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US4855091A Expired / Lapsed US ⏱️ 0.0 years remaining

Method for the preparation of carbon filaments

Assignee: Dow Chemical Co
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Filing: 1985-04-15
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Granted: 1989-08-08
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Expires: 2005-04-15
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Abstract

Abstract A method of preparing carbon filaments which comprises exposing a suitable thermostable substrate which is covered with reduced monocrystalline metal particles with a diameter of at least 5 nanometers to a carbon containing gas mixture at temperatures of about 250° up to about 700° C. to 800° C., for a period of time sufficient to form filaments of the desired length, and thereafter removing the substrate and/or the metal particles. The filaments are characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along the axis of the filaments. A high carbide content is a prerequisite for the nucleation of the filamentous carbon with a fishbone like structure.

Inventors

  • 👤 John W. Geus
  • 👤 John W. Linowski

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-07 07:32
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; D01F9/12; D01F9/127; D01F9/1278; B; B82; B82Y; B82Y30/00; D01F9/1271; D01F9/1272

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 196 words
A method for the preparation of carbon filaments, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, and thereafter separating the carbon filaments from the support.
Claim 2
Independent Claim 196 words
A method for the preparation of carbon filaments, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, and thereafter separating the carbon filaments from the support.
Claim 3
Dependent Claim 25 words
The method of claim 1, including the step of employing monocrystalline metal particles on the support surface which are able to form unstable metal carbides.
Claim 4
Dependent Claim 22 words
The method of claim 1, wherein the ferromagnetic particles are selected from the group consisting of iron, cobalt, nickel, and alloys thereof.
Claim 5
Dependent Claim 20 words
The method of claim 1, wherein the metal particles have a particle size of at least about 10 nanometer (nm).
Claim 6
Dependent Claim 40 words
The method of claim 1, wherein said ferro-magnetic particles are located at the ends of the carbon filaments, and subjecting said filaments and particles to an electric field, a magnetic field, or a combination of an electric and magnetic field.
Claim 7
Dependent Claim 54 words
The method of claim 1, wherein, after completion of longitudinal growth of the carbon filaments, they are subjected to a controlled amount of a carbon-containing gas at a temperature at which the fibers no longer grow in said longitudinal direction, said temperature being in the range of from about 900° to about 1100° C.
Claim 8
Dependent Claim 42 words
The method of claim 1 or 6, wherein the carbon filaments are subjected to a temperature of from about 1100° to about 1800° C., in the absence of a carbon-containing gas, to effect a re-orientation of the crystals in the carbon filaments.
Claim 9
Dependent Claim 21 words
The method of claim 1, wherein a bundle of parallel carbon filaments is grown on the support covered by metal particles.
Claim 10
Dependent Claim 31 words
The method of claim 1, wherein said support is selected from the group consisting of non-metallic materials, metals not forming bulk carbide metal alloys, metal oxides, metal carbides, and metal sulfides.
Claim 11
Dependent Claim 42 words
The method of claim 9, wherein said non-metallic materials are selected from the group consisting of carbon, silica, alumina, and other inert support materials which exhibit desirable metal particle-support interactions to promote the formation of carbon filaments from the supported metal particles.
Claim 12
Independent Claim 213 words
A method for the preparation of reinforced polymers comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support, and impregnating the carbon filaments with a molten polymer, a monomer, or a mixture thereof, that is subsequently polymerized.
Claim 13
Independent Claim 213 words
A method for the preparation of reinforced polymers comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support, and impregnating the carbon filaments with a molten polymer, a monomer, or a mixture thereof, that is subsequently polymerized.
Claim 14
Independent Claim 226 words
A method for the preparation of a reinforced polymer, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support, dispersing the carbon filaments in a molten polymer, a monomer, or mixture thereof, subjecting the suspension thus obtained to a shear force, and polymerizing the molten polymer, monomer, or mixture thereof.
Claim 15
Independent Claim 226 words
A method for the preparation of a reinforced polymer, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support, dispersing the carbon filaments in a molten polymer, a monomer, or mixture thereof, subjecting the suspension thus obtained to a shear force, and polymerizing the molten polymer, monomer, or mixture thereof.
Claim 16
Independent Claim 241 words
A method for the preparation of a reinforced polymer, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support with the metal particles attached to the ends of the filaments, dispersing the carbon filaments in a molten polymer, monomer, or mixture thereof, and subjecting the suspension to an applied external electric and magnetic field or a combination of an electric and magnetic field during solidification.
Claim 17
Independent Claim 241 words
A method for the preparation of a reinforced polymer, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, separating the carbon filaments from the support with the metal particles attached to the ends of the filaments, dispersing the carbon filaments in a molten polymer, monomer, or mixture thereof, and subjecting the suspension to an applied external electric and magnetic field or a combination of an electric and magnetic field during solidification.
Claim 18
Independent Claim 231 words
A method for the production of an electrode, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, raising the temperature to above about 900° C. while maintaining the atmosphere of the carbon-containing gas mixture to enhance the growth of carbon deposits on the filaments to form a dense and homogeneous block of carbon, and separating the carbon block from the support.
Claim 19
Independent Claim 231 words
A method for the production of an electrode, comprising the steps of exposing a thermostable support having substantially completely reduced monocrystalline ferro-magnetic metal particles to a carbon containing gas at a temperature of from about 250° C. up to about 700° C. to 800° C. for a period of time sufficient to promote epitaxial growth of graphite layers at the interface of the metal particle and the support, substantially each of said metal particle having a particle size of at least about 5 nanometers, forming carbon filaments on the support, the upper temperature limit of from 700° C. to 800° C. being contingent upon the stability of a metal carbide which is formed preceding the nucleation of filamentous carbon, said filaments being characterized by a crystalline graphitic structure and a morphology defined by a fishbone-like arrangement of the graphite layers along an axis of the filaments, adjusting loading of the support surface with the metal particles prior to the step of exposing the support and metal particles to the carbon containing gas to control the desired number of the carbon filaments per unit area of support surface, raising the temperature to above about 900° C. while maintaining the atmosphere of the carbon-containing gas mixture to enhance the growth of carbon deposits on the filaments to form a dense and homogeneous block of carbon, and separating the carbon block from the support.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1992-08-07 1993-02-06 1993-08-08 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1996-08-07 1997-02-06 1997-08-08 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2000-08-07 2001-02-06 2001-08-08 $7700.00 Window Closed / Lapsed

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