WO2013083931A1 - Procédé de synthèse amélioré de nanotubes de carbone sur multi-supports - Google Patents
Procédé de synthèse amélioré de nanotubes de carbone sur multi-supports Download PDFInfo
- Publication number
- WO2013083931A1 WO2013083931A1 PCT/FR2012/052840 FR2012052840W WO2013083931A1 WO 2013083931 A1 WO2013083931 A1 WO 2013083931A1 FR 2012052840 W FR2012052840 W FR 2012052840W WO 2013083931 A1 WO2013083931 A1 WO 2013083931A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- particles
- mixture
- fibers
- cnts
- ferrocene
- Prior art date
- Legal status (The legal status 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 status listed.)
- Ceased
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- 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
-
- 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
- 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
- C01B32/162—Preparation characterised by catalysts
-
- 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
- C01B32/164—Preparation involving continuous processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
- H01B3/445—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds from vinylfluorides or other fluoroethylenic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/26—Mechanical properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/734—Fullerenes, i.e. graphene-based structures, such as nanohorns, nanococoons, nanoscrolls or fullerene-like structures, e.g. WS2 or MoS2 chalcogenide nanotubes, planar C3N4, etc.
- Y10S977/742—Carbon nanotubes, CNTs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2918—Rod, strand, filament or fiber including free carbon or carbide or therewith [not as steel]
- Y10T428/292—In coating or impregnation
Definitions
- the subject of the invention is a process for the synthesis of carbon nanotubes (abbreviated NTC) by chemical vapor deposition (abbreviated as CVD) on the surface of articles under a stream of inert gas (s) using (i) a carbon source consisting of acetylene and / or xylene, and (ii) a catalyst comprising ferrocene, said articles being in the form of a mixture A (i) of particles and / or fibers of a material comprising at least at least one oxygen atom and (ii) particles and / or fibers of a material selected from carbides and / or comprising at least one silicon atom.
- NTC carbon nanotubes
- CVD chemical vapor deposition
- step (iv) recovering a mixture B at the end of step (iii), possibly after a cooling step, said mixture B being formed of the mixture A of articles comprising on their surface CNTs;
- the terms "material”, “reinforcement” or “material / reinforcement” are indifferently used to designate a material comprising at least one oxygen atom, for example ⁇ 2 ⁇ 3 and a material chosen from carbides and / or comprising at least one silicon atom, such as, for example, silicon nitride (Si3N), silicon carbide (SiC), silica (S12O), TiC and BC, said materials can be used to ensure for example, to composite materials physical and mechanical properties such as tensile strength, flexural strength and compressive strength, stiffness and service life, resistance to friction and wear, lightening of specific gravity, resistance corrosion, electrical and thermal conductivity and shielding of electromagnetic waves.
- the reaction chamber may be any device allowing a simultaneous and controlled introduction of chemical precursors, provided with at least one furnace with a gas circulation system and at least one gas and liquid flow meter for measuring and controlling the flow rates. gases and liquids.
- An example of a device that may be suitable for carrying out the method of the invention is shown in FIG. 12.
- the ferrocene can also be introduced alone into the chamber.
- the ferrocene prior to its introduction, the ferrocene is vaporized and it is the ferrocene vapor which is introduced into the reaction chamber for example by a flow of gas, for example argon optionally mixed with hydrogen .
- step (iv) the mixture B obtained at the end of step (iii), which comprises particles and / or fibers comprising on their surface CNTs, can be recovered (i) without prior cooling, for example at the outlet of the reactor when the synthesis is "continuous", or (ii) after cooling to a temperature of, for example, 15 to 100 ° C.
- the weight gain is more particularly between 5 and 50%, for example between 10 and 40% relative to the mass of the starting mixture A.
- FIGS. 4 and 5 show the photographs taken under a scanning electron microscope respectively (i) of a mixture of microparticles with average diameters of between 3 and 7 microns of Al 2 O 3 and SiC (50/50) and (i) of microparticles of AI2O3 alone after carrying out the synthesis process of the CNTs according to the invention at a temperature of 700 ° C.
- the overall mass yield refers to the ratio between the mass of nanotubes synthesized on the total mass of produced hybrids (nanotubes + micro-particles), such as: p "mass nanotube
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ES12810373.6T ES2578629T3 (es) | 2011-12-08 | 2012-12-07 | Procedimiento de síntesis mejorado de nanotubos de carbono sobre multisoportes |
| EP12810373.6A EP2788288B1 (fr) | 2011-12-08 | 2012-12-07 | Procédé de synthèse amélioré de nanotubes de carbone sur multi-supports |
| US14/363,826 US9779850B2 (en) | 2011-12-08 | 2012-12-07 | Process for synthesizing carbon nanotubes on multiple supports |
| JP2014545337A JP6422779B2 (ja) | 2011-12-08 | 2012-12-07 | 複数のサポート上にカーボンナノチューブを合成するための改善された方法 |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR1161344A FR2983846B1 (fr) | 2011-12-08 | 2011-12-08 | Procede de synthese ameliore de nanotubes de carbone sur multi-supports |
| FR1161344 | 2011-12-08 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2013083931A1 true WO2013083931A1 (fr) | 2013-06-13 |
Family
ID=47505235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/FR2012/052840 Ceased WO2013083931A1 (fr) | 2011-12-08 | 2012-12-07 | Procédé de synthèse amélioré de nanotubes de carbone sur multi-supports |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US9779850B2 (https=) |
| EP (1) | EP2788288B1 (https=) |
| JP (1) | JP6422779B2 (https=) |
| ES (1) | ES2578629T3 (https=) |
| FR (1) | FR2983846B1 (https=) |
| WO (1) | WO2013083931A1 (https=) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347326A (zh) * | 2015-11-19 | 2016-02-24 | 南昌大学 | 一种碳纳米葫芦结构材料的制备方法 |
| US9987608B2 (en) | 2014-09-19 | 2018-06-05 | NanoSynthesis Plus, Ltd. | Methods and apparatuses for producing dispersed nanostructures |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6688932B1 (ja) * | 2019-08-21 | 2020-04-28 | D−Power株式会社 | カーボンナノチューブ(cnt)製造に使用する材料の供給装置 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010066990A2 (fr) | 2008-12-08 | 2010-06-17 | Centre National De La Recherche Scientifique - Cnrs - | Procede de synthese de nanotubes de carbone sur materiaux micrometriques longs et particulaires |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2475790A1 (en) * | 2002-02-11 | 2003-08-21 | Rensselaer Polytechnic Institute | Directed assembly of highly-organized carbon nanotube architectures |
| US7981396B2 (en) * | 2003-12-03 | 2011-07-19 | Honda Motor Co., Ltd. | Methods for production of carbon nanostructures |
| US20070189953A1 (en) | 2004-01-30 | 2007-08-16 | Centre National De La Recherche Scientifique (Cnrs) | Method for obtaining carbon nanotubes on supports and composites comprising same |
| FR2927619B1 (fr) * | 2008-02-20 | 2011-01-14 | Commissariat Energie Atomique | Croissance de nanotubes de carbone sur substrats de carbone ou metalliques. |
-
2011
- 2011-12-08 FR FR1161344A patent/FR2983846B1/fr active Active
-
2012
- 2012-12-07 US US14/363,826 patent/US9779850B2/en active Active
- 2012-12-07 WO PCT/FR2012/052840 patent/WO2013083931A1/fr not_active Ceased
- 2012-12-07 JP JP2014545337A patent/JP6422779B2/ja active Active
- 2012-12-07 ES ES12810373.6T patent/ES2578629T3/es active Active
- 2012-12-07 EP EP12810373.6A patent/EP2788288B1/fr active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010066990A2 (fr) | 2008-12-08 | 2010-06-17 | Centre National De La Recherche Scientifique - Cnrs - | Procede de synthese de nanotubes de carbone sur materiaux micrometriques longs et particulaires |
Non-Patent Citations (8)
| Title |
|---|
| BRUNAUER; EMMET; TELLER, THE JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, vol. 60, pages 309 51938 |
| CI L ET AL: "Novel micro/nanoscale hybrid reinforcement: Multiwalled carbon nanotubes on SiC particles", ADVANCED MATERIALS 20041118 WILEY-VCH VERLAG DE, vol. 16, no. 22, 18 November 2004 (2004-11-18), pages 2021 - 2024, XP002678899, DOI: DOI:10.1002/ADMA.200400379 * |
| CI L J ET AL: "Direct growth of carbon nanotubes on the surface of ceramic fibers", CARBON, ELSEVIER, OXFORD, GB, vol. 43, no. 4, 1 January 2005 (2005-01-01), pages 883 - 886, XP004738900, ISSN: 0008-6223, DOI: 10.1016/J.CARBON.2004.11.010 * |
| J. K. YUAN; Z. M. DANG; S. H. YAO; J. W. ZHA; T. ZHOU; S. T. LI; J. BAI, J. MATER. CHEM., vol. 20, 2010, pages 2441 |
| Q. M. ZHANG; V. BHARTI; X. ZHAO, SCIENCE, vol. 280, 1998, pages 2101 |
| VEEDU V P ET AL: "Multifunctional composites using reinforced laminae with carbon-nanotube forests", NATURE MATERIALS, NATURE PUBLISHING GROUP, LONDON, GB, vol. 5, 1 June 2006 (2006-06-01), pages 457 - 462, XP002500845, ISSN: 1476-4660, DOI: 10.1038/NMAT1650 * |
| W. J. LI; Q. J. MENG; Y. S. ZHENG; Z. C. ZHANG; W. M. XIA; Z. XU, APPL. PHYS. LETT., vol. 96, 2010, pages 192905 |
| ZHAO Z-G ET AL: "The growth of multi-walled carbon nanotubes with different morphologies on carbon fibers", CARBON, ELSEVIER, OXFORD, GB, vol. 43, no. 3, 1 January 2005 (2005-01-01), pages 663 - 665, XP004694151, ISSN: 0008-6223, DOI: 10.1016/J.CARBON.2004.10.013 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9987608B2 (en) | 2014-09-19 | 2018-06-05 | NanoSynthesis Plus, Ltd. | Methods and apparatuses for producing dispersed nanostructures |
| CN105347326A (zh) * | 2015-11-19 | 2016-02-24 | 南昌大学 | 一种碳纳米葫芦结构材料的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| US9779850B2 (en) | 2017-10-03 |
| EP2788288A1 (fr) | 2014-10-15 |
| EP2788288B1 (fr) | 2016-05-04 |
| FR2983846A1 (fr) | 2013-06-14 |
| ES2578629T3 (es) | 2016-07-28 |
| JP2015507593A (ja) | 2015-03-12 |
| US20140343210A1 (en) | 2014-11-20 |
| JP6422779B2 (ja) | 2018-11-14 |
| FR2983846B1 (fr) | 2014-01-31 |
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