WO2012118808A2 - Nanotubes de carbone associés à du pentafluorure d'antimoine - Google Patents

Nanotubes de carbone associés à du pentafluorure d'antimoine Download PDF

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Publication number
WO2012118808A2
WO2012118808A2 PCT/US2012/026949 US2012026949W WO2012118808A2 WO 2012118808 A2 WO2012118808 A2 WO 2012118808A2 US 2012026949 W US2012026949 W US 2012026949W WO 2012118808 A2 WO2012118808 A2 WO 2012118808A2
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Prior art keywords
carbon nanotubes
molecules
composition
antimony pentafluoride
intercalated
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PCT/US2012/026949
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English (en)
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WO2012118808A3 (fr
Inventor
Padraig G. MOLONEY
Pulickel M. Ajayan
Enrique V. Barrera
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William Marsh Rice University
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Publication of WO2012118808A3 publication Critical patent/WO2012118808A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • 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
    • C01B32/168—After-treatment
    • 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
    • C01B32/168—After-treatment
    • C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
    • 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
    • C01B2202/10—Filled nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Definitions

  • the present invention pertains to compositions that include carbon nanotubes and antimony pentafluoride molecules associated with the carbon nanotubes.
  • the carbon nanotubes are at least one of single-walled carbon nanotubes, multi- walled carbon nanotubes, double-walled carbon nanotubes, few-walled carbon nanotubes, ultrashort carbon nanotubes, and combinations thereof.
  • the carbon nanotubes are endohedrally intercalated with the antimony pentafluoride molecules. In some embodiments, the carbon nanotubes are exohedrally intercalated with the antimony pentafluoride molecules. In other embodiments, the carbon nanotubes are exohedrally and endohedrally intercalated with the antimony pentafhioride molecules.
  • the method comprises associating carbon nanotubes with antimony pentafhioride molecules.
  • the associating step comprises mixing the carbon nanotubes with the antimony pentafhioride molecules.
  • the associating step occurs in an inert atmosphere, such as non-aqueous conditions.
  • the carbon nanotube compositions of the present invention can also have various arrangements. For instance, in some embodiments, the carbon nanotube compositions of the present invention can be used as part of a composite. In other embodiments, the carbon nanotube compositions of the present invention can be used as part of a carbon nanotube fiber.
  • the carbon nanotube compositions of the present invention provide various advantageous properties, including enhanced conductivity and stability.
  • the carbon nanotube compositions of the present invention can be used for various electrical applications, including use as conducting wires, motor windings and battery components.
  • FIGURE 1 shows a setup for a vacuum heating flask (FIG. 1A) and a nitrogen filled glove-bag (FIG. IB) that were used to make antimony pentafhioride (SbFs) intercalated. single- walled carbon nanotubes (SWNTs).
  • FIG. 1A vacuum heating flask
  • FIG. IB nitrogen filled glove-bag
  • SBFs antimony pentafhioride
  • SWNTs single- walled carbon nanotubes
  • FIGURE 2 shows the resultant SbF 5 intercalated SWNTs that were formed from the use of the setup in FIG. 1.
  • FIGURE 3 shows scanning electron microscope (SEM) images of two types of SbFs intercalated SWNTs.
  • FIGS. 3A and 3B show low resolution SEM images of large diameter and small diameter SWNTs.
  • FIG. 3C shows a high resolution SEM image of small diameter SWNTs.
  • FIGURE 4 illustrates the characterization of SbFs intercalated SWNTs containing large diameter SWNTs.
  • FIG. 4A is a scanning transmission electron microscopy (STEM) image of the SWNTs.
  • FIG. 4B is an energy dispersive x-ray spectroscopy (EDS) of the SWNTS.
  • STEM scanning transmission electron microscopy
  • EDS energy dispersive x-ray spectroscopy
  • FIGURE 5 shows STEM images of large diameter SbF 5 intercalated SWNTs.
  • FIGURE 6 shows STEM images of small diameter SbF 5 intercalated SWNTs.
  • FIGURE 7 is an EDS of small diameter SbF 5 intercalated SWNTs.
  • FIGURE 8 shows EDS and STEM area scans of small diameter SbF 5 intercalated SWNTs. The scans confirm the presence of C, Sb and F in the compositions.
  • FIGURE 9 shows thermographic analysis (TGA) data for GCIOO SbF 5 intercalated SWNTs.
  • FIGURE 10 shows TGA data for HiPco SbF 5 intercalated SWNTs.
  • intercalation is a term used to describe the reversible incorporation of a foreign molecule between two other molecules, most often in a periodic structure. For instance, intercalation is associated with the incorporation of foreign species between layers of graphite to form graphite intercalation compounds (GICs).
  • GICs graphite intercalation compounds
  • compositions of the present invention provide applications where electrically conductive materials are needed, such as in batteries, motor windings and wires.
  • the present invention pertains to compositions that include carbon nanotubes and SbFs molecules that are associated with the carbon nanotubes.
  • Various carbon nanotubes may be utilized in such compositions.
  • SbFs may have various forms of associations with the carbon nanotubes.
  • Suitable carbon nanotubes include single-walled carbon nanotubes (SWNTs), double-walled carbon nanotubes (DWNTs), multi-walled carbon nanotubes (MWNTs), few- walled carbon nanotubes (FWNTs), ultra-short carbon nanotubes, and combinations thereof.
  • the carbon nanotube compositions of the present invention include SWNTs.
  • the carbon nanotubes are pristine carbon nanotubes.
  • the carbon nanotubes are functionalized with various functional groups.
  • suitable functional groups include carboxyl groups, carbonyl groups, oxides, alcohol groups, phenol groups, aryl groups, and combinations thereof.
  • the carbon nanotubes are combinations of pristine and functionalized carbon nanotubes.
  • the functionalization of carbon nanotubes helps separate, de- aggregate or individualize carbon nanotubes. This in turn provides a more effective environment for associating the carbon nanotubes with SbFs or other dopants (such as iodine).
  • SbF 5 molecules are associated with carbon nanotubes. To Applicants' knowledge, SbF 5 was not previously combined with carbon nanotubes.
  • SbFs association generally refers to the reversible or irreversible incorporation of SbFs molecules with carbon nanotubes.
  • SbFs molecules may be associated with carbon nanotubes in various manners.
  • the SbF 5 molecules may be intercalated with carbon nanotubes. Such intercalation may involve the reversible association of carbon nanotubes with the SbFs molecules.
  • the carbon nanotubes may be doped with SbFs molecules. Such doping may involve the reversible or irreversible incorporation of the SbF 5 molecules with the carbon nanotubes.
  • the SbFs molecules may be endohedrally intercalated with SbFs molecules.
  • the SbFs molecules may be included in free spaces within carbon nanotubes.
  • the carbon nanotubes are exohedrally intercalated with the SbF 5 molecules.
  • the SbFs molecules may be included between outer surfaces of carbon nanotubes.
  • SbF 5 molecules may replace carbon atoms within a carbon nanotube structure.
  • the carbon nanotubes may be exohedrally and endohedrally intercalated with the SbFs molecules.
  • SbFs molecules may be located near or within defective carbon nanotube sites (e.g., holes or openings within the sidewalls)
  • the carbon nanotubes of the present invention may also be associated with one or more dopants.
  • suitable dopants include compounds or heteroatoms containing iodine, silver, chlorine, bromine, potassium, fluorine, gold, copper, aluminum, sodium, iron, boron, antimony, arsenic, silicon, sulfur, and combinations thereof.
  • the carbon nanotubes may be associated (i.e., doped) with one or more heteroatoms, such as AuCl 3 or BH 3 .
  • the carbon nanotubes may be associated with an acid, such as sulfuric acid or nitric acid.
  • the carbon nanotubes may also be associated with arsenic pentafluoride (AsF 5 ), metal chlorides (e.g., FeCl 3 and/or CuCl 2 ), iodine, melamine, carboranes, aminoboranes, phosphines, aluminum hydroxides, silanes, polysilanes, polysiloxanes, sulfides, thiols, and combinations thereof.
  • the carbon nanotubes of the present invention may be associated with iodine and SbFs.
  • the carbon nanotube compositions of the present invention may also be associated with one or more polymers.
  • suitable polymers include polyethylenes, polypropylenes, poly(methyl methacrylate) (PMMA) , polyvinyl alcohols (PVA), epoxide resins, and combinations thereof.
  • Additional embodiments of the present invention pertain to methods of making the above-mentioned carbon nanotube compositions. Such methods generally comprise associating carbon nanotubes with SbFs molecules.
  • the associating step comprises mixing the carbon nanotubes with the SbF 5 molecules.
  • the associating step occurs in an inert atmosphere.
  • inert atmospheres may include non-aqueous environments, oxygen-free environments, and/or environments under a steady flow of an insert gas (e.g., Ar, N 2 , and combinations of such gases).
  • association occurs by sputtering or spraying the SbF 5 molecules onto carbon nanotubes. In some embodiments, the association may occur by chemical vapor deposition. Additional association methods can also be envisioned.
  • the carbon nanotube compositions of the present invention can have various arrangements.
  • the carbon nanotube compositions of the present invention can be used as part of a composite.
  • the carbon nanotube compositions of the present invention can be used as part of a carbon nanotube fiber. Examples of such carbon nanotube fibers are disclosed in Applicants' co-pending Provisional Patent Application No. 61/449,309 and the corresponding PCT Application entitled "Doped Multi- walled Carbon Nanotube Fibers and Methods of Making the Same", which is concurrently being filed herewith.
  • the carbon nanotube compositions of the present invention also provide various advantageous properties.
  • a highly unstable acid (SbFs) with carbon nanotubes, Applicants have produced a composition that is stable and resistant to normal atmospheric conditions.
  • the formed carbon nanotube composition also has a higher electrical conductivity than that of the carbon nanotubes alone. In fact, an improved electrical conductivity by a factor of ten has already been observed.
  • the carbon nanotube fibers of the present invention provide numerous applications.
  • the carbon nanotube compositions of the present invention can be assembled into one dimensional, two dimensional or even three dimensional macroscopic engineering components.
  • Such structures could in turn be used as conducting wires, sensors, diodes, battery components, reinforcement fabrics in composites, thermal conductors, microwave absorption materials, motor windings, and components in energy harvesting or conversion systems.
  • the carbon nanotube compositions of the present invention can be utilized as hall-effect devices, infrared detectors, antifriction compositions, lead-free solders, fire retardant materials, and hardeners for lead in batteries.
  • the carbon nanotube compositions of the present invention may be used as fluorinating agents.
  • SbFs molecules were intercalated with SWNTs.
  • SbFs was chosen as the intercalate or dopant species due to its high conductivity, its ease of use relative to AsF 5 , and the novelty of the combination.
  • SWNTs and SbFs molecules were combined in a method based on one from Lalancette et al. Journal of the Chemical Society-Chemical Communications, 815 (1973).
  • the SWNTs were supplied by South West NanoTechnologies, Inc. (CG 100 grade).
  • These SWNTs were produced by a catalytic CVD process utilizing CO disproportionation at 700-950 °C in the presence of a Co-Mo catalysts.
  • 250 mg of as-produced SWNTs were dried by heating under vacuum in a boiling flask for 72 hours at a temperature range of 90-110°C. The setup is shown in FIG. 1A.
  • SWNTs were then transferred to a plastic glove bag for processing under an atmosphere of dry nitrogen. See FIG. IB.
  • FTIR Fourier transform infrared spectroscopy
  • Nicolet XPS data was also collected and analyzed
  • PHI Quantera Two primary materials were studied using SEM and scanning transmission electron microscopy (STEM): materials recovered from inside the vacuum line, and the main body of materials produced. The specimens shared a number of key characteristics, while some differences were also observed.
  • the materials from the vacuum line contained two types of tube structures: one similar in size to the starting SWNTs but with clear additions to the sidewalls; and a second tube type in the size range of 20-40nm. See FIG. 3 (and herein referred to as large diameter and small diameter SWNTs).
  • EDS energy dispersive x-ray spectroscopy
  • the main body of the sample showed a similar mix of two tube types, but the microscopy consistently found very rigid and straight nanotubes in the 20-40nm range. See FIG. 5.
  • High-resolution STEM images of the smaller (i.e., ⁇ 2nm) nanotubes suggest that the SWNTs are modified or functionalized SWNTs. See FIG. 6.
  • EDS data shows the presence of C, Sb and F on these smaller nanotubes. See FIGS. 7-8.
  • thermographic analysis (TGA) data confirmed that the CNTs suffered damage, as the oxidation peak has been broadened and shifted. See FIGS. 9-10. Without being bound by theory, the production of large diameter, straight tubular structures is envisioned. It is also envisioned that a considerable amount of metallic species has been added by the process (i.e., >40 ).
  • X-ray photoelectron spectroscopy (XPS) data did not provide a concrete answer to the species present. It appeared from the literature that no XPS standard for SbF 5 currently exists. The data collected showed the presence of C, Sb and F. Analysis software suggested numerous forms of Sb present, including KSbFs and KSbF 6 .
  • SWNTs were used in this Example, although MWNTs or other types of CNTs could have also been used.
  • DWNTs may provide a more robust nanotube surface, as STEM and TEM analyses of the GC 100 SWNTs showed a rough surface morphology of carbon.

Abstract

Dans certains modes de réalisation, la présente invention concerne des compositions qui comprennent des nanotubes de carbone associés à des molécules de pentafluorure d'antimoine. Dans certains modes de réalisation, les nanotubes de carbone sont intercalés de façon endohédrique avec les molécules de pentafluorure d'antimoine. Dans certains modes de réalisation, les nanotubes de carbone sont intercalés de façon exohédrique avec les molécules de pentafluorure d'antimoine. Des modes de réalisation supplémentaires de la présente invention concernent des procédés de fabrication des compositions de nanotubes de carbone susmentionnées. Dans certains modes de réalisation, le procédé consiste à associer les nanotubes de carbone avec les molécules de pentafluorure d'antimoine par mélange. Dans certains modes de réalisation, l'étape d'association se produit dans une atmosphère inerte. Les compositions de nanotubes de carbone de la présente invention peuvent présenter différentes dispositions. Dans certains modes de réalisation, les compositions de nanotubes de carbone de la présente invention peuvent être utilisées comme partie d'un composite. Dans d'autres modes de réalisation, les compositions de nanotubes de carbone de la présente invention peuvent être utilisées comme partie d'une fibre de nanotube de carbone.
PCT/US2012/026949 2011-02-28 2012-02-28 Nanotubes de carbone associés à du pentafluorure d'antimoine WO2012118808A2 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030133865A1 (en) * 2001-07-06 2003-07-17 William Marsh Rice University Single-wall carbon nanotube alewives, process for making, and compositions thereof
US6645455B2 (en) * 1998-09-18 2003-11-11 William Marsh Rice University Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof; and use of derivatized nanotubes to form catalyst-containing seed materials for use in making carbon fibers
US20040223900A1 (en) * 2002-11-15 2004-11-11 William Marsh Rice University Method for functionalizing carbon nanotubes utilizing peroxides
US20090326278A1 (en) * 2005-09-01 2009-12-31 Teodor Silviu Balaban Modified carbon nanoparticles, method for the production thereof and use thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6645455B2 (en) * 1998-09-18 2003-11-11 William Marsh Rice University Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof; and use of derivatized nanotubes to form catalyst-containing seed materials for use in making carbon fibers
US20030133865A1 (en) * 2001-07-06 2003-07-17 William Marsh Rice University Single-wall carbon nanotube alewives, process for making, and compositions thereof
US20040223900A1 (en) * 2002-11-15 2004-11-11 William Marsh Rice University Method for functionalizing carbon nanotubes utilizing peroxides
US20090326278A1 (en) * 2005-09-01 2009-12-31 Teodor Silviu Balaban Modified carbon nanoparticles, method for the production thereof and use thereof

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