EP1901995A2 - Nanoparticules de carbone, leur production et leur utilisation - Google Patents

Nanoparticules de carbone, leur production et leur utilisation

Info

Publication number
EP1901995A2
EP1901995A2 EP06762488A EP06762488A EP1901995A2 EP 1901995 A2 EP1901995 A2 EP 1901995A2 EP 06762488 A EP06762488 A EP 06762488A EP 06762488 A EP06762488 A EP 06762488A EP 1901995 A2 EP1901995 A2 EP 1901995A2
Authority
EP
European Patent Office
Prior art keywords
carbon nanoparticles
carbon
nanoparticles according
spherical
fibers
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.)
Withdrawn
Application number
EP06762488A
Other languages
German (de)
English (en)
Inventor
Peter Axmann
Margret Wohlfahrt-Mehrens
Ulrich Storr
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Futurecarbon GmbH
Original Assignee
Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Futurecarbon GmbH
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
Application filed by Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg, Futurecarbon GmbH filed Critical Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Publication of EP1901995A2 publication Critical patent/EP1901995A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • 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
    • 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
    • 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
    • C01B2202/00—Structure or properties of carbon nanotubes
    • C01B2202/02—Single-walled nanotubes
    • 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
    • C01B2202/06—Multi-walled nanotubes
    • 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
    • C01B2202/36—Diameter
    • 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]

Definitions

  • Carbon nanoparticles their preparation and their use
  • the present invention relates to carbon nanoparticles of fibers or tubes which are morphologically present in the form of separate spherical and / or spherical secondary agglomerates, a process for their preparation and their use.
  • Nanomaterials Solid substances with nanoscopic particle sizes are called nanomaterials. Compared to microscopic particle sizes, this can lead to sudden changes in properties or even new product properties. Nanomaterials are attributed a high technical application potential. Compared with the variety of new nanoscopic material systems, however, only a few nanomaterials have already been established on the market.
  • carbon nanoparticles in the form of tubes or fibers also referred to as carbon nanotubes or fibers
  • arc discharge a carbon gas is generated between two carbon electrodes, from which carbon nanotubes are formed in the presence of a catalyst or even without a catalyst.
  • CVD Chemical Vapor Deposition
  • a carbon target is evaporated under Ar or He atmosphere by means of a laser. Upon cooling, the carbon units condense and form carbon nanomaterials.
  • a gaseous carbon source under reaction conditions for example methane, ethene or CO, as well as a catalyst, which usually contains active components from the series of transition elements Fe, Co and Ni, are used.
  • a catalyst which usually contains active components from the series of transition elements Fe, Co and Ni.
  • carbon nanotubes are deposited on the catalyst particles.
  • the Navonoubes are entangled here and fall in loose powder form.
  • Carbon, Vol. 41 (2003), pp. 539-547 describes the production of carbon nanotubes by a CVD process in which acetylene is used as carbon source and an iron catalyst. Again, the carbon nanotubes form entanglements.
  • the invention is therefore based on the object to provide carbon nanoparticles of fibers or tubes, in which the emission of nanoscopic units including carbon nanoparticles and metal nanoparticles is reduced to the environment and in terms of their separation and processing and Further processing in technically advanced processes are improved. Furthermore, a simple process for their production should be specified.
  • the invention thus provides carbon nanoparticles of fibers or tubes or combinations thereof, which are morphologically present in the form of macroscopic, mutually delimited spherical and / or spherical secondary agglomerates.
  • the invention further provides a process for the preparation of the carbon nanoparticles by a CVD process using nanoporous catalyst particles having a spherical and / or spherical secondary structure which contain as catalytically active components nanoparticulate metals and / or metal oxides or their precursors.
  • the invention relates to the use of the carbon nanoparticles, for example as adsorbents, additives or active materials in energy storage systems, in supercapacitors, as filter media, as supports for catalysts, as sensors or as a substrate for sensors or as additives for polymers, ceramics, Metals and metal alloys, glasses, textiles and composites, such as carbon composites.
  • the carbon nanoparticles according to the invention differ from conventional carbon nanoparticles in that they are morphologically present in the form of macroscopic, sharply delimited spherical and / or spherical secondary agglomerates.
  • the carbon nanoparticles according to the invention can be better used and optimized with respect to their technical further processing in comparison to the prior art.
  • the fibers or tubes of the carbon nanoparticles according to the invention typically have a diameter of 1-500 nm, preferably 10-100 nm, more preferably 10-50 nm.
  • the size of the secondary agglomerates is controllable by the size of the catalyst particles, the composition of the catalyst and the choice of synthesis parameters, such as carbon source, concentrations, temperatures and reaction time.
  • the shape of the final product is determined by the catalyst predetermined morphology.
  • the secondary agglomerates according to the invention preferably have a diameter of 500 nm to 1000 ⁇ m. The relative particle size distribution remains in the final product in comparison to the particle size distribution of the catalyst despite a strong volume increase.
  • the carbon originating from gaseous carbon sources dissolves in the catalytically active metal and can then be deposited again in nanoscopic form.
  • the secondary agglomerates contain no core of the catalyst particle, but consist entirely of carbon nanomaterials that are entangled in one another.
  • the carbon nanofibers of the present invention may be herringbone type as well as platelet-type and screw-type.
  • the carbon nanotubes can be of the single-walled or multi-walled type or of the loop type.
  • the circumference Up of the nanoparticles in two-dimensional projection and the circumference of a circle of equal area Uk in a ratio in the range of Uk: Up is from 1.0 to 0.65.
  • the preparation of the carbon nanoparticles according to the invention is carried out by a CVD method using nanoporous catalyst particles having a spherical and / or spheroidal secondary structure which contain nanoparticulate metals or their precursors as catalytically active components.
  • These catalyst particles may additionally contain metal oxides or their precursors, which serve as a substrate for the actually catalytically active metals.
  • the catalyst metal is in particular Fe, Co, Ni and Mn. Both the pure metals and metal oxide / metal composites can be used, as well as their precursors.
  • sparingly soluble compounds such as hydroxides, carbonates or other compounds that can be converted into catalytically active metals or metal / support composites can be used.
  • the carbon source used is the carbonaceous compounds used according to the prior art, which are reacted at the respective reaction temperature. be present in the gas, such as methane. Ethene, acetylene, CO,
  • Figures 2a, 2b and 2c are SEM images of the product of Example 1
  • Figures 5a, 5b and 5c are SEM images of the product of Example 2.
  • Figures 7a and 7b are SEM images of the catalyst used in Example 3.
  • Figures 8a, 8b, 8c and 8d are SEM images of the product of Example 3.
  • FIGS. 10a and 10b SEM images of the catalyst from Example 4.
  • Figures 13a and 13b are SEM images of the catalyst from Example 5
  • Figures 14a, 14b, 14c and 14d are SEM images of the product of Example 5.
  • Example 1 Preparation of Multi-walled Carbon Nanotube Spherical Aggregates via a Co / Mn-Based Catalyst
  • the catalyst is prepared by continuously combining three educt solutions.
  • Solution II 3130 ml of a solution of 960.4 g of Co (NO 3 ) 2 .6H 2 O and
  • the individual solutions are metered simultaneously with a constant metering rate over a period of 24 h in a 1 1 reactor, which allows intensive mixing and is equipped with an overflow, is continuously discharged through the product suspension.
  • the precipitation reaction takes place at 50 0 C.
  • the product is taken from the overflow.
  • the suspension has a deep blue-violet color.
  • the solid is separated on a suction filter from the mother liquor, then washed six times with 100 ml of demineralized water and then dried at 80 0 C for 30 h in a drying oven.
  • a pulverulent, readily flowable, violet precursor having a spherical particle morphology is obtained.
  • Figure 4 shows a size comparison between the catalyst particles used and the carbon nanoproduct obtained.
  • Example 2 Production of multi-walled carbon nanotube aggregates via a (Co, Mn) CO 3 catalyst
  • a catalyst according to Example 1 is used directly without prior activation for the production of multi-walled carbon nanotubes.
  • the conversion to multi-walled carbon nanotubes takes place as in Example 1 without a preceding reduction step.
  • the product shows a uniform distribution in the thickness of the nanotubes, as can be seen from the SEM images in Figures 5a, 5b, and 5c.
  • the TEM images in Figures 6a and 6b demonstrate the presence of multi-walled carbon nanotubes.
  • Example 3 Production of multi-walled carbon nanotube aggregates with narrow particle distribution over a (Co, Mn) CO 3 catalyst
  • a catalyst according to Example 1 is classified by sieving size and a particle size fraction of 20 microns - 32 microns used without prior activation directly as a catalyst.
  • Figures 7a and 7b show SEM images of the catalyst sieve fraction used.
  • Figures 10a and 10b show SEM images of the catalyst.
  • the activation of the catalyst takes place during heating between 300 0 C and 600 0 C by reduction of the precursor with H 2 for about 20 min. (Gas mixture 24 l / h C 2 H 4 , 6 l / h H 2 ).
  • the synthesis takes place at 500-600 0 C 2 h with a mixture of 32 l / h C 2 H 4 , 81 / h H 2 instead.
  • Figures I I a and I Ib show SEM images of the product. The morphological expression as sharply demarcated spherical and / or spherical secondary structures is preserved.
  • Figures 13a and 13b show SEM images of the catalyst sieve fraction> 20 ⁇ m.
  • the carbon nanofibers are synthesized under carbon monoxide / hydrogen (20: 8) over a four-hour period. A black voluminous product is obtained.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne des nanoparticules de carbone à base de fibres ou de tubes ou de combinaisons des deux, se présentant sous forme d'agglomérats secondaires morphologiquement macroscopiques, sphériques et/ou sphéroïdes, délimités les uns par rapport aux autres. L'invention concerne en outre un procédé permettant de produire des nanoparticules de carbone par un procédé de dépôt chimique en phase vapeur, au moyen de particules de catalyseur nanoporeuses de structure sphérique et/ou sphéroïde, qui contiennent comme constituants à action catalytique, des métaux nanoparticulaires et/ou des oxydes métalliques ou leurs précurseurs. Lesdites particules de carbone selon l'invention peuvent s'utiliser comme adsorbants, additifs ou matériaux actifs dans des systèmes d'accumulation d'énergie, dans des supercondensateurs, comme milieux filtrants, comme catalyseurs ou excipients pour catalyseurs, comme détecteurs ou comme substrats de détecteurs, comme additifs pour polymères, céramiques, métaux et alliages métalliques, verres, textiles et matériaux composites.
EP06762488A 2005-07-08 2006-07-07 Nanoparticules de carbone, leur production et leur utilisation Withdrawn EP1901995A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005032072A DE102005032072A1 (de) 2005-07-08 2005-07-08 Kohlenstoff-Nanopartikel, deren Herstellung und deren Verwendung
PCT/EP2006/006680 WO2007006511A2 (fr) 2005-07-08 2006-07-07 Nanoparticules de carbone, leur production et leur utilisation

Publications (1)

Publication Number Publication Date
EP1901995A2 true EP1901995A2 (fr) 2008-03-26

Family

ID=37461558

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06762488A Withdrawn EP1901995A2 (fr) 2005-07-08 2006-07-07 Nanoparticules de carbone, leur production et leur utilisation

Country Status (6)

Country Link
US (1) US20090081454A1 (fr)
EP (1) EP1901995A2 (fr)
JP (1) JP2009500281A (fr)
KR (1) KR20080048457A (fr)
DE (1) DE102005032072A1 (fr)
WO (1) WO2007006511A2 (fr)

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US20080053922A1 (en) * 2006-09-01 2008-03-06 Honsinger Charles P Jr Nanostructured materials comprising support fibers coated with metal containing compounds and methods of using the same
MY160277A (en) 2009-04-17 2017-02-28 Seerstone Llc Method of producing solid carbon by reducing carbon oxides
NO2749379T3 (fr) 2012-04-16 2018-07-28
US9221685B2 (en) 2012-04-16 2015-12-29 Seerstone Llc Methods of capturing and sequestering carbon
EP2838837A4 (fr) 2012-04-16 2015-12-23 Seerstone Llc Procédés et structures de réduction d'oxydes de carbone avec des catalyseurs non ferreux
EP2838839B1 (fr) 2012-04-16 2020-08-12 Seerstone LLC Procédé de production de carbone solide par réduction du dioxyde de carbone
WO2013158158A1 (fr) 2012-04-16 2013-10-24 Seerstone Llc Procédé de traitement d'un dégagement gazeux contenant des oxydes de carbone
US9896341B2 (en) 2012-04-23 2018-02-20 Seerstone Llc Methods of forming carbon nanotubes having a bimodal size distribution
JP6284934B2 (ja) 2012-07-12 2018-02-28 シーアストーン リミテッド ライアビリティ カンパニー カーボンナノチューブを含む固体炭素生成物およびそれを形成する方法
US10815124B2 (en) 2012-07-12 2020-10-27 Seerstone Llc Solid carbon products comprising carbon nanotubes and methods of forming same
JP6025979B2 (ja) 2012-07-13 2016-11-16 シーアストーン リミテッド ライアビリティ カンパニー アンモニアおよび固体炭素生成物を形成するための方法およびシステム
US9779845B2 (en) 2012-07-18 2017-10-03 Seerstone Llc Primary voltaic sources including nanofiber Schottky barrier arrays and methods of forming same
MX382104B (es) 2012-11-29 2025-03-13 Seerstone Llc Reactores y métodos para producir materiales de carbono sólido.
US9783421B2 (en) 2013-03-15 2017-10-10 Seerstone Llc Carbon oxide reduction with intermetallic and carbide catalysts
US9783416B2 (en) 2013-03-15 2017-10-10 Seerstone Llc Methods of producing hydrogen and solid carbon
EP3129135A4 (fr) 2013-03-15 2017-10-25 Seerstone LLC Réacteurs, systèmes et procédés de formation de produits solides
US9586823B2 (en) 2013-03-15 2017-03-07 Seerstone Llc Systems for producing solid carbon by reducing carbon oxides
EP3129321B1 (fr) 2013-03-15 2021-09-29 Seerstone LLC Electrodes comprenant du carbone en nanostructure
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Also Published As

Publication number Publication date
KR20080048457A (ko) 2008-06-02
JP2009500281A (ja) 2009-01-08
DE102005032072A1 (de) 2007-01-11
WO2007006511A3 (fr) 2007-04-26
WO2007006511A2 (fr) 2007-01-18
US20090081454A1 (en) 2009-03-26

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