WO2004035463A2 - Production continue et separation de materiaux en carbone - Google Patents

Production continue et separation de materiaux en carbone Download PDF

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Publication number
WO2004035463A2
WO2004035463A2 PCT/US2003/032535 US0332535W WO2004035463A2 WO 2004035463 A2 WO2004035463 A2 WO 2004035463A2 US 0332535 W US0332535 W US 0332535W WO 2004035463 A2 WO2004035463 A2 WO 2004035463A2
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chamber
section
electrode
effective cross
carbon compounds
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PCT/US2003/032535
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WO2004035463A3 (fr
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Dal-Yung Jung
Kook-Hyang Lee
Doo-Young Jung
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Dal-Yung Jung
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Priority to AU2003282823A priority Critical patent/AU2003282823A1/en
Publication of WO2004035463A2 publication Critical patent/WO2004035463A2/fr
Publication of WO2004035463A3 publication Critical patent/WO2004035463A3/fr

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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
    • 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
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • 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
    • C01B32/152—Fullerenes
    • C01B32/154—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
    • 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
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0809—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0816—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes involving moving electrodes
    • B01J2219/0818—Rotating electrodes
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0822—The electrode being consumed
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0824—Details relating to the shape of the electrodes
    • B01J2219/0826—Details relating to the shape of the electrodes essentially linear
    • B01J2219/083—Details relating to the shape of the electrodes essentially linear cylindrical
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0837—Details relating to the material of the electrodes
    • B01J2219/0839—Carbon
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0869—Feeding or evacuating 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0871—Heating or cooling of 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894—Processes carried out in the presence of a plasma
    • B01J2219/0898—Hot plasma

Definitions

  • the present invention relates to an apparatus and a process for optimized annealing during graphite vaporization wherein exposure to intense ultraviolet radiation is minimized.
  • the invention provides mass production methods for fuUerenes, endohedral metallofuUerenes (EMFs) and other carbon-based materials through effective shielding from destructive UV radiation during graphite vaporization. This provides for slower cooling of the annealed carbon compounds and increased yields of up to 10 times or even better over conventional production techniques.
  • FuUerenes can also be doped to form electronic materials or reacted to form superconductors. All of these applications have been discovered since the first macroscopic amounts of the most common two fuUerenes, C 6 o and C o, were isolated in 1990 [Kratschmer, et al., Nature 347, 354 (1990)]. Much of the work on fuUerenes is performed using small amounts of material, as synthetic production of these forms of carbon yielded limited quantities of material. The major drawback to the commercialization of some of the applications mentioned has been the lack of a large-scaled method for producing and isolating fuUerenes.
  • a more useful method of synthesizing fullerene-containing soot is the electric-arc method [Kratschmer, et al., Nature 347, 354 (1990)].
  • this method known as the contact arc process
  • lightly contacting graphite electrodes are heated electrically by an electric-arc welder in an atmosphere of helium at a pressure of about 50 to about 300 torr.
  • the porous graphite electrodes are vaporized by the arc welder to produce soot containing fuUerenes.
  • the soot condenses upon cool walls of a chamber, and is scraped off after the electrodes are consumed.
  • FuUerenes are then extracted from the soot by a solvent, such as toluene, carbon disulfite, toluene, or benzene.
  • a solvent such as toluene, carbon disulfite, toluene, or benzene.
  • This method is capable of producing a few tens of milligrams of fuUerenes per run.
  • the process is capable of producing several grams of fuUerenes per day.
  • the process is encumbered, however, with scaling problems. For example, as the diameter of the rods gets bigger and the current supplied to the rods gets higher to increase the amount of graphite evaporated per unit of time, the yield of fuUerenes decreases.
  • the invention provides an apparatus and method for producing fuUerenes, EMFs, carbon nanotubes, and other carbon materials in quantities greater than the few hundred milligrams produced per day by the conventional techniques such as contact-arc, laser ablation, and solar radiation vaporization.
  • the invention provides a scalable method for continuously producing fuUerenes in greater quantities than the small amounts available through current methods, without losing efficiency in production from increases in the electrode diameters.
  • the invention provides an apparatus and method for effectively transferring fuUerenes, EMFs, carbon nanotubes, and other carbon materials from the destructive vaporization zone using the constant flow of buffer gas.
  • the invention provides a method or producing increased amounts of fuUerenes, EMFs and other carbonaceous compounds using longer annealing times by using a graphite guide tube, which can be heated by an arc plasma.
  • the invention provides an apparatus and method for producing increased amounts of fuUerenes, EMFs and other carbonaceous compounds under more optimal conditions for delivering metal precursors.
  • the invention provides an apparatus and method for producing increased amounts of fuUerenes, EMFs and other carbonaceous compounds by decreasing the exposure from destructive high energy radiation during vaporization by using a graphite guide tube and a rotary shielding block.
  • FIG. 1 shows a prior art apparatus with A) bisectional view of the conventional contact-arc reactor in prior art, and the different arrangement of the contact-arc electrodes, B) 180 degree angle between the rotary and linear motion graphite electrodes, and C) 90 degree angle between rotary and linear motion graphite electrodes.
  • FIG. 2 shows a block diagram of the present invention.
  • FIG. 3 shows a bisectional view of the apparatus with the graphite shielding tube of the present invention.
  • FIG. 4 shows A) the detail of the bottom side, B) the connection mode of the separated collector with a sublimator, and C) a sublimation process in a tube furnace.
  • FIG. 5 shows A) a Schlenk line collector and B) anaerobic manipulation by using the cannular technique .
  • FIG. 6 shows a bisectional view of the apparatus with a heat reserving guide tube and a rotary graphite shielding block.
  • FIG. 7 shows A) a the bisectional view of the modified apparatus of FIG. 6 of which both electrodes are tilted 30 degrees from horizon and B) the position of two electrodes, which are perpendicular each other, which are perpendicular each other, from top view.
  • FIG. 8 shows another block diagram of the present invention.
  • FIG. 9 shows a bisectional view of the apparatus with laser and solar radiation sources.
  • FuUerenes requires a source of small, gas phase carbon clusters of from 2 to 10 atoms.
  • One is the disproportionation reaction in flame of hydrocarbons or CO in an oxygen deficient flame to produce carbon soot. While the percentage of fuUerenes in the soot may seem relatively high, the yield of fuUerenes compared to the mass of hydrocarbon consumed is low.
  • the other source is the vaporization of graphite at temperatures above 3000 degree C, whereupon the vaporized carbon is then condensed into carbon soot. While this arc method has proven to be the most useful, even this method yields only tenths of grams of fuUerenes per hour. None of the existing methods of production are capable of being adapted for large-scale production.
  • the present invention provides an apparatus and a process for optimized annealing during graphite vaporization wherein heat from plasma carbon is directed into a limited area to provide a slower cooling process.
  • the invention uses a shielding block and narrowed gas flow channels to rapidly move vaporized carbon from the area of intense destructive radiation to a shielded condensation area.
  • the geometric arrangement of the shielding block can further reduce the exposure on products to destructive high-energy UV radiation during vaporization. Under these conditions, yields are dramatically increased and the apparatus can be scaled-up for mass production.
  • FIG. 1 shows a conventional electric-arc reactor that is well-known in art.
  • Rotary graphite electrodes (RGE) 20 and linear-feeding porous graphite electrode (LFE) 30 are arranged for arc contact in a stainless steel, water-cooled, double- wall (SWD) chamber 10.
  • FIG. 2 shows the block diagram of an electric-arc reactor of the present invention.
  • the collector section can be separated without disturbing the main system and allows continuous collections and anaerobic manipulation of the resultant product soot.
  • FIG. 3 shows another embodiment of the present invention.
  • the main chamber 10 is the SWC jacket, which has two O-rings or cupper gasket sealed flanges (OSFs or CGFs) attached at both ends or a quartz tube with SWD installed OSF on both ends.
  • constant inert gas typically helium, nitrogen, argon
  • MFC mass flow controller
  • electric current is applied to both electrodes (20 and 30), which are electrically insulated, while the constant inert gas flows though inlet valve 35.
  • Final product will be transferred into the quartz collector 90 by opening the stopper 75 and wide-mouth, straight-through, metal or o-ring sealed valves, 80 and 82. After collecting all the carbon soot from the chamber, the stopper 75 is closed and several inert gas pulses are directed into the chamber to collect soot from the wall. The stopper 75 is then opened to collect the rest of the carbon soot. This process can be repeated several times.
  • FIG. 4 shows the bottom part of the apparatus, which can produce carbon- based material in continuous mode.
  • an attached stopcock with schlenk connector 92 provides anaerobic manipulation.
  • the Schlenk line is used while valves 80 and 82 are kept closed to keep pressure in the chamber and collector.
  • valve 82 is closed, the collector 90 can be detached for removal of the carbon materials.
  • An additional flange covers the bottom of the middle chamber 70, and the valve 85 opens to the vacuum to evacuate all the air from the connection.
  • an additional sublimator can be attached on top of the valve 82, and then valve 95 is opened to evacuate all the buffer gas from the sublimator. This cycle of purging and opening is then repeated.
  • the sublimation system can be set up into a tube furnace, and then the valve 82 is opened carefully.
  • the sublimator 97 inserts into the collector, running the cooling water in rod 93, as a heat exchange system, and then the system is purged until the pressure goes down to 10-3 torr by using a secondary diffusion or other high performance vacuum pump.
  • the fraction collected in a certain temperature range gives specific fullerene molecules, as is well known in art. Repeated sublimations provide initial purification of fuUerenes and EMFs. Before detaching sublimator with valve 82, if necessary, additional solvent extraction can be done in anaerobic conditions, as shown in FIG. 5.
  • FIG. 5 shows anaerobic manipulations by using Schlenk Techniques.
  • the resultant soot can be transferred to other glassware by using a common Schlenk technique, such as the cannular method. Then solvent extraction can be performed for further separations.
  • the resultant soot can be transferred without detaching collector 90 by using the Schlenk Technique.
  • FIG.6 shows another embodiment of the present invention.
  • the main chamber 10 will be the SWD jacket or quartz tube, as in FIG. 3.
  • the vaporization area surrounded by a main guide tube (MGT) 100 and a rotary shielding block (RSB) 120 can reserve the heat from plasma and escape the resultant product from the plasma area to minimize exposure high energy UN radiation.
  • MTT main guide tube
  • RTB rotary shielding block
  • the guide graphite tube 100 will be fixed by using a water-cooled feed through valve 102.
  • Inert gas flow rate through inlet valve 35 can be adjusted by using a MFC.
  • Zirconia tube 33, or other high temperature resistant material can be used or guide tube 60 can be directly attached on the wall in main chamber 10.
  • the quartz tube chamber does not need electric insulation, but it needs an additional air-cooling system around the chamber.
  • the cartridge 36 can load several porous graphite rods. After consuming the feeding electrode, a new porous graphite rod in 36 can be easily replaced without any difficulty.
  • the cartridge 36 can be employed and modified in the bullet loading system from the conventional automatic weapon and others easily available in art.
  • the RSB 120 can be rotated in various speeds with rotary feed-through and an additional scrapper directly attached on RSB 120, if necessary. Rotation of the shield block creates a suction effect, thereby drawing the vaporized carbon particles downstream.
  • Middle chamber 70 is a SWD jacket with a stopper 75 used for accumulating vaporized soot. The collection process is the same as described in connection with the description of FIG. 3.
  • FIG.7 shows another variation of the apparatus of the present invention.
  • product yields vary according to the position of the electrodes. This figure show only one position of the electrodes.
  • the flow of inert gas gives the effective escape of the resultant carbon soot by following the Bernoulli Theorem.
  • the rotation speed of the shielding block 120 is an additional factor in reducing the exposure of the product to UV radiation.
  • FIG.8 shows a block diagram of the apparatus using laser or solar vaporization techniques.
  • the vaporization energy source can be attached to the top of the reactor with the stream of the inert gas flow.
  • preheating the graphite element can raise the temperature up to 2000 degree C, and gives smoother vaporization and better yields.
  • FIG. 9 shows one type of the apparatus of the present invention developed from FIG. 8.
  • Vaporization sources such as a laser or a solar radiation collector system
  • the position of the focal point can be adjusted by using a reflecting system or by changing the lens positions.
  • optional preheating system 152 can be used for smoother vaporization.
  • Heating system 152 is made of a graphite heating element found in commercial vacuum furnaces, which can heat up to 2000 degree C.
  • the heat distributions inside the main chamber can be monitored as mentioned in FIG. 3.
  • the rotation speed of RSB 120 can be affected the efficiency of the production.
  • Carbon source materials for producing fuUerenes can be selected from among graphite, graphite powder, glassy carbon and amorphous carbon; however, graphite is preferred.
  • a porous graphite rod is also preferred because it has more surface area, including a hemispherical cavity in its top surface. Also, it provides greater amounts of soot containing higher amounts of fuUerenes. Moreover, it can be handled very easily. Furthermore, the impregnation of the metal precursor in a porous graphite rod to prepare EMFs is well-known in the art.
  • increased yields from the present invention are accomplished by effective shielding and by directing heat from plasma carbon into a limited area of the reactor during vaporization, and by quickly transporting vaporized graphite in flowing inert gas to keep the resultant product away from the destructive UV radiation area.
  • Fullerene production yields are also affected by the: a) length and diameter of the both end on main guide tube (MGT), b) diameter of the both electrodes, c) number of vaporized electrodes, d) flow rate of inert gas, e) mixed ratio of inert gas, f) interval of the vaporization process, g) rotation speed of the shielding block (in FIG. 6 and 9), h) geometry of the electrodes and number of electrodes (FIG. 6), i) mixed ratio of inert gas, if necessary, (He, N 2 , Ar, and others) j) preheating temperature for inert gas, and k) energy source on vaporization.
  • EMFs can be produced by the vaporization of metal compound impregnated porous graphite rods and other metal containing carbon sources.
  • Various metal impregnation processes on porous graphite rod are readily available from the prior art.
  • the soaking method [Cagle et al, JACS, 118, 8043 (1996)] has been developed, and the content of the metal precursor on the graphite rod can be controlled by the concentration of the metal compound solution.
  • Metal impregnated graphite rods can be purchased from Toyo Tanso, Co, in Japan. [Shinohara, et al, Bioconjugate Chem., 12, 510 (2001)]
  • Table 1 shows some EMFs obtained from the present invention.
  • TNT trimetallic nitride template

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Abstract

Cette invention concerne plusieurs appareils et procédés de production continue d'une suie présentant une teneur élevée en fullerènes, métallofullerènes endohédraux (EMF), et de nanotubes de carbone. L'invention concerne également des manipulations anaérobies de composés à base de carbone. Les appareils et procédés de l'invention fournissent des conditions optimales dans des traitements de recuit. En particulier, le bloc de protection rotatif de l'invention peut effectivement empêcher l'exposition de produits résultants à un rayonnement ultraviolet intense associé à des processus de vaporisation.
PCT/US2003/032535 2002-10-16 2003-10-15 Production continue et separation de materiaux en carbone WO2004035463A2 (fr)

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US60/418,964 2002-10-16
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US10/684,626 US20040124093A1 (en) 2002-10-16 2003-10-14 Continuous production and separation of carbon-based materials

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010100492A3 (fr) * 2009-03-03 2011-03-31 Isis Innovation Limited Procédés et appareil destinés à la production de substances contenant du carbone
EP2969941A4 (fr) * 2013-03-15 2016-04-06 Luna Innovations Inc Procédés et dispositifs pour la synthèse de métallofullerènes
EP3050617A4 (fr) * 2013-11-12 2017-08-30 Xiamen Funano New Material Technology Company.ltd Source d'arc à fullerène et appareil d'obtention de fullerène comprenant la source d'arc

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102047370B1 (ko) * 2016-07-14 2019-11-22 주식회사 엘지화학 카본나노튜브 제품 건조 및 회수 장치 및 이를 이용한 카본나노튜브 제조방법
CN112978712A (zh) * 2019-12-13 2021-06-18 北京三弧创科技术有限公司 利用等离子体炬制备富勒烯的方法

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