US3537877A - Low temperature method for producing amorphous boron-carbon deposits - Google Patents

Low temperature method for producing amorphous boron-carbon deposits Download PDF

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Publication number
US3537877A
US3537877A US603781A US3537877DA US3537877A US 3537877 A US3537877 A US 3537877A US 603781 A US603781 A US 603781A US 3537877D A US3537877D A US 3537877DA US 3537877 A US3537877 A US 3537877A
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United States
Prior art keywords
boron
amorphous boron
carbon deposits
low temperature
carbon
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Expired - Lifetime
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US603781A
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English (en)
Inventor
Robert Bruce Reeves
Joseph J Gebhardt
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General Electric Co
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General Electric Co
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals

Definitions

  • Amorphous boron-carbon is deposited, at very low absolute pressure, on a substrate heated to 700-900 C., from a reactant gas mixture of boron hydride and acety lene.
  • the substrate is a filament
  • the pressure is 5 mm. mercury
  • the temperature is 850 C.
  • the boron hydride is diborane
  • the reactant gas mixture also includes hydrogen.
  • This invention relates to a process for producing amorphous boron-carbon deposits and more particularly to a process in which amorphous boron-carbon deposits are produced at relatively low temperature.
  • Amorphous boron-carbon deposits either in the boron carbide form or in non-stoichiometric mixtures of boron and carbon, have been found to have highly desirable mechanical properties. In particular, these materials are known for their extremely high tensile strength and modulus of elasticity even at very high temperatures. It should be noted that while this material is referred to herein as amorphous, this term is not intended to signify the complete absence of a crystalline structure in the deposit but instead indicates only that no crystalline structure is discernible by the presently available techniques, such as X-ray diffraction, etc.
  • Another object of this invention is to provide a practical low temperature process for producing amorphous boron-carbon deposits in a form which can be utilized as a structural material reinforcement.
  • a process which comprises, briefly, heating a substrate material to a temperature in the range from 700-900 C. at a very low pressure and contacting the substrate material with a gaseous mixture 3,537,877. Patented Nov. 3, 1970 of acetylene and a boron hydride.
  • a filamentary substrate is contacted with a mixture of acetylene, diborane, and hydrogen at a temperature of about 850 C. and a pressure of about 5 millimeters mercury.
  • boron hydrides which constitute the source of boron in the present invention
  • diborane is preferred because of its relative volatility, availability and low cost. These materials are relatively stable at ordinary temperatures and apparently undergo controlled decomposition at the reaction temperature and pressure of the present process. Although the specific mode of decomposition is unknown, it is likely that numerous intermediate products, including higher molecular weight boron hydrides, are formed as the decomposition proceeds. This further suggests that other boron hydrides may be used in lieu of, or in addition to, the better known and more readily available diborane.
  • amorphous boron-carbon deposits may be produced at low pressure by decomposition of a mixture consisting only of a boron hydride and acetylene
  • hydrogen is usually included in the reactant gas mixture.
  • the role of the hydrogen is two-fold. First, it aids in the reduction to boron carbide, and second, it moderates deleterious side reactions.
  • the effectiveness of the present invention to produce boron-carbon deposits in the temperature range below 1000 C. is an important feature of the process taught herein. It permits the production of amorphous boroncarbon deposits on many substrates which would undergo undesirable physical or chemical changes at temperatures above 1000 C.
  • the latter category includes metallic substrates, which may undergo crystalline changes or exhibit a loss in ductility if they are heated above 1000 C., and also includes substrates such as silica and glass which would deteriorate at temperatures above 1000 C.
  • the latter are particularly desirable substrates for use in producing low density boron-carbon filaments.
  • Such filaments, produced, in accordance with the present invention, by the deposition of amorphous boron-carbon on a filamentary silica or glass substrate have excellent potential as the reinforcing constituent of composite structural materials.
  • a tungsten filament 1 mill in diameter, was mounted axially in a horizontally disposed cylindrical reactor 2 inches long and inches in internal diameter.
  • This reactor included electrical contacts for resistively heating the filament in the reactor and means for maintaining a high vacuum and a low concentration of contaminants in the reactor.
  • Other features of the reactor included inlets and outlets for streams of reactant gases flowing generally perpendic ularly to the reactor axis and a reactant gas diverter, comprising a slotted barrier between the gas inlets and the filament in the reactor, for directing the reactant gases into the space immediately surrounding the filament.
  • the temperature of the substrate was raised to about 850 C. by resistive heating.
  • a mixture of hydrogen, flowing at 20 cubic centimeters per minute, diborane 3 flowing at 120 cubic centimeters per minute, and acetylene flowing at 30 cubic centimeters per minute was passed through the reactor. This resulted in production of an amorphous boron-carbon deposit at a rate, in diameter growth, of about 25 mils per hour.
  • the filament produced in the above example was hard and, under X-ray analysis, devoid of any discernible crystal structure.
  • an indefinite length of amorphous boron-carbon-coated filament may be produced by passing a substrate filament of indefinite length through a reactor of the type described in the above example. This filament would be continuously heated and contacted with the gaseous reactant mixture as it passes through the reactor.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Chemical Vapour Deposition (AREA)
US603781A 1966-09-28 1966-12-22 Low temperature method for producing amorphous boron-carbon deposits Expired - Lifetime US3537877A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US58248366A 1966-09-28 1966-09-28
US58779866A 1966-10-19 1966-10-19
US58893666A 1966-10-24 1966-10-24
US60378166A 1966-12-22 1966-12-22

Publications (1)

Publication Number Publication Date
US3537877A true US3537877A (en) 1970-11-03

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Family Applications (1)

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US603781A Expired - Lifetime US3537877A (en) 1966-09-28 1966-12-22 Low temperature method for producing amorphous boron-carbon deposits

Country Status (6)

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US (1) US3537877A (de)
CH (1) CH534744A (de)
DE (1) DE1621248A1 (de)
FR (1) FR93676E (de)
GB (1) GB1190824A (de)
SE (1) SE353354B (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3861953A (en) * 1969-03-27 1975-01-21 United Aircraft Corp Node-free boron composite filament
US4225355A (en) * 1979-02-16 1980-09-30 United Technologies Corporation Amorphous boron-carbon alloy in bulk form and methods of making the same
US4287259A (en) * 1979-12-05 1981-09-01 The United States Of America As Represented By The United States Department Of Energy Preparation and uses of amorphous boron carbide coated substrates
US4942062A (en) * 1984-06-27 1990-07-17 Coating Development Societe Anonyme Process for producing boron carbide coatings of controlled hardness
US5088202A (en) * 1988-07-13 1992-02-18 Warner-Lambert Company Shaving razors

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4716083A (en) * 1983-09-23 1987-12-29 Ovonic Synthetic Materials Company Disordered coating

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2671735A (en) * 1950-07-07 1954-03-09 Bell Telephone Labor Inc Electrical resistors and methods of making them
US2810365A (en) * 1952-12-31 1957-10-22 Shallcross Mfg Company Apparatus for resistor film deposition
US2853969A (en) * 1953-06-10 1958-09-30 Erie Resistor Ltd Apparatus for producing electric resistors
US3125428A (en) * 1964-03-17 Uethod for coating silica rods
US3365330A (en) * 1964-05-28 1968-01-23 Air Force Usa Continuous vapor deposition

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3125428A (en) * 1964-03-17 Uethod for coating silica rods
US2671735A (en) * 1950-07-07 1954-03-09 Bell Telephone Labor Inc Electrical resistors and methods of making them
US2810365A (en) * 1952-12-31 1957-10-22 Shallcross Mfg Company Apparatus for resistor film deposition
US2853969A (en) * 1953-06-10 1958-09-30 Erie Resistor Ltd Apparatus for producing electric resistors
US3365330A (en) * 1964-05-28 1968-01-23 Air Force Usa Continuous vapor deposition

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3861953A (en) * 1969-03-27 1975-01-21 United Aircraft Corp Node-free boron composite filament
US4225355A (en) * 1979-02-16 1980-09-30 United Technologies Corporation Amorphous boron-carbon alloy in bulk form and methods of making the same
US4287259A (en) * 1979-12-05 1981-09-01 The United States Of America As Represented By The United States Department Of Energy Preparation and uses of amorphous boron carbide coated substrates
US4942062A (en) * 1984-06-27 1990-07-17 Coating Development Societe Anonyme Process for producing boron carbide coatings of controlled hardness
US5088202A (en) * 1988-07-13 1992-02-18 Warner-Lambert Company Shaving razors

Also Published As

Publication number Publication date
CH534744A (de) 1973-03-15
DE1621248A1 (de) 1971-12-23
GB1190824A (en) 1970-05-06
FR93676E (fr) 1969-05-02
SE353354B (de) 1973-01-29

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