EP2393966A1 - Fibrilles et fils de nanotubes de nitrure de bore - Google Patents

Fibrilles et fils de nanotubes de nitrure de bore

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Publication number
EP2393966A1
EP2393966A1 EP09839785A EP09839785A EP2393966A1 EP 2393966 A1 EP2393966 A1 EP 2393966A1 EP 09839785 A EP09839785 A EP 09839785A EP 09839785 A EP09839785 A EP 09839785A EP 2393966 A1 EP2393966 A1 EP 2393966A1
Authority
EP
European Patent Office
Prior art keywords
boron nitride
boron
nanotubes
laser beam
nitride nanotubes
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Withdrawn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
EP09839785A
Other languages
German (de)
English (en)
Other versions
EP2393966A4 (fr
Inventor
Michael W. Smith
Kevin Jordan
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Individual
Original Assignee
Individual
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Filing date
Publication date
Priority claimed from US12/322,591 external-priority patent/US8753578B1/en
Application filed by Individual filed Critical Individual
Publication of EP2393966A1 publication Critical patent/EP2393966A1/fr
Publication of EP2393966A4 publication Critical patent/EP2393966A4/fr
Withdrawn legal-status Critical Current

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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
    • B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0641—Preparation by direct nitridation of elemental boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0648—After-treatment, e.g. grinding, purification
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62286—Fibres based on nitrides
    • C04B35/6229—Fibres based on nitrides based on boron nitride
    • 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
    • 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
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
    • C01P2004/133—Multiwall nanotubes
    • 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
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/526—Fibers characterised by the length of the fibers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5284—Hollow fibers, e.g. nanotubes
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/10—Inorganic fibres based on non-oxides other than metals
    • D10B2101/14—Carbides; Nitrides; Silicides; Borides
    • 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
    • Y10T428/2916—Rod, strand, filament or fiber including boron or compound thereof [not as steel]

Definitions

  • the present invention relates to the production of nanostructures and more particularly to a method for the high rate production of long stranded boron nitride nanotube fibers, boron nitride nanotube fibrils and boron nitride nanotube yarns.
  • FW-BNNTs relatively high-aspect-ratio few-walled boron nitride nanotubes
  • FW-BNNTs have been produced in small amounts (from individual tubes to milligrams) by arc- discharge or laser heating methods.
  • a separate class of boron nitride nanotubes has also been produced by chemical vapor deposition of nitrogen compounds (e. g. ammonia) over ball-milled precursors, but these tubes are of larger diameter and do not exhibit the continuous crystalline sp2-type bonding structure which has drawn most theoretical interest.
  • BNNTs Boron nitride nanotubes
  • 2009 describes an apparatus for the large scale production of boron nitride nanotubes comprising; a pressure chamber containing; a continuously fed boron containing target; a source of thermal energy preferably a focused laser beam; a cooled condenser; a source of pressurized nitrogen gas; and a mechanism for extracting boron nitride nanotubes that are condensed on or in the area of the cooled condenser from the pressure chamber.
  • the disclosure of this application is similarly hereby incorporated herein by reference in its entirety.
  • boron nitride nanotubes and fibrils composed of single or multi-walled nanotubes aligned in bundles of tubes 20 ⁇ m and longer at a rate of above about 1 meter per second.
  • nanotube yarns comprised of twisted bundles of such nanotube fibrils are also described.
  • Figure 1 is a schematic side view of an apparatus useful in the successful practice of the present invention.
  • Figure 2 shows a collected mass of boron nitride nanotube fibrils harvested in accordance with the present invention.
  • Figure 3 shows a yarn formed by simply spinning the boron nitride fibril mass shown in Figure 2.
  • Figure 4 is a schematic representation of transmission electron microscope views of single and three-walled nanotubes in accordance with the present invention.
  • the boron- containing target is thermally excited by means of a laser, such as a free electron laser or a carbon dioxide laser.
  • the boron-containing target is made of compressed boron powder or compressed boron nitride powder.
  • the target is advantageously cylindrical, rotating, and illuminated on the radius, or cylindrical, rotating, and illuminated on one face.
  • the target may also be stationary. Further preferred target orientation and illuminations are described in greater detail below.
  • the source of boron vapor is advantageously provided by supplying energy to a solid boron-containing target, such energy being sufficient to break bonds in the solid boron-containing target, thereby allowing boron vapor to enter the vapor state.
  • This energy is preferably focused thermal energy.
  • This energy is conveniently and advantageously in the form of a laser beam which is directed at the solid boron-containing target.
  • Exemplary lasers employed to supply such a laser beam beneficially include a free electron laser and a carbon dioxide laser, among others known to the skilled artisan.
  • Other thermal techniques that produce an appropriately shaped boron vapor plume under the elevated ambient nitrogen pressure may also be useful.
  • the solid boron- containing target is a plug or block of pressed boron powder or pressed boron nitride powder.
  • a laser beam which is directed at the solid boron- containing target, is allowed to bore an depression in the solid boron- containing target as the laser beam is directed thereat, thereby creating a stream of boron vapor by laser heating inside the depression.
  • This stream of boron vapor is allowed to flow upwardly from the bottom of the depression and through the depression, after which it contacts the nitrogen gas.
  • the nitrogen gas is kept under pressure in a synthesis chamber which encloses the solid boron-containing target and contains the nitrogen gas under pressure.
  • nitrogen gas may be advantageously employed at a pressure greater than about 2 atmospheres but less than about 250 atmospheres, very excellent results are achieved if nitrogen gas is provided at a pressure from greater than about 2 atmospheres up to about 12 atmospheres.
  • Boron nitride nanotubes as described herein are formed according to the present invention at a nucleation site, preferably in the absence of a catalyst.
  • the nucleation site is advantageously a surface, especially a surface having an asperity. It has been found to be very beneficial if the nucleation site is the upper periphery of the indentation in the solid boron-containing target, where any asperity exists. Boron nitride nanotubes are formed at this nucleation site and propagate away therefrom in the direction of flow of the stream of boron vapor, which stream has been created by heating within the indentation.
  • the boron nitride nanotubes are harvested, advantageously continuously, by standard means known to the skilled artisan. As an example of such continuous harvesting, a growth rate of about 10 cm/sec for the boron nanotubes has been achieved by the present process.
  • a suitable, but not exclusively useful, harvesting process and apparatus are described below in connection with the description of the apparatus depicted in Figure 1.
  • boron nitride nanotubes are produced which are crystalline nanotubes having continuous, parallel, substantially defect-free and sp2 bonded walls. These nanotubes are single, double, few, and/or multi-walled nanotubes.
  • Highly preferred nanotubes prepared in accordance with the present invention have elongated lengths with inside diameters of between about 1.5 and about 2.5 nanometers and tubular walls having a thickness of at least one molecule boron nitride. Typical such nanotubes are shown in the schematic representation of transmission electron microscope photos of single and multi-walled nanotubes prepared in accordance tithe the present invention shown in Figure 4.
  • a preferred heating source comprising a laser beam comprising a 1.6 micron wavelength, 8 mm diameter, unfocused, 1 kW, beam from a FEL (free electron laser), propagates vertically downward into the target.
  • the target according to this example, a 2.5 cm diameter plug of pressed boron metal powder rotates on a turntable at 20 sec/revolution. The center of rotation of the target is offset by about a half beam diameter from the center of the beam, so that the laser drills or bores a depression about twice its diameter as the target spins.
  • An ambient temperature elevated pressure nitrogen gas is fed into the synthesis chamber continuously.
  • streamers form and are elongated by the upward flow of boron vapor.
  • the flapping motion occurs as the fibers/fibrils follow the streamlines of the turbulent boron vapor flow.
  • the boron vapor is created by laser heating at the bottom of the indentation.
  • Streamers form quickly, reaching over a centimeter in length within about l/30 th of a second. Sections of streamers snap off and swirl above the target before being carried from the chamber by the apparatus described hereinafter. Elevated chamber nitrogen pressure is critical to the formation of streamers.
  • Streamers are collected from both the target face and downstream on collector surfaces (described below). When held by its ends, a streamer feels like a piece of spider silk, and is similar thereto in appearance, medium matte grey in color. It can be plucked like a guitar string to two or three times its length and then returns to its original shape.
  • boron nitride nanotubes do not require a chemically catalytic surface for nucleation. They will simply form spontaneously and continuously by root growth on any suitable surface, e.g., an asperity in a zone where hot boron vapor and cold nitrogen gas mix to the correct stoichiometry. Under the elevated pressure employed, the growth rate is centimeters (preferably at least 10) per second in a localized fiber/fibril.
  • BNNT production is fundamentally less complicated than carbon nanotube (CNT) production where a gas-borne cloud or coated surface of catalytic particles must be produced and kept active during the growth process.
  • CNT carbon nanotube
  • the laser is only one means of heating powdered boron metal to create boron vapor.
  • the heating zone and BNNT formation zone are physically separated.
  • the laser- boring mechanism that forms the depressions in this implementation may be unique to the FEL beam properties, the technique is applicable with other lasers and other sources of heat given an appropriate geometry.
  • substantial engineering obstacles as the boiling point of boron, for example, at 12 bar is high (3250 C). This temperature is readily accessible to laser and arc heating.
  • Other heating methods that can achieve the appropriate temperatures and generate the flow of boron vapor from the depression should be equally effective.
  • the method of the present invention entails vaporizing boron under high pressure and impinging the resultant buoyant plume of gaseous boron on a condenser, initiating the formation of BNNTs.
  • the technique is fast and scalable, seemingly dependent only on the rate at which boron can be vaporized in the chamber.
  • Previous work reviewed the limited success of BNNT synthesis techniques available to date, i.e. those using: arc discharge, laser vaporization, chemical vapor deposition, chemical reaction, and atomic deposition.
  • the current technique is most closely related to 'laser vaporization' but introduces the use of forced condensation (a new growth mechanism) and operates in an unexplored range of pressure.
  • Our technique uses laser heating to create boron vapor, but the method is not a 'laser' method per se.
  • the type of heating source in this case a laser, is not critical.
  • the growth zone is physically isolated from the heating zone, near or on a separate condenser surface.
  • the technique works equally well with the two heat sources currently available to us, a near-infrared free electron laser and a far infrared commercial metal- cutting laser.
  • a high power laser is used to boil boron in a high pressure nitrogen environment within a chamber as described more fully below.
  • the high ambient pressure produces a large density ratio between the boron vapor plume and the nitrogen and thus a strong buoyancy force that accelerates the boron vapor vertically towards the ceiling of chamber.
  • the growth of the fibrils initiates when the boron vapor plume crosses the condenser and rapidly proceeds towards the ceiling of the chamber.
  • Flow visualization indicates that 10 cm of growth often occurs within a single video frame, less than 33 milliseconds, indicating a growth rate equal to or greater than 3 meters per second. Fibrils on the order of ⁇ 1 mm in diameter have been observed under these fabricating conditions.
  • Such fibrils comprise a bunch or collection of parallel oriented BNNTs distinct vertical strands which extend the full height of the image indicating that the material has an alignment axis parallel to the growth direction.
  • the material can be stretched elastically like a cobweb. Transverse to the growth axis, the material can easily be separated into individual strands with the fingers.
  • the structure is a network of long, branching nanotubes and tube bundles, often linked at nodes. SEM showed that the nodes were primarily nano-droplets of boron, coated with layers of boron nitride.
  • a yarn can be spun from a mass of raw BNNT fibrils grown as described herein. Such a yarn is fabricated from a collected mass of fibrils as shown/depicted in Figure 2. This mass of about 60 mg, with the appearance and texture of a soft elongated cotton ball, is the raw product of a 30 minute production run. A group of fibrils weighing about 10 mg (representing 5 minutes of synthesis time)was separated from the mass, drawn in the growth direction, i.e. lengthwise, and finger-twisted to form a simple one-ply yarn (see Figure 3) with a twist angle of about 45 degrees.
  • the yarn in Figure 3 had a relatively large diameter of about 1 mm, was loosely packed, and was spun dry from unwashed raw material — all unfavorable conditions for mechanical strength. This implies that the underlying staple fibers (BNNT bundles/fibrils) are relatively long to counteract these disadvantages and that considerable improvement in strength can be expected with more refined spinning processes.
  • an apparatus 10 useful in the production of BNNT fibrils in accordance with the present invention comprises: a pressure chamber 12 containing; a continuously fed or rotated boron nitride target 14; a source of thermal energy preferably a focused laser beam 16; a rotating cooled condenser ring 18; a source of pressurized nitrogen gas 20; and a mechanism 22 for extracting boron nitride nanotubes from pressure chamber 12 after boron nitride vaporized by the thermal energy source forms a boron nitride plume 24 that condenses on or in the vicinity of rotating cooled condenser ring 18.
  • thermal energy source 16 is preferably a laser beam introduced into pressure chamber 12 via a convex lens 26 that allows for focusing of laser beam/thermal energy source 16 within pressure chamber 12.
  • cooled condenser ring 18 is rotated continuously by virtue of its being mounted on a rotating shaft 28 such that a new surface thereof is constantly being brought into the proximity of mechanism 22, in the embodiment shown in Figure 1, a condenser tube 22.
  • boron nitride target 14 is a commercially available hot pressed hexagonal boron nitride rod 14 that is continuously fed into the field of laser beam 16 by a motor driven plunger rod, rotator or similar device 30.
  • boron nitride target 14 is of square cross-section about 0.050" on a side and is introduced into laser beam 16 not at the focal waist of laser beam 16 but rather at a position where laser beam 16 is of approximately the same size as boron nitride target rod 14.
  • target rod 14 is advanced at a rate of about 1 mm/sec into the beam 16 of a 2 kW CO 2 laser having a wavelength of about 10.6 microns and a diameter of about 12 mm.
  • a small flow of nitrogen gas is of about 40 SCFH is maintained into pressure chamber 12 via nitrogen feed 20 whose flow is regulated, for example, by a needle valve 32 in the chamber exhaust 34.
  • laser beam 16 terminates in a copper block 38 cooled by water provided thereto by inlet and outlet 38 and 40. Copper block 38 is designed to absorb the full, continuous power of laser beam 16 without damage.
  • rotating condenser 18 is water cooled by conventional means well within the skills of the skilled artisan to maintain it a temperature of about 20° C. According to the preferred embodiment depicted in Figure 1, rotating condenser 18 is a hoop of about 0.025" copper attached to a water cooled rotating copper shaft 28 although other materials such as stainless steel, tungsten, niobium, hot pressed boron nitride , boron powder, boron castings etc. are similarly useful.
  • the boron nitride nanotube fibrils are removed from rotating condenser 18 by means of a collection tube 22 which leads to the outside of pressure chamber 12.
  • a ball valve (not shown) in collection tube 22 is opened, the boron nitride nanotube fibrils are "vacuumed” from rotating condenser ring 18 by the nitrogen gas exhausting to 1 atmosphere.
  • Boron nitride nanotube fibrils can be collected, for example, in a wire mesh filter installed in-line in collection tube 22 (not shown) or simply spun into yarn as they exit collection tube 22.
  • Nd:YAG, or free electron lasers are 2 examples; the shape of condenser 18 can take many variations as long as it provides for free flow of the vapor plume it will work and Nb wire, W wire, Nb sheetstock, and Cu sheetstock have all proven useful; both mechanical and suction have been shown as useful to collect boron nitride nanotubes. Since the material tends to stick to itself or to a surface, it can be wrapped around, stuck to, or sucked into any number of geometries and since boron nitride nanotubes also responds well to static charging they can be collected by this mechanism as well.
  • the cooled condenser has been depicted as a cooled ring, it could equally as well comprise a cooled oscillating structure and the mechanism for collecting boron nitride nanotubes could comprise one or more collection tubes in the vicinity of the extremes of oscillation of the cooled oscillating condenser.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Structural Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

L'invention concerne un procédé et un appareil permettant de produire des nanotubes de nitrure de bore longs et à rapport de forme élevé et des fibrilles de nanotubes de nitrure de bore composées de nanotubes de nitrure de bore à paroi simple ou à quelques parois alignés en faisceaux de nanotubes d'au moins 20 μm à une vitesse de plus de 1 mètre par seconde environ. L'invention concerne enfin des fils de nanotubes comprenant des faisceaux torsadés de telles fibrilles de nanotubes
EP09839785.4A 2009-02-04 2009-05-08 Fibrilles et fils de nanotubes de nitrure de bore Withdrawn EP2393966A4 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US12/322,591 US8753578B1 (en) 2009-02-04 2009-02-04 Apparatus for the production of boron nitride nanotubes
US12/387,703 US20100192535A1 (en) 2009-02-04 2009-05-06 Boron nitride nanotube fibrils and yarns
PCT/US2009/002861 WO2010090624A1 (fr) 2009-02-04 2009-05-08 Fibrilles et fils de nanotubes de nitrure de bore

Publications (2)

Publication Number Publication Date
EP2393966A1 true EP2393966A1 (fr) 2011-12-14
EP2393966A4 EP2393966A4 (fr) 2018-04-18

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Family Applications (1)

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EP09839785.4A Withdrawn EP2393966A4 (fr) 2009-02-04 2009-05-08 Fibrilles et fils de nanotubes de nitrure de bore

Country Status (6)

Country Link
US (1) US20100192535A1 (fr)
EP (1) EP2393966A4 (fr)
JP (1) JP2012516827A (fr)
KR (1) KR20110113201A (fr)
CA (1) CA2750847A1 (fr)
WO (1) WO2010090624A1 (fr)

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WO2018236312A2 (fr) 2016-12-30 2018-12-27 Sabanci Üniversitesi Procédé de production de structures de bn de haute cristallinité et de haute pureté à des températures modérées

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US10068968B2 (en) 2011-01-04 2018-09-04 Jefferson Science Associates, Llc BxCyNz nanotube formation via the pressurized vapor/condenser method
US8673120B2 (en) 2011-01-04 2014-03-18 Jefferson Science Associates, Llc Efficient boron nitride nanotube formation via combined laser-gas flow levitation
US20130144576A1 (en) * 2011-11-10 2013-06-06 U.S.A. as represented by the Administrator of the National Aeronautics and Space Admimistration Modeling of Laser Ablation and Plume Chemistry in a Boron Nitride Nanotube Production Rig
US10047015B2 (en) * 2012-01-20 2018-08-14 Free Form Fibers, Llc High strength ceramic fibers and methods of fabrication
US9463433B2 (en) * 2013-06-24 2016-10-11 Jefferson Science Associates, Llc Nano-materials for adhesive-free adsorbers for bakable extreme high vacuum cryopump surfaces
US10458049B2 (en) * 2013-07-30 2019-10-29 University Of New Hampshire Continuous boron nitride nanotube yarns and methods of production
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CA2750847A1 (fr) 2010-08-12

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