WO2006137852A3 - Apparatus and methods for synthesis of large size batches of carbon nanostructures - Google Patents

Apparatus and methods for synthesis of large size batches of carbon nanostructures Download PDF

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Publication number
WO2006137852A3
WO2006137852A3 PCT/US2005/032624 US2005032624W WO2006137852A3 WO 2006137852 A3 WO2006137852 A3 WO 2006137852A3 US 2005032624 W US2005032624 W US 2005032624W WO 2006137852 A3 WO2006137852 A3 WO 2006137852A3
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WO
WIPO (PCT)
Prior art keywords
reaction zone
synthesis
methods
large size
carbon nanostructures
Prior art date
Application number
PCT/US2005/032624
Other languages
French (fr)
Other versions
WO2006137852A2 (en
Inventor
Alexandru Sorin Biris
Alexandru Radu Biris
Dan Lupu
Jon Gardner Wilkes
Dan Alexander Buzatu
Dwight Wayne Miller
Jerry Alexander Darsey
Original Assignee
Univ Arkansas
Alexandru Sorin Biris
Alexandru Radu Biris
Dan Lupu
Jon Gardner Wilkes
Dan Alexander Buzatu
Dwight Wayne Miller
Jerry Alexander Darsey
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US11/131,912 external-priority patent/US20050287297A1/en
Application filed by Univ Arkansas, Alexandru Sorin Biris, Alexandru Radu Biris, Dan Lupu, Jon Gardner Wilkes, Dan Alexander Buzatu, Dwight Wayne Miller, Jerry Alexander Darsey filed Critical Univ Arkansas
Publication of WO2006137852A2 publication Critical patent/WO2006137852A2/en
Publication of WO2006137852A3 publication Critical patent/WO2006137852A3/en

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
    • D01F9/133—Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087—Heating or cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/12—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by gravity in a downward flow
    • B01J8/125—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by gravity in a downward flow with multiple sections one above the other separated by distribution aids, e.g. reaction and regeneration sections
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/42—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with fluidised bed subjected to electric current or to radiations this sub-group includes the fluidised bed subjected to electric or magnetic fields
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4418—Methods for making free-standing articles
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/442—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using fluidised bed process
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45502—Flow conditions in reaction chamber
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45587—Mechanical means for changing the gas flow
    • C23C16/45591—Fixed means, e.g. wings, baffles
    • 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
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/10—Induction heating apparatus, other than furnaces, for specific applications
    • H05B6/105—Induction heating apparatus, other than furnaces, for specific applications using a susceptor
    • H05B6/108—Induction heating apparatus, other than furnaces, for specific applications using a susceptor for heating a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00389—Controlling the temperature using electric heating or cooling elements
    • B01J2208/00407—Controlling the temperature using electric heating or cooling elements outside the reactor bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00433—Controlling the temperature using electromagnetic heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Nanotechnology (AREA)
  • Thermal Sciences (AREA)
  • Electromagnetism (AREA)
  • Textile Engineering (AREA)
  • Combustion & Propulsion (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

An apparatus and method for synthesizing nanostructures. In one embodiment, the apparatus includes a reactor having a reaction zone and a conductive susceptor positioned in the reaction zone. The method includes the steps of transporting a gas mixture having an aerosolized catalyst, a feedstock and a carrier gas into the reaction zone of the reactor, inductively heating the reaction zone, and regulating a flow rate of the gas mixture to allow the catalyst to spend a sufficient amount of time in the reaction zone for the growth of nanostructures.
PCT/US2005/032624 2004-09-17 2005-09-15 Apparatus and methods for synthesis of large size batches of carbon nanostructures WO2006137852A2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US61101804P 2004-09-17 2004-09-17
US60/611,018 2004-09-17
US11/131,912 US20050287297A1 (en) 2004-05-18 2005-05-18 Apparatus and methods of making nanostructures by inductive heating
US11/313,912 2005-05-18

Publications (2)

Publication Number Publication Date
WO2006137852A2 WO2006137852A2 (en) 2006-12-28
WO2006137852A3 true WO2006137852A3 (en) 2007-12-06

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PCT/US2005/032624 WO2006137852A2 (en) 2004-09-17 2005-09-15 Apparatus and methods for synthesis of large size batches of carbon nanostructures

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3068028B1 (en) * 2017-06-26 2021-06-11 Nawatechnologies PROCESS FOR MANUFACTURING CARBON NANOTUBES FIXED ON A SUBSTRATE

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4147571A (en) * 1977-07-11 1979-04-03 Hewlett-Packard Company Method for vapor epitaxial deposition of III/V materials utilizing organometallic compounds and a halogen or halide in a hot wall system
US4900525A (en) * 1986-08-25 1990-02-13 Gte Laboratories Incorporated Chemical vapor deposition reactor for producing metal carbide or nitride whiskers
US5895526A (en) * 1995-08-07 1999-04-20 Nippondenso Co., Ltd. Process for growing single crystal
US6299683B1 (en) * 1996-01-30 2001-10-09 Siemens Aktiengesellschaft Method and apparatus for the production of SiC by means of CVD with improved gas utilization
US6336971B1 (en) * 1997-09-12 2002-01-08 Showa Denko Kabushiki Kaisha Method and apparatus for producing silicon carbide single crystal
WO2002060813A2 (en) * 2001-01-31 2002-08-08 William Marsh Rice University Process utilizing two zones for making single-wall carbon nanotubes
US20030148086A1 (en) * 2001-12-18 2003-08-07 Lisa Pfefferle Controlled growth of single-wall carbon nanotubes
US20040052289A1 (en) * 2000-03-07 2004-03-18 Chang Robert P.H. Carbon nanostructures and methods of preparation
US6713519B2 (en) * 2001-12-21 2004-03-30 Battelle Memorial Institute Carbon nanotube-containing catalysts, methods of making, and reactions catalyzed over nanotube catalysts
US20040100902A1 (en) * 2002-11-27 2004-05-27 Pannalal Vimalchand Gas treatment apparatus and method
US6759025B2 (en) * 2000-09-22 2004-07-06 Iljin Nanotech Co., Ltd. Method of synthesizing carbon nanotubes and apparatus used for the same

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4147571A (en) * 1977-07-11 1979-04-03 Hewlett-Packard Company Method for vapor epitaxial deposition of III/V materials utilizing organometallic compounds and a halogen or halide in a hot wall system
US4900525A (en) * 1986-08-25 1990-02-13 Gte Laboratories Incorporated Chemical vapor deposition reactor for producing metal carbide or nitride whiskers
US5895526A (en) * 1995-08-07 1999-04-20 Nippondenso Co., Ltd. Process for growing single crystal
US6299683B1 (en) * 1996-01-30 2001-10-09 Siemens Aktiengesellschaft Method and apparatus for the production of SiC by means of CVD with improved gas utilization
US6336971B1 (en) * 1997-09-12 2002-01-08 Showa Denko Kabushiki Kaisha Method and apparatus for producing silicon carbide single crystal
US20040052289A1 (en) * 2000-03-07 2004-03-18 Chang Robert P.H. Carbon nanostructures and methods of preparation
US6759025B2 (en) * 2000-09-22 2004-07-06 Iljin Nanotech Co., Ltd. Method of synthesizing carbon nanotubes and apparatus used for the same
WO2002060813A2 (en) * 2001-01-31 2002-08-08 William Marsh Rice University Process utilizing two zones for making single-wall carbon nanotubes
US20030148086A1 (en) * 2001-12-18 2003-08-07 Lisa Pfefferle Controlled growth of single-wall carbon nanotubes
US6713519B2 (en) * 2001-12-21 2004-03-30 Battelle Memorial Institute Carbon nanotube-containing catalysts, methods of making, and reactions catalyzed over nanotube catalysts
US20040100902A1 (en) * 2002-11-27 2004-05-27 Pannalal Vimalchand Gas treatment apparatus and method

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