The method of making a formed oxidation-resistant article which comprises mixing at least one member of the group consisting of titanium carbide and boron carbide with comminuted petroleum coke and coal tar pitch; forming said mixture into at least one shaped article; baking said formed article to about 850 C., thereby carbonizing said pitch and curing said article, in a protective coke covering; replacing at least part of said coke covering with sand; and graphitizing said article at about 2700 C. to about 2800 C. for about 30 minutes.
References Cited in the file of this patent UNITED STATES PATENTS 2,154,271 Higgins Apr. 11, 1939 2,307,550 Toepfer Ian. 5, 1943 2,358,615 Arnott Sept. 14, 1944 2,906,632 Nickerson Sept. 29, 1959 2,908,553 Frank Oct. 13, 1959 2,997,744 Stoddard et al Aug. 29, 1961 3,003,860 Sermon et al Oct. 10, 1961 3,019,128 Smiley Jan. 30, 1962

Claims (2)

1. A FORMED GRAPHITE OXIDATION-RESISTANT ARTICLE HAVING SILICON CARBIDE AND AT LEAST ONE MEMBER OF THE GROUP CONSISTING OF BORON CARBIDE AND TITANIUM CARBIDE SUBSTANTIALLY UNIFORMLY DISTRIBUTED THERETHROUGH.
4. THE METHOD OF MAKING A FORMED OXIDATION-RESISTANT ARTICLE WHICH COMPRISES MIXING AT LEAST ONE MEMBER OF THE GROUP CONSISTING OF TITANIUM CARBIDE AND BORON CARBIDE WITH CARBON AND A CARBONIZABLE BINDER; FORMING SAID MIXTURE INTO AT LEAST ONE SHAPED ARTICLE; BAKING SAID FORMED ARTICLE, THEREBY CARBONIZING SAID BINDER AND CURING SAID ARTICLE, IN A NON-OXIDIZING ATMOSPHERE; COVERING SAID BAKED ARTICLE WITH A SILICON-CONTAINING PACKING; AND GRAPHITIZING SAID ARTICLE AT 2500*C. TO 2900*C.
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3140190A (en) * 1961-01-23 1964-07-07 Boeing Co Graphite base ceramic refractory composition
US3165864A (en) * 1961-03-13 1965-01-19 Carborundum Co Refractory body having high resistance to flame erosion and thermal shock
US3265528A (en) * 1963-03-27 1966-08-09 Bell Telephone Labor Inc Method of forming metal carbide coating on carbon base
US3419656A (en) * 1967-05-12 1968-12-31 Atomic Energy Commission Usa Method of making solid solution carbide-graphite compositions
US3520526A (en) * 1966-04-01 1970-07-14 Morganite Crucible Ltd Container having a composite refractory wall
US3649342A (en) * 1967-10-30 1972-03-14 Norton Co Product for fabrication of dense ceramic armorplate and like
US3676371A (en) * 1969-01-30 1972-07-11 Conradty Fa C High output electrode with stabilized electric arc
US3808012A (en) * 1971-04-19 1974-04-30 Carborundum Co Dense composite ceramic bodies
US4004934A (en) * 1973-10-24 1977-01-25 General Electric Company Sintered dense silicon carbide
US4863649A (en) * 1988-01-29 1989-09-05 Mitsubishi Pencil Co., Ltd. Process for producing carbon heat generator
US8923360B2 (en) 2010-07-01 2014-12-30 Graftech International Holdings Inc. Graphite electrodes

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2154271A (en) * 1937-03-02 1939-04-11 Carborundum Co Refractory article
US2307550A (en) * 1942-05-07 1943-01-05 Westinghouse Electric & Mfg Co Make-alive electrode and method of making
US2358615A (en) * 1941-10-22 1944-09-19 Westinghouse Electric & Mfg Co Starter electrode
US2906632A (en) * 1957-09-10 1959-09-29 Union Carbide Corp Oxidation resistant articles
US2908553A (en) * 1955-01-14 1959-10-13 Frank Hubert Process for the production of silicon carbide
US2997744A (en) * 1957-09-19 1961-08-29 Stephen D Stoddard Method of graphite preparation
US3003860A (en) * 1957-08-05 1961-10-10 Unimatic Mfg Inc Abrasive tools and methods of making and using same
US3019128A (en) * 1957-09-17 1962-01-30 Union Carbide Corp Coated carbonaceous articles

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2154271A (en) * 1937-03-02 1939-04-11 Carborundum Co Refractory article
US2358615A (en) * 1941-10-22 1944-09-19 Westinghouse Electric & Mfg Co Starter electrode
US2307550A (en) * 1942-05-07 1943-01-05 Westinghouse Electric & Mfg Co Make-alive electrode and method of making
US2908553A (en) * 1955-01-14 1959-10-13 Frank Hubert Process for the production of silicon carbide
US3003860A (en) * 1957-08-05 1961-10-10 Unimatic Mfg Inc Abrasive tools and methods of making and using same
US2906632A (en) * 1957-09-10 1959-09-29 Union Carbide Corp Oxidation resistant articles
US3019128A (en) * 1957-09-17 1962-01-30 Union Carbide Corp Coated carbonaceous articles
US2997744A (en) * 1957-09-19 1961-08-29 Stephen D Stoddard Method of graphite preparation

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3140190A (en) * 1961-01-23 1964-07-07 Boeing Co Graphite base ceramic refractory composition
US3165864A (en) * 1961-03-13 1965-01-19 Carborundum Co Refractory body having high resistance to flame erosion and thermal shock
US3265528A (en) * 1963-03-27 1966-08-09 Bell Telephone Labor Inc Method of forming metal carbide coating on carbon base
US3520526A (en) * 1966-04-01 1970-07-14 Morganite Crucible Ltd Container having a composite refractory wall
US3419656A (en) * 1967-05-12 1968-12-31 Atomic Energy Commission Usa Method of making solid solution carbide-graphite compositions
US3649342A (en) * 1967-10-30 1972-03-14 Norton Co Product for fabrication of dense ceramic armorplate and like
US3676371A (en) * 1969-01-30 1972-07-11 Conradty Fa C High output electrode with stabilized electric arc
US3808012A (en) * 1971-04-19 1974-04-30 Carborundum Co Dense composite ceramic bodies
US4004934A (en) * 1973-10-24 1977-01-25 General Electric Company Sintered dense silicon carbide
US4863649A (en) * 1988-01-29 1989-09-05 Mitsubishi Pencil Co., Ltd. Process for producing carbon heat generator
US8923360B2 (en) 2010-07-01 2014-12-30 Graftech International Holdings Inc. Graphite electrodes
US9253827B2 (en) 2010-07-01 2016-02-02 Graftech International Holdings, Inc. Graphite electrodes
US9497804B2 (en) 2010-07-01 2016-11-15 Graftech International Holdings Inc. Graphite electrode

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