WO2011034408A2 - Procédé de préparation d'un liquide de dispersion de nanocarbone, liquide de dispersion de nanocarbone préparé selon ce procédé, procédé d'évaluation de nanocarbones, procédé de production de matériaux en nanocarbone et procédé de production de matières solides en nanocarbone - Google Patents

Procédé de préparation d'un liquide de dispersion de nanocarbone, liquide de dispersion de nanocarbone préparé selon ce procédé, procédé d'évaluation de nanocarbones, procédé de production de matériaux en nanocarbone et procédé de production de matières solides en nanocarbone Download PDF

Info

Publication number
WO2011034408A2
WO2011034408A2 PCT/KR2010/006521 KR2010006521W WO2011034408A2 WO 2011034408 A2 WO2011034408 A2 WO 2011034408A2 KR 2010006521 W KR2010006521 W KR 2010006521W WO 2011034408 A2 WO2011034408 A2 WO 2011034408A2
Authority
WO
WIPO (PCT)
Prior art keywords
nanocarbon
dispersion
carbon
nano
weight
Prior art date
Application number
PCT/KR2010/006521
Other languages
English (en)
Korean (ko)
Other versions
WO2011034408A3 (fr
Inventor
김상옥
Original Assignee
(주)월드튜브
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
Priority claimed from KR1020090088968A external-priority patent/KR101136776B1/ko
Priority claimed from KR1020090122319A external-priority patent/KR101218366B1/ko
Application filed by (주)월드튜브 filed Critical (주)월드튜브
Publication of WO2011034408A2 publication Critical patent/WO2011034408A2/fr
Publication of WO2011034408A3 publication Critical patent/WO2011034408A3/fr

Links

Images

Classifications

    • 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
    • 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
    • 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

Definitions

  • the present invention relates to nanocarbon, and more particularly, to a nanocarbon dispersion, a method for preparing a nanocarbon dispersion, a method for evaluating nanocarbon using the same, and a method for preparing a nanocarbon material using the same, to prepare a nanocarbon solid using the same. It is about a method.
  • nanocarbon is used as a meaning including carbon nanotubes, carbon nanohorns, carbon nanofibers, carbon nanorods, carbon nanoropes, graphane, etc., which are made of a single layer of SWNT and 2-several layers of MWNT.
  • Nano carbon has attracted much attention because of its higher conductivity, strength, and specific surface area than other carbon allotropees, and many researches and products have been tried.
  • advanced dispersing technology should be advanced, but dispersion through mechanical method, dispersion using solvent and dispersant, dispersion using strong acid, dispersion by surface functionalization, polymer using Dispersion methods, such as dispersion, require high cost to disperse, pollute the environment, and are difficult to apply to products in earnest because a high concentration of the dispersion cannot be prepared.
  • the present invention is to solve the above-mentioned problems, low cost, environmentally friendly, high-carbon nano-carbon dispersions that can be produced freely to a high concentration of nano-carbon dispersions and nanocarbon dispersions and nanocarbon solids using the same To provide.
  • the present invention provides a method for evaluating nanocarbon using the method for preparing a nanocarbon dispersion and a method for preparing a nanocarbon material using the nanocarbon dispersion.
  • the present invention provides a method for preparing a nanocarbon solid using a nanocarbon dispersion, a nanocarbon solid using the same, and a nanocarbon dispersion in which the nanocarbon solid is dispersed again.
  • the present invention provides a method for evaluating nanocarbon using the above-described nanocarbon solids and a method for producing the same, and a method for producing a nanocarbon material using a nanocarbon dispersion.
  • a nanocarbon cutting step of cutting the associated nanocarbon bundle in the provided nanocarbon to an average particle size of 0.1 ⁇ m to 5 ⁇ m;
  • nanocarbon dispersion comprising the nanocarbon dispersion step of dispersing the nanocarbon with a disperser by mixing the cut nanocarbon, 0.01 to 200 parts by weight of a dispersant with respect to 100 parts by weight of the nanocarbon, and a solvent. do.
  • the cutting in the nanocarbon cutting step may be made by a wet method.
  • the wet method may use at least one device selected from the group consisting of an ultrasonic grinder, wheat grinder, fluidizer, and nanomizer.
  • the wet method may further comprise 0.01 to 50 parts by weight based on 100 parts by weight of the nanocarbon dispersing agent in the nanocarbon cutting step.
  • the cutting in the nanocarbon cutting step may be made by a dry method.
  • the method may further include passing the nanocarbon cut by the dry method through a mesh filter.
  • the mesh filter is preferably used 200 to 500mesh.
  • the dry method may use one apparatus selected from the group consisting of a cutter, a ball mill, a jet mill, and an atrium mill.
  • the dispersing agent is a dry method, surfactants, coupling agents, block copolymers, monomers, oligomers, vinyls, lactics, caprolactones, silicones, waxes, silanes, fluorine, ethers, It may be composed of at least one dispersant selected from the group consisting of alcohols, esters and mixtures thereof.
  • the solvent is composed of at least one solvent selected from the group consisting of water, alcohol, cellulsolve, ketone, amide, ester, ether, aromatic, hydrocarbon, and mixtures thereof. Can be.
  • nanocarbon dispersion prepared according to the method for producing a nanocarbon dispersion described above.
  • the nanocarbon contained in the nanocarbon dispersion may exceed 2% by weight.
  • the dispersant is preferably included in 0.01 to 200 parts by weight based on 100 parts by weight of nanocarbon.
  • Another aspect of the present invention is an evaluation method of nanocarbon using the above-described nanocarbon dispersion,
  • Presenting a method for evaluating nanocarbon using a nanocarbon dispersion comprising a measurement step of measuring at least one characteristic selected from the group consisting of electrical conductivity, transmittance, scratch resistance, and surface hardness for the film coated with nanocarbon. do.
  • the water-soluble urethane is preferably included in 50 to 1000 parts by weight based on 100 parts by weight of the nanocarbon.
  • Another aspect of the invention is a method for producing a material of nano carbon using the above-described nano carbon dispersion
  • It provides a method for producing a material of nano-carbon using a nano-carbon dispersion to produce a nano-carbon material by mixing the nano-carbon contained in the nano-carbon dispersion with a general material.
  • the nanocarbon material is a compound, a masterbatch, a transparent electrode, a coating agent for ESD / EMI, an ink, a paint, a high conductive paint, a high heat-resistant paint, a very high strength sintered fiber, an electron emitting emitter, Backlights for adhesives, adhesives, tapes, secondary battery active materials and electrodes, solar cell electrodes, battery active materials and electrodes, fuel cell separators, heating elements, radiators, car, aircraft, motorcycle, tank and ship brake systems; Industrial] abrasives, smart cement, glass, foams, prepregs, nanofluids, biomaterials, extruded products, injection molded products, blow molded articles, and compression molded articles.
  • the compound or the master batch may be prepared by mixing while the siding liquid feeding the nanocarbon dispersion at 1-50% by weight during the extrusion of the matrix resin.
  • the nanocarbon dispersion may be used as the transparent electrode, the coating agent for ESD / EMI, the ink, the paint, the adhesive agent, the tape, the secondary battery active material and the electrode, the solar cell electrode, the battery active material and the electrode, the nanofluid, and the RFID. It can be diluted and mixed.
  • the coating agent for UV is prepared by mixing the UV oligomer to alcohol or MEK type in the nano-carbon dispersion.
  • the high conductivity, high heat dissipating paint and adhesive-adhesive may be prepared by mixing the nanocarbon dispersion with high conductivity or high heat dissipating material and binder resin, respectively, and then stirring or dispersing with a stirrer or disperser, and the tape is electrically conductive and insulated. After applying the adhesive, the release paper is attached and then coated on the opposite side to meet the conductive and insulating purpose.
  • the active materials and electrodes of secondary batteries and accumulators are manufactured by mixing nanocarbon dispersions and solid bodies to obtain high energy density and high output density. .
  • the electrode attaches nanocarbon dispersion or nanocarbon solids of FTO-coated glass substrate or transparent electrode film to 0.02-1 ⁇ m, attaches nano filler (titanium dioxide), and dyes on the other side.
  • nano filler titanium dioxide
  • a fuel cell is an electrolyte, an electrode material, a separator, and the most important component, and a separator is manufactured by adding a filler to a nanocarbon dispersion and a solid to a resin having a smaller amount of binding force and physical properties.
  • the heating element, the radiator, the abrasive, and the smart cement are prepared by adding a nano carbon dispersion or solid to the substrate (metal, ceramic, diamond, cement, resin, filler).
  • Nanofluids are made by heating or cooling nanocarbon dispersions in boilers or heat exchangers.
  • Prepreg is a high-strength structural material such as aircraft fuselage, ships, and sporting goods, but it is a material that can be made lighter, which was impossible due to the carbon fiber's properties.
  • the ultra high-strength ⁇ ⁇ ball ⁇ high conductivity fibers may be prepared by spinning the nanocarbon liquid dispersion with a liquid resin or solid resin for the fiber or while side-feeding.
  • the electron emission emitter or the backlight for the electronic product may be prepared by mixing a nanocarbon liquid dispersion with an electrode, an electron emission source, or an inorganic filler.
  • the extruded article, the injection molded article, the blow molded article, or the extruded molded article may be prepared by mixing 3 to 50% by weight of the nanocarbon dispersion liquid 1 to 50% while siding liquid feeding.
  • a nanocarbon cutting step of cutting the associated nanocarbon bundle in the provided nanocarbon to an average particle size of 0.1 ⁇ m to 5 ⁇ m;
  • a nanocarbon dispersion step of dispersing the nanocarbon with a disperser by mixing the cut nanocarbon with 0.01 to 300 parts by weight of a dispersant and a solvent with respect to 100 parts by weight of the nanocarbon;
  • nanocarbon solidification step of preparing a solid by drying the nanocarbon powder in a predetermined shape and then dried.
  • the dispersant may be a surfactant, a coupling agent, a block copolymer, a monomer, an oligomer, a vinyl, a lactic, a caprolactone, a silicone, a wax, a silane, a fluorine, an ether, an alcohol, an ester And at least one or more dispersants selected from the group consisting of compounds and mixtures thereof.
  • the solvent is one solvent or cosolvent selected from the group consisting of water, alcohol, cellulsolve, ketone, amide, ester, ether, aromatic, hydrocarbon, and mixtures thereof. It is preferred to include other solvents.
  • the flocculant is composed of chitosan, mineral additives, polymer electrolytes, polyacrylamide-based synthetic polymers, metal salts, inorganic polymers, counter charge dispersant of the dispersant used, natural organic streams, organic solvents, and mixtures thereof. It is preferable that it is composed of one selected from the group consisting of.
  • Nanocarbon solids according to another aspect of the present invention is prepared by the method for producing the nanocarbon solids described above.
  • the apparent density of the nanocarbon solids is preferably 0.1 to 0.5g / cc.
  • the nanocarbon solids were 3mm to 9mm in diameter, and the ratio of diameter to height was 1: 2, and the compressive strength measured according to the room temperature compressive strength test method (KS-L1601 method) of monolithic ceramics was 0.1 to 3 MPa. It is preferable.
  • Nanocarbon material according to another aspect of the present invention is preferably to use the above-described nanocarbon solids.
  • the nanocarbon material is a compound, a masterbatch, a transparent electrode, a coating agent for ESD / EMI, an ink, a paint, a fiber, an emitter for an electronic product, a backlight, a contact-adhesive, a tape, a secondary battery active material and an electrode, a solar cell electrode , Battery active materials and electrodes, fuel cell separators, heating elements, heat sinks, abrasives [for cars, aircraft, ships, tanks, motorcycles and industrial materials], smart cement, glass, foams, prepregs, nano fluids, bio materials, RFID , Extrudates, reinforcements, waste water and waste air purifiers, injection, blow molded, compressed molded article may be one selected from the group consisting of.
  • Another aspect of the present invention is a method of manufacturing a nanocarbon material using a nanocarbon solid
  • the nanocarbon solids may be made while feeding the sider feeder and the hopper during extrusion of the matrix resin.
  • nanocarbon solids are preferably prepared by dispersing them in a solvent or a liquid resin.
  • the nanocarbon dispersion preferably contains 50 to 999900 parts by weight of solvent or 50 to 9900 parts by weight of resin based on 100 parts by weight of the nanocarbon solid.
  • Still another aspect of the present invention is a method of manufacturing a molded article by extrusion, injection, compression, blue, rotational molding, etc. by feeding the above-described nanocarbon dispersion and solid body together with a liquid resin or a solid resin.
  • a metal, a heat dissipating material, and a resin are added to the nanocarbon dispersion and the solid to produce any one of a paint, an adhesive, an adhesive, and a tape.
  • nanocarbon in order to increase the content of the nanocarbon may further comprise a heat treatment step before or after the above-described nanocarbon solidification step.
  • Nanocarbon dispersion and preparation method according to an aspect of the present invention is a simple but conventional method for dispersion, which has not been predicted at all.
  • the method of evaluating nanocarbon using the nanocarbon dispersion according to another aspect of the present invention can be applied to the nanocarbon dispersion on the film to evaluate the nanocarbon by nanocarbon manufacturers can use a nanocarbon suitable for the application.
  • the manufacturing method of the nanocarbon material using the nanocarbon dispersion it is possible to easily make a concentrate with the nanocarbon dispersion, dilute the high concentrate produced by the transparent electrode, coating agent for ESD / EMI Nanocarbon-based coating solution or ink for printing semiconductors, IC packaging, displays, energy fields, automobiles, building glass and anti-static flooring, and electronics , Backlight, adhesive-adhesive, tape, secondary battery active material and electrode, solar cell electrode, battery active material and electrode, fuel cell separator, heating element, radiator, abrasive [car, aircraft, ship, tank, motorcycle, industrial material ], Smart cement, glass, foam, prepreg, nano-fluid, biomaterials, RFID can be used.
  • CNF high heat-resistant materials
  • SiC silicon carbide
  • ZnS boron-silicon
  • Boron Nitride magnetic material
  • (expanded) graphite metals and high heat-resistant materials in high concentrations, heat resistance, water resistance, flame resistance, fire resistance, heat dissipation, wear resistance, high dielectric constant for special applications
  • a mixture of a mixture of hydrophobic fluorine, silicones, magnetic bodies, thermally conductive fillers, and foamed insulations may be added to form a high-electron-conductive and multifunctional slime intermediate.
  • a method for preparing a nanocarbon solid may include reducing the size of a nanocarbon bundle in one step, liquefying by applying a dispersion using a solvent and a dispersant in two steps, and then coagulating, powdering and solidifying steps.
  • a dispersion using a solvent and a dispersant in two steps, and then coagulating, powdering and solidifying steps.
  • the manufacturing method of the nanocarbon material using the nanocarbon solids it is possible to easily make a dispersion (concentrate) to the nanocarbon solids, dilute the high concentrates made transparent electrode, ESD Nano-carbon-based coating solution or ink for printing, semiconductors, IC packaging, displays, energy and automotive, architectural glass and anti-static flooring, printing, etc./ coating for EMI, high-heat and heat-resistant nanocarbon-polymer slime intermediates and paints, Emitters for electronic products, backlights, adhesives, tapes, secondary battery active materials and electrodes, solar cell electrodes, battery active materials and electrodes, fuel cell separators, heating elements, radiators, abrasives [cars, aircraft, ships, tanks, two-wheelers Machine and industrial materials], smart cement, glass, foam, prepreg, nano fluid, bio materials, RFID and the like.
  • 1 is a graph analyzing the particle size of the carbon nanotube bundle according to the first experimental example of the present invention.
  • 2 to 4 are photographs showing a state in which carbon nanotube bundles are cut for 10 minutes, 20 minutes, and 30 minutes according to the second experimental example of the present invention.
  • 5 and 6 are graphs of the particle size analysis in the state of cutting the carbon nanotube bundle 10 minutes and 30 minutes respectively according to the third experimental example of the present invention.
  • FIG. 7 is a photograph of the results obtained by SEM photographing the 2 wt% nanocarbon dispersion prepared according to Example 1 in Experimental Example 4.
  • FIG. 7 is a photograph of the results obtained by SEM photographing the 2 wt% nanocarbon dispersion prepared according to Example 1 in Experimental Example 4.
  • FIG. 8 is a photograph taken after preparing a high thermal conductive paint according to Experimental Example 9 and applying a thermal shock.
  • FIG. 8 is a photograph taken after preparing a high thermal conductive paint according to Experimental Example 9 and applying a thermal shock.
  • SWCNT 9 is a SEM picture of a transparent electrode of a single wall carbon nanotube (SWCNT).
  • 10 to 13 is a graph showing the Raman characteristics of the nanocarbon solids according to Examples 21 to 24 of the present invention.
  • FIG. 23 is a SEM photograph of a nanocarbon solid (Example) and a general nanocarbon powder (Comparative Example) according to an embodiment of the present invention in which nanocarbon solids are well dispersed and isolated.
  • a solid refers to an object having a certain shape as a solid and is simply distinguished from a powder.
  • the nanocarbon solids means that the solids containing nanocarbon, the content of the nanocarbon is greater than the total content of the other components, which means that can be used as a substitute for nanocarbon powder when powdered.
  • the method for producing a nanocarbon dispersion according to one aspect of the present invention includes a nanocarbon cutting step, and a nanocarbon dispersion step.
  • Nanocarbon cutting step is to cut the provided nanocarbon.
  • cutting the nanocarbon does not mean, for example, cutting the length of carbon nanotubes, which is a type of nanocarbon, but generally due to the noncovalent ⁇ - ⁇ bond and the force of van der Waals. This means that the nanocarbon bundles that are associated with each other are cut to a certain size.
  • the size of the nanocarbon bundle to be cut varies according to the purity, diameter, length, BET, D / G ratio, and degree of entanglement of the provided nanocarbon, and the responsiveness to each solvent and dispersant also appears differently, thus cutting to a certain size.
  • the way to do this may depend on the nanocarbon provided.
  • the size of the bundle of nanocarbons suitable for the dispersion of nanocarbon, which has not been studied or attempted at all, is identified and used for preparing the nanocarbon dispersion.
  • the average particle size of the nanocarbon bundle to facilitate the dispersion of nanocarbon was confirmed to be 0.1 ⁇ m to 5 ⁇ m. If the average particle size is less than 0.1 ⁇ m the excessive cutting process may destroy the properties of the nanocarbon, and the long time cutting process has a problem that is uneconomical, if it exceeds 5 ⁇ m the excessive concentration takes a long time or do not disperse Because there is.
  • the nanocarbon bundle can be cut by dry method using a cutter with a rotation speed of 10000-30000 or by using a ball mill, jet mill, or attrition mill, or by the wet method using ultrasonic wave, wheat, fluidizer, and nanomizer. Can be cut with
  • the cleavage of the nanocarbon used in the present invention means reducing the average particle size of the nanocarbon bundle through grinding of the provided nanocarbon or dispersion in an incomplete liquid phase.
  • the nanocarbon dispersion step comprises nanocarbon bundles having an average particle size of 0.1 to 5 micrometers, 0.01 to 200 parts by weight of a dispersant based on 100 parts by weight of nanocarbon, and an amount of solvent determined according to the nanocarbon content to be made. It is a step of dispersing nanocarbon by mixing into a disperser (ultrasound disperser). If the weight of the dispersant is less than 0.01, there is a problem that the dispersion is difficult due to too few dispersants, if it is more than 200, it is difficult to disperse due to bubbles generated during the process, and troubles when using with other applications There is this.
  • surfactants anionic-SDS, NaDDBS, cationic-CTAB, nonionic-Tween, Triton, amphoteric-Tego5, SAZM Z-3-18
  • coupling agents block copolymers
  • Dispersants such as vinyls, silanes, fluorines, ethers, alcohols, and esters may be used.
  • water, alcohols, cellulsolves, ketones, amides, esters, ethers, aromatics, hydrocarbons, and mixtures thereof may be used as the solvent.
  • dispersants and solvents include, without limitation, all dispersants and solvents for nanocarbon dispersions that are readily available at the lowest cost on the market and include other expensive dispersants.
  • a nanocarbon dispersion in which nanocarbon particles are uniformly dispersed may be prepared, in particular, the concentration of the nanocarbon is more than 2% by weight, 3% by weight, 4% by weight, or High concentration nanocarbon dispersions in excess of 5% by weight can be readily prepared.
  • the nanocarbon dispersion includes a dispersant having 0.01 to 200 parts by weight with respect to 100 parts by weight of nanocarbon, and a predetermined weight percent solvent.
  • the defined weight refers to a predetermined weight percent in order to match the nanocarbon concentration in the nanocarbon dispersion according to the intended use.
  • the viscosity of the nanocarbon dispersion of 2-3% by weight is preferably 100-500cps.
  • Evaluation method of nanocarbon using a nanocarbon dispersion includes a mixing step, a film coating step, and a measuring step.
  • the nanocarbon content of the above-described nanocarbon dispersion is 0.0001 to 0.5% by weight, and is dissolved in a solvent used in a water-soluble urethane (PUD) or a nanocarbon dispersion, for example, acrylic, epoxy, and polyimide.
  • PLD water-soluble urethane
  • nanocarbon dispersion for example, acrylic, epoxy, and polyimide.
  • NMP enmethylpyrrolidone
  • Cellulsolve [EC, BC] melamine / acrylic, when using ethyl acetate [EA] acryl, etc. by mixing 50 to 1000 parts by weight compared to 100 parts by weight of the nanocarbon to prepare a nanocarbon mixture to be.
  • a leveling agent, an antifoaming agent may be further included.
  • the film coating step is a step of forming a coating film by applying the above-described nanocarbon mixture on a substrate with a bar coater, a doctor blade, an application, and the like.
  • the substrate may be a PET, polycarbonate, acrylic, polyimide film, glass, PCB substrate and the like.
  • the measuring step is to measure the electrical conductivity, transmittance, scratch resistance, surface hardness and stability and viscosity of the nanocarbon mixture on the substrate coated with the nanocarbon mixture.
  • the quality of the conventional nanocarbon was made simply by measuring the purity or compressing the powder to evaluate the electrical resistance, but this did not take into account the dispersibility required in manufacturing the application.
  • the evaluation method of the present invention is easy to measure the stability and viscosity of the electrical conductivity, permeability, scratch resistance, surface hardness and nanocarbon mixture after mixing and drying the dispersion dispersion of the same content of nano carbon dispersed in a resin It is easy to evaluate nanocarbon suitable for an application product.
  • a method of manufacturing a nanocarbon material using a nanocarbon dispersion is to prepare a nanocarbon material using the above-described nanocarbon dispersion. That is, by controlling the content of the nano-carbon contained in the nano-carbon dispersions and mixing with a general material it can be produced a nano-carbon material in a simpler method than conventional.
  • the general material means all materials that do not contain nanocarbon.
  • Nanocarbon materials that can be prepared include compounds, masterbatches, transparent electrodes, coatings for ESD / EMI, inks, paints, UV curing coatings, high conductivity, high thermal conductivity paints, ultra high strength, ultra high elasticity and high strength fibers. Manufacturing, large area emitters, backlights, adhesives, tapes, secondary battery active materials and electrodes, solar cell electrodes, battery active materials and electrodes, fuel cell separators, heating elements, radiators, abrasives, smart cement, glass, foams, pres Plugs, nanofluids, biomaterials, RFID, extruded products, various injection molded products, blow molded articles, compressed molded articles, vacuum molded articles, rotary molded articles, and the like can be listed without limitation.
  • the method for producing a nanocarbon solid includes a nanocarbon cutting step, nanocarbon dispersion step, nanocarbon aggregation step, nanocarbon powdering step, and nanocarbon solidification step. That is, the method further includes a nanocarbon agglomeration step, a nanocarbon powdering step, and a nanocarbon solidification step in the method for preparing a nanocarbon dispersion.
  • Nanocarbon cutting step is to cut the provided nanocarbon.
  • cutting the nanocarbon does not mean, for example, cutting the length of carbon nanotubes, which is a type of nanocarbon, but generally due to the noncovalent ⁇ - ⁇ bond and the force of van der Waals. This means that the nanocarbon bundles that are associated with each other are cut to a certain size.
  • the size of the nanocarbon bundle to be cut varies according to the purity, diameter, length, BET, D / G ratio, and degree of entanglement of the provided nanocarbon, and the responsiveness to each solvent and dispersant also appears differently, thus cutting to a certain size.
  • the way to do this may depend on the nanocarbon provided.
  • the size of a bundle of nanocarbons suitable for dispersion of nanocarbons, which has not been studied or attempted at all, is identified and used for preparing nanocarbon solids.
  • the average particle size of the nanocarbon bundle to facilitate the dispersion of nanocarbon was confirmed to be 0.1 ⁇ m to 5 ⁇ m. If the average particle size is less than 0.1, excessive cutting process may destroy the properties of nanocarbon, and long time cutting process is uneconomical, and if it is more than 5, it takes excessive time or high dispersion when concentrated. to be.
  • the nanocarbon bundle can be cut by dry method using a cutter with a rotation speed of 10000-30000 or by using a ball mill, jet mill, or attrition mill, or by the wet method using ultrasonic wave, wheat, fluidizer, and nanomizer. Can be cut with
  • the cleavage of the nanocarbon used in the present invention means reducing the average particle size of the nanocarbon bundle through grinding of the provided nanocarbon or dispersion in an incomplete liquid phase.
  • the nanocarbon dispersion step includes nanocarbon bundles having an average particle size of 0.1 to 5 ⁇ m, a dispersant for 0.01 to 300 parts by weight based on 100 parts by weight of nanocarbon, and an amount of solvent determined according to the nanocarbon content to be made. It is a step of dispersing nanocarbon by mixing into a disperser (ultrasound disperser and high dispersion molten metal, etc.). If the weight of the dispersant is less than 0.01, it is difficult to disperse due to too few dispersants. If the dispersant exceeds 300, it is difficult to disperse due to bubbles generated during the process due to excessive dispersant, and it becomes a trouble factor when using with other applications. There is this.
  • a disperser ultrasound disperser and high dispersion molten metal, etc.
  • surfactants eg, anionic: sodium dodecyl sulfate), NaDDBS (sodium dodecylbenzenesulfonate), cationic: CTAB (Cetyl Trimethyl Ammonium Bromide), nonionic: Tween TM (poly oxyethylene sorbitan), Triton TM, positive system: Tego5 TM, SAZM TM Z-3-18), coupling agents, block copolymers, monomers, oligomers, vinyls, lactics, caprolactones, silicones, waxes , Dispersants such as silanes, fluorines, ethers, alcohols, esters and mixtures thereof may be used.
  • CTAB Cetyl Trimethyl Ammonium Bromide
  • Tween TM poly oxyethylene sorbitan
  • Triton TM positive system: Tego5 TM, SAZM TM Z-3-18
  • coupling agents block copolymers, monomers, oligomers, vinyls,
  • water, alcohols, cellulsolves, ketones, amides, esters, ethers, aromatics, hydrocarbons, and mixtures thereof may be used as the solvent.
  • dispersants and solvents include, without limitation, all dispersants and solvents for nanocarbon dispersions that are readily available at the lowest cost on the market and include other expensive dispersants.
  • Nanocarbon flocculation step is a step of sludge the nanocarbon liquid by further adding a flocculant to the above-described dispersed nanocarbon liquid.
  • a flocculant chitosan, mineral additives (lime, calcium salts), polymer electrolytes, polyacrylamide-based synthetic polymers, polyaluminum chloride-based metal salts, organic solvents, inorganic polymers (PFS (Polyferrocenylsilane) , PFC (Polyferricchloride), metal salts, anti-dispersant of the dispersant used, natural organic streams (starch derivatives, guar gums, tannins, alginates) can be used, the amount of flocculant added is 0.01 to 100 parts by weight of nanocarbon 200 parts by weight is preferred.
  • Nanocarbon powdering step is a step of removing the liquid components from the precipitated sludge-ized nanocarbon sludge by filtering, centrifugation and spray drying, and pulverizing or crushing into powder.
  • the nanocarbon solidification step is to put the nanocarbon powder into a mold to form a predetermined shape, and put it in a dryer such as a cabinet dryer, a rotary quill dryer, a hot air dryer, a conveyor hot air dryer, a vacuum dryer, a far-infrared dryer, a microwave dryer, and dry it between 80-350.
  • a dryer such as a cabinet dryer, a rotary quill dryer, a hot air dryer, a conveyor hot air dryer, a vacuum dryer, a far-infrared dryer, a microwave dryer, and dry it between 80-350.
  • the mold for making the powder into a predetermined shape includes an intaglio molder, a crusher, a tablet press, a ceramic press, an extruder (screw, hydraulic, pneumatic) and the like.
  • the shape of the solid to be produced can be produced in a variety of shapes, such as chips, pellets, eggs, pills, beads, necklaces, thin flakes, etc. are not limited to the shape.
  • the nanocarbon may further comprise a heat treatment step after the nanocarbon solidification step. That is, high-purity nanocarbon solids can be prepared by removing the dispersing agent and the flocculant contained in the nanocarbon solids through heat treatment.
  • the heat treatment may be performed in 350-400 before the nanocarbon is burned with a dryer in the presence of oxygen, or heat-treated with 600-2200 without oxygen (for example, nitrogen or argon atmosphere) (see FIGS. 14 to 17). Can be done in a manner.
  • the nanocarbon solids prepared according to the above-described method for preparing the nanocarbon solids measured the oil absorption according to the KS M ISO 787-5 measuring method. As a result, the oil absorption of the normal carbon nanocarbons was about 400-1100 g / ml.
  • the oil absorption of the eggplant but the solid body according to the present invention is characterized by 200g / ml to ⁇ 500g / ml. This is judged to be the result of being made into a solid body again after the preparation of the dispersion (see Experimental Example 16).
  • FIG. 22 is a TGA / DSC graph in the oxygen atmosphere of the nanocarbon solid according to the present invention, which shows that the dispersing agent and the coagulant included in the nanocarbon solid preparation are finally included in the nanocarbon solid. In other words, the dispersant and flocculant are burned out in the oxygen atmosphere.
  • Figure 23 is a SEM photograph of the nano-carbon solids according to the present invention showing the difference between the particles and the well-dispersed state between the normal nanocarbon powder.
  • the compressive strength is 0.1 to 3MPa
  • the apparent density is 0.1 to 0.5g / cc
  • the nanocarbon content of 90 to 99.9wt% can be prepared nanocarbon solids.
  • the compressive strength is less than 0.1, it is difficult to maintain the mold due to the low strength, and there is no advantage as a solid body when handling, and when it is over 3, it is too hard to be broken, making liquid dispersion or compounding difficult to disperse. have.
  • the apparent density is less than 0.1, there is a problem that it is difficult to maintain solids due to the low density, and when it exceeds 0.5, it is difficult to solve because it is too hard due to the high density.
  • the nanocarbon content is less than 90wt%, there is a problem that it affects the manufacture and quality of the final product due to volatilization of the additive caused by excessive additives, incompatibility with the application matrix, and when manufacturing more than 99.9wt% Due to the high heat treatment-utility (non-oxygen atmosphere) cost and the use of very little dispersant and flocculant, there is a problem in that dispersion and flocculation are difficult in preparing a solid.
  • nanocarbon dispersions may be prepared as the above-described nanocarbon solids.
  • the nanocarbon dispersion is a liquid dispersion liquid by vacuum-defoaming while adjusting the temperature, pressure, and rotational speed with 100 to 100 parts by weight of nanocarbon solids, together with 50 to 990000 parts by weight of solvent or 50 to 9900 parts by weight of liquid resin in a disperser or stirrer.
  • the solvent is used in less than 50 parts by weight, it is difficult to form a dispersion due to the high specific surface area of the nanocarbon solids, and when it exceeds 999900 parts by weight, the solid content of the nanocarbon solids is too small, making it difficult to implement thermal-electric properties. There is a problem.
  • liquid resin when used in less than 50 parts by weight of the high specific surface area of the nano-carbon is difficult to use and difficult to match the product properties of the product made difficult, if it exceeds 9900 parts by weight of the solid content of the nano-carbon solids too There is a problem in that it is difficult to implement the thermal-electrical properties.
  • the solvent used is not limited, and water, alcohol, and various commercial solvents may be used, and the liquid resin may use a liquid resin and a liquefied thermoplastic, thermosetting resin.
  • Evaluation method of nanocarbon using a nanocarbon solid according to another aspect of the present invention includes a mixing step, a molding step, and a measuring step.
  • the mixing step is a step of mixing the nanocarbon and the matrix resin.
  • a simple mixer is mixed with 97 to 99% by weight of the matrix resin (for example, polycarbonate) and 1 to 3% by weight of the nanocarbon solid prepared according to the present invention, followed by mixing at low speed.
  • the molding step is a step of forming a molded article by molding a mixture of the matrix resin and the nanocarbon solids after the mixing step by an extruder or an injection machine.
  • the measuring step is a step of measuring the electrical resistance, tensile strength, elongation, modulus, impact strength for the manufactured molded product specimens.
  • the shearing force is increased in a twin screw extruder having at least 40 L / D, at least 3 kneading blocks, and at least one reverse screw segment (1 / 2-1D).
  • a method for producing a nanocarbon material using a nanocarbon solid and a dispersion is to prepare a nanocarbon material using the above-described nanocarbon solid or dispersion. That is, the nanocarbon material may be manufactured by a simpler method than the conventional method by controlling the content of the nanocarbon contained in the nanocarbon solids or dispersion and mixing it with a general material.
  • the general material means all materials that do not contain nanocarbon.
  • Nanocarbon materials that can be prepared from these include compounds, masterbatches, transparent electrodes, coatings for ESD / EMI, inks / coatings / paints, high-conductivity conductive paints, and ultra high-strength steels.
  • the nanocarbon-polymer composite according to the present invention is an automotive plastic exterior material such as Fender, Door handles, Mirror housing, Fuel line / tank for On-line painting. (Fuel line / tank), quick connects, O-rings, pump modules, etc. can be used in the automotive industry, such as automotive fuel systems, and a variety of products in the computer and semiconductor industry Can be applied.
  • the mixture consisting of 900 parts by weight of water and 10-100 parts by weight of nanocarbon was placed in an ultrasonic grinder and cut for 48 hours to cut the average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 50-200 parts by weight of dispersant NADDBS and a solvent were mixed with 100 parts by weight of the nanocarbon bundle, and the mixture was placed in an ultrasonic disperser for 1-3 hours to prepare a 2% by weight nanocarbon dispersion.
  • the nanocarbon was cut into a 20000 rpm caterer, cut through a 300-500 mesh filter, and cut to an average particle size of about 5 ⁇ m.
  • 100-200 parts by weight of dispersant PVP and alcohol were mixed with 100 parts by weight of the nanocarbon bundle of cut nanocarbon bundle, and put into an ultrasonic disperser for 1-3 hours to prepare a nanocarbon dispersion containing 3% by weight of nanocarbon. It was.
  • Example 3 A mixture of 100 parts by weight was placed in a nanomizer and cut for 0.5-1 hour to cut the average particle size of the nanocarbon bundle to about 0.2-3 ⁇ m. 100-200 parts by weight of the dispersant CTAB and the solvent were mixed with 100 parts by weight of the nanocarbon bundle, and the mixture was placed in an ultrasonic disperser for 1-3 hours to prepare a 2.5% by weight nanocarbon dispersion.
  • a mixture of 900 parts by weight of water, 30 parts by weight of dispersant, and 10-100 parts by weight of nanocarbon was placed in a fluidizer and cut for 0.5 hours to cut the average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 100 parts by weight of the dispersant block copolymer and 100 parts by weight of the mixture containing the cut nanocarbon bundle was mixed and put into a high-dispersion mill disperser for 1-3 hours to prepare a 3% by weight nanocarbon dispersion It was.
  • Compounds, masterbatches, and the like can be prepared while feeding 3 to 50% by weight of the nanocarbon dispersion to 1-50% of the sider liquid during extrusion of the matrix resin.
  • the mixed mixture may be fed with a cider liquid phase to prepare a compound and a masterbatch.
  • the matrix resin of the compound may be a thermoplastic resin, a thermosetting resin, an enpra resin, a super enpra resin, an alloy resin, a vegetable-friendly resin, a liquid resin, or a mixed form.
  • the nanocarbon dispersion can be diluted or prepared as is, for transparent electrodes, ESD / EMI, ink / coating agents / paints.
  • the nanocarbon dispersion in which water is dispersed in water and alcohol in 3% by weight of carbon nanocarbon, to 0.2-1% by weight, it is applied to a substrate [glass, film, metal plate, PCB, plastic molding ..] and the dispersant is washed with a solvent.
  • the conductive polymer is vapor-phase polymerized in the CVD chamber, or is made on the surface of the gas-polymerized substrate as it is, or the surface is made very hard, and then put into a sputtering chamber to prepare a metal thin film by metal sputtering.
  • Highly conductive paint is made with a stirrer or disperser while vacuum degassing by adding 2-50% by weight of nanocarbon liquid dispersion to 0.5-50% by weight of metal (gold, silver, nickel, copper, alloy) particles, conductive filler and binder resin. .
  • nanocarbon dispersion 3 to 80% by weight of the nanocarbon dispersion is added with a thermally conductive material (CNF, CF, metal, alumina, SiC, nanodiamond, ZnS, Boron Nitride, magnetic material, (expansion) graphite, conductive polymer) and binder resin
  • a high heat dissipation paint is produced with a disperser.
  • Nanocarbon dispersion (0.1-10% by weight of nanocarbon solids) and filler (1-80% by weight of total solids) and filler (total solids 1-80% by weight) are added to a resin composition for adhesive-adhesive to prepare a mixture under heat, pressure, vacuum or deoxygenation atmosphere.
  • conductive-insulating adhesive agent suitable for the purpose of tape materials metal, resin film, ceramic, graphite, etc.
  • attaching release paper and then applying non-coating, conductive and insulating paint or adhesive agent as necessary.
  • conductive-insulating adhesive agent suitable for the purpose of tape materials metal, resin film, ceramic, graphite, etc.
  • Nanocarbon dispersions and solids are added to active materials for high energy density and high output of secondary batteries and capacitors, or nanocarbon dispersions or solids are used to form electrodes to increase electrical conductivity per unit weight and volume.
  • Nanocarbon dispersions or solids are used for low viscosity, high stiffness resins to produce separation plates having the required physical properties of 50 S / CM and 60 Mpa.
  • the nanocarbon liquid dispersions or solids are spun-fiberized together with the liquid resins or solid resins for the fibers or with side-feeding, and weaved or spun to produce fibers of ultra high strength, ultra high elasticity, and ultra high conductivity.
  • Nanocarbon dispersion or nanocarbon solids of FTO coated glass substrate or transparent electrode film are attached at 0.02-1 ⁇ m, and then nanofiller (titanium dioxide) is applied, dye is applied thereon, and the other side is the same glass, film After attaching the platinum coated [plated] nanocarbon to the conductive material containing the nanocarbon dispersion in the middle is prepared after sealing.
  • nanofiller titanium dioxide
  • Nanocarbon dispersions or nanocarbon solids are added to metals, ceramics, graphite, cement raw materials, glass raw materials, and diamonds to uniformly disperse and mix, compress them with a press, or use a molding machine to make various shapes such as circular, spherical, rod, and plate.
  • Eggplants are made in the form of heat and pressure, vacuum sintering and deoxygenation.
  • a fine foam by adding a nano-carbon dispersion or solid to the foam base resin, or by adding a nano-carbon dispersion and a solid to the prepreg resin, anti-static, microwave absorbing material or thermal management material of LED heat dissipation parts, It is used for structural materials such as aircraft fuselage, car body, and sporting goods.
  • Smart clothing made of nanocarbon dispersions or solid fibers can be used to make smart garments that can check the medical condition of the human body, or nanocarbon dispersions can be prepared to maximize thermal efficiency by putting the nanocarbon dispersion into a heat exchanger.
  • Nanocarbon liquid dispersions or solids can be added to electrodes, electron emitters, or inorganic fillers to produce large area emitters and backlights.
  • Extruded products injection molded products, blow molded products, compression molded products, vacuum molded products, rotational molded products, and the like can be manufactured while siding the nanocarbon dispersion or solids at 1-50%.
  • fluorides, silicones, magnetic bodies, thermally conductive fillers, foaming agents, and heat insulating agents which exhibit heat resistance, water resistance, flame resistance, heat dissipation, fire resistance, abrasion resistance, high dielectric constant, and hydrophobicity together with the nanocarbon dispersion or solid body.
  • Mixing the mixture mixed together, etc. is used to feed extruded products (sheets, films, pipes, fibers, building-civil engineering, automobile parts, electrical-electronic parts), injection molded products, blow molded products, compressed molded products, vacuum molded products, rotary molded products, etc. It can manufacture.
  • the dispersion liquid may be mixed with the matrix resin powder to dry the liquid phase, and then a molded article or a compound for manufacturing a molded article may be manufactured.
  • a solvent and a resin for UV eg Urethane acrylate 50-80, Isobornyl acrylate 1-15, Tripropylene glycol diacrylate 1-15, 1-hydroxy -cyclohexyl-phenyl-ketone 1-10) is mixed to make UV coatings, and to make films, panels (sheets), fibers, metal wires, coatings for electrostatic coatings for automobiles, and electrolytic-fuel cell electrodes. ), It can be used for particle (ceramic, metal) coating.
  • the mixture consisting of 900-990 parts by weight of water and 10-100 parts by weight of nanocarbon was placed in an ultrasonic grinder and cut for 48 hours to cut the average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 10-300 parts by weight of a dispersant NaDDBS and a solvent were mixed with 100 parts by weight of the nanocarbon bundle in a mixture containing the cut carbon nanotube bundle, and then placed in an ultrasonic disperser for 1-3 hours to obtain a 2-10% by weight nanocarbon dispersion.
  • nanocarbon powder is put into a mold or the like to form a predetermined body, and put into a cabinet dryer to dry between 80-350 to make a nanocarbon solid.
  • a mixture consisting of 900-990 parts by weight of water and 10-100 parts by weight of nanocarbon was cut with a fluidizer for 0.5-2 hours to cut an average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 10-300 parts by weight of a dispersant block copolymer and a solvent are mixed with 100 parts by weight of the carbon nanotube bundle and a mixture containing the cut carbon nanotube bundle, and placed in an ultrasonic disperser for 1 to 3 hours to process 2-10% by weight of nanoparticles.
  • nanocarbon powder is made into a predetermined shape through an extruder, put in a cabinet drier, and dried between 80-350 to make a nanocarbon solid.
  • a mixture consisting of 900-990 parts by weight of water [alcohol] and 10-100 parts by weight of nanocarbon was cut by a ball mill for 60-100 hours to cut the average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 10-300 parts by weight of dispersant PVP and solvent are mixed with 100 parts by weight of carbon nanotubes in a mixture containing the cut carbon nanotube bundles, and then placed in an ultrasonic disperser for 1 to 3 hours to obtain a 2-10% by weight nanocarbon dispersion.
  • a vinyl resin is added 0.01-200 parts by weight based on 100 parts by weight of nanocarbon as a flocculant to the dispersed nanocarbon dispersion to form a nanocarbon sludge, and then the liquid component is removed from the sludged nanocarbon sludge, and crushed or crushed.
  • the nanocarbon powder is made into a predetermined body through an extruder, put in a cabinet drier, and dried between 80-250 to make a nanocarbon solid.
  • a mixture consisting of 900-990 parts by weight of water and 10-100 parts by weight of nanocarbon was cut with a nanomizer for 0.5-2 hours to cut the average particle size of the nanocarbon bundle to about 0.2-5 ⁇ m.
  • 10 to 300 parts by weight of dispersant Triton and a solvent are mixed with 100 parts by weight of carbon nanotubes in a mixture containing the cut carbon nanotube bundles, and then placed in an ultrasonic disperser for 1 to 3 hours to obtain a 2-10% by weight nanocarbon dispersion.
  • metal salt FeCl3
  • metal salt FeCl3
  • nanocarbon powder is made into a predetermined shape through an extruder, put into a cabinet drier, and dried between 80-350 (dispersant and flocculant) to make a nanocarbon solid.
  • nanocarbon solids prepared in Example 21-24 100-500 parts by weight of nanocarbon solids prepared in Example 21-24 were added to 999900-500 parts by weight of solvent or liquid resin, and then mixed with mixers, wheat, ultrasonic equipment, rolls, etc., and extruder, kneader, rolls, etc. Prepare -50 parts by weight of nano carbon dispersion.
  • PC resin was introduced into the hopper using a twin screw extruder (TEK-45, L / D: 45, full length: 2040), and the nanocarbon solids prepared in Example 21 were added to the die feed side feeder. Compounding was carried out by compounding at a weight% to 50% by weight to prepare a compound resin.
  • ABS resin was added to the hopper using a twin screw extruder (TEK-45, L / D: 45, full length: 2040), and the nanocarbon solids prepared as in Example 22 were 1% by weight to 50 in the side feeder of the die portion.
  • Compound resin was prepared by compounding, either by weight or by feeding nanocarbon dispersions and solids in another feeder.
  • PP resin was added to the hopper using a twin screw extruder, and the nanocarbon solids prepared as in Example 23 were added at 1% by weight to 50% by weight in the side feeder of the die portion, or the nanocarbon dispersion and the solids were added in another feeder. Molded compound resin was produced while feeding.
  • HDPE resin was introduced into a hopper using a twin screw extruder, and nanocarbon solids, glass fibers, carbon fibers, metal powders, alumina, SiC, nanodiamonds, ZnS, Boron Nitride, magnetic bodies, or the like prepared in Example 21 were used.
  • Compound resin was prepared by mixing the miner filler and compounding it at 1% by weight to 50% by weight in the side feeder of the die portion or by feeding the nanocarbon dispersion and the solid body in another feeder.
  • Nylon resin is introduced into the hopper using a twin screw extruder, and the 3 to 50% by weight of the nanocarbon dispersion and glass fiber, carbon fiber, metal powder, alumina, SiC, nano diamond, ZnS, Boron Nitride, magnetic material, graphite, or mineral filler was mixed and compounded at 5% by weight to 30% by weight in a side feeder of the die portion to prepare a compound resin.
  • HDPE resin was introduced into a hopper using a twin screw extruder, and a compound resin was prepared by feeding the nanocarbon solids prepared as in Example 21 and the nanocarbon dispersion prepared as in Example 24 with a sider feeder.
  • the nanocarbon is cut and mixed with 100 parts by weight of dispersant NADDBS and water with respect to 100 parts by weight of nanocarbon in an average particle size of about 10 ⁇ m, and then put into an ultrasonic disperser for 1-3 hours to prepare 2.5 wt% nanocarbon solution. It was.
  • the average particle size was about 6 ⁇ m, mixed with 100 parts by weight of dispersant CTAB and water with respect to 100 parts by weight of nanocarbon and put into an ultrasonic disperser for 1-3 hours to produce 2.5% by weight of nanocarbon solution It was.
  • Example 1 As in Example 1, a mixture of 900 parts by weight of water and 10-100 parts by weight of nanocarbon was placed in an ultrasonic grinder, and cut for 48 hours to analyze the particle size of the nanocarbon bundle to obtain a result as shown in FIG. 1. According to this, nanocarbon bundles having an average particle size of 0.230 ⁇ m were prepared by wet cutting.
  • Example 2 the shape and size of the nanocarbon bundles were taken when 10 minutes, 20 minutes, and 30 minutes of nanocarbon was put in a 20000 rpm carter. 2 to 4 are photographs showing the state after 10 minutes, 20 minutes, and 30 minutes respectively.
  • Experimental Example 1 shows that the nanocarbon bundle can be cut to an average particle size of 0.1 to 5 ⁇ m by dry cutting.
  • Example 3 a mixture consisting of 900 parts by weight of water and 10-100 parts by weight of nanocarbon was placed in a nanomizer and cut.
  • 5 and 6 are particle size analysis graphs when 10 minutes and 30 minutes treatment with a nanomizer, respectively. According to this, the nanocarbon bundle can be cut to an average particle size of 0.1 to 5 ⁇ m even by wet grinding.
  • the comparative examples show that the characteristics are not good when compared with the examples.
  • the nanocarbon was put into a 10000 to 30000rpm catterer dry, and the average particle size and volume swelling degree of the nanocarbon bundle were examined for each cutting time to obtain the results shown in Table 2.
  • Water-soluble urethane was added to 0.25% by weight of a nanocarbon dispersion prepared by cutting nanocarbon bundles by preparing nanocarbons of six companies (A, B, C, D, E, and F), and dispersing them in water with a nonionic dispersant Tween. 0.5-10 times compared to nanocarbon, the coating film was formed on the film with a bar coater # 6, and the quality of nanocarbon by manufacturer was evaluated.
  • Table 3 is a nanocarbon evaluation table of six companies.
  • Example 7 to prepare a highly conductive paint containing 2% by weight of nanocarbon dispersed in isopropyl alcohol and 2% by weight of silver coated copper, and formed a sample coating film to measure the resistance value of the paint as shown in Table 4 The result was obtained.
  • FIG. 8 shows the surface of the surface due to shrinkage-expansion according to the temperature change to the surface state after 100 times of the process of coating the PET film at a thickness of 5um and then heating at 125 ° C. for 15 minutes and heating at 65 ° C. for 15 minutes The crack condition was tested and shows a good condition.
  • a highly heat-resistant material CNF, metal, alumina, SiC, nanodiamond, ZnS, Boron Nitride, magnetic body, (expanded) graphite

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention concerne un liquide de dispersion de nanocarbone, un procédé d'évaluation de nanocarbones au moyen de ce liquide, un procédé de production de matériaux en nanocarbone au moyen de ce liquide, un procédé de production de matières solides à partir du liquide de dispersion de nanocarbone, des matières solides de nanocarbone produites selon ce procédé, un procédé d'évaluation de nanocarbones au moyen des matières solides de nanocarbone et un procédé de production de matériaux en nanocarbone au moyen de ces matières solides, comprenant une étape de coupe de nanocarbone, consistant à couper des nanocarbones préparés agrégés en paquets à une taille de particule moyenne de 0.1 μm à 5 μm, une étape de dispersion de nanocarbone consistant à mélanger les nanocarbones coupés, 0.01 à 300 parties en poids d'un agent de dispersion pour 100 parties en poids de nanocarbones et un solvant, la dispersion des nanocarbones étant réalisée à l'aide d'un moyen de dispersion.
PCT/KR2010/006521 2009-09-21 2010-09-24 Procédé de préparation d'un liquide de dispersion de nanocarbone, liquide de dispersion de nanocarbone préparé selon ce procédé, procédé d'évaluation de nanocarbones, procédé de production de matériaux en nanocarbone et procédé de production de matières solides en nanocarbone WO2011034408A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2009-0088968 2009-09-21
KR1020090088968A KR101136776B1 (ko) 2009-09-21 2009-09-21 나노카본 분산액의 제조방법, 이를 이용한 나노카본 분산액, 나노카본의 평가방법, 나노카본 소재의 제조방법
KR1020090122319A KR101218366B1 (ko) 2009-12-10 2009-12-10 나노카본 고형체의 제조방법, 이를 이용한 나노카본 고형체, 나노카본 분산액, 나노카본 소재의 제조방법
KR10-2009-0122319 2009-12-10

Publications (2)

Publication Number Publication Date
WO2011034408A2 true WO2011034408A2 (fr) 2011-03-24
WO2011034408A3 WO2011034408A3 (fr) 2011-09-09

Family

ID=43759208

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2010/006521 WO2011034408A2 (fr) 2009-09-21 2010-09-24 Procédé de préparation d'un liquide de dispersion de nanocarbone, liquide de dispersion de nanocarbone préparé selon ce procédé, procédé d'évaluation de nanocarbones, procédé de production de matériaux en nanocarbone et procédé de production de matières solides en nanocarbone

Country Status (1)

Country Link
WO (1) WO2011034408A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111705501A (zh) * 2020-06-12 2020-09-25 山东非金属材料研究所 一种碳纳米材料改性超高分子量聚乙烯纤维及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050097711A (ko) * 2004-04-02 2005-10-10 주식회사 디피아이 솔루션스 고농도 탄소나노튜브 수분산액 및 이의 제조방법
JP2008201626A (ja) * 2007-02-20 2008-09-04 Toray Ind Inc カーボンナノチューブ集合体、その製造方法
JP2008274502A (ja) * 2007-05-07 2008-11-13 Hokkaido Univ 再分散用微細炭素繊維集合塊およびその製造方法
KR100879219B1 (ko) * 2007-10-10 2009-01-16 인하대학교 산학협력단 라텍스 응집에 의한 고분자/탄소나노튜브 복합재료의 제조방법

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050097711A (ko) * 2004-04-02 2005-10-10 주식회사 디피아이 솔루션스 고농도 탄소나노튜브 수분산액 및 이의 제조방법
JP2008201626A (ja) * 2007-02-20 2008-09-04 Toray Ind Inc カーボンナノチューブ集合体、その製造方法
JP2008274502A (ja) * 2007-05-07 2008-11-13 Hokkaido Univ 再分散用微細炭素繊維集合塊およびその製造方法
KR100879219B1 (ko) * 2007-10-10 2009-01-16 인하대학교 산학협력단 라텍스 응집에 의한 고분자/탄소나노튜브 복합재료의 제조방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111705501A (zh) * 2020-06-12 2020-09-25 山东非金属材料研究所 一种碳纳米材料改性超高分子量聚乙烯纤维及其制备方法

Also Published As

Publication number Publication date
WO2011034408A3 (fr) 2011-09-09

Similar Documents

Publication Publication Date Title
KR101324707B1 (ko) 방열용 조성물 및 이를 이용한 방열제품
JP6121074B1 (ja) アルミナ系熱伝導性酸化物及びその製造方法
WO2016190722A1 (fr) Graphène fonctionnalisé comprenant deux types d'amines ou plus, et son procédé de préparation
KR101218366B1 (ko) 나노카본 고형체의 제조방법, 이를 이용한 나노카본 고형체, 나노카본 분산액, 나노카본 소재의 제조방법
WO2017217759A1 (fr) Feuille de film mince conductrice de la chaleur et article comprenant celle-ci.
WO2003024602A1 (fr) Nanostructures en plaquettes de graphite
CN110352178B (zh) 氧化铝系导热性氧化物及其的制造方法
WO2017065340A1 (fr) Procédé de fabrication de composite hybride bidimensionnel
WO2015147449A1 (fr) Feuille de blindage contre les ondes électromagnétiques et son procédé de fabrication
WO2019066543A1 (fr) Procédé de production d'un film mince thermoconducteur à l'aide de poudre de graphite synthétique
Zhao et al. Vitrimeric silicone composite with high thermal conductivity and high repairing efficiency as thermal interface materials
WO2022103116A1 (fr) Procédé de préparation d'une composition de résine composite à l'aide de séparateurs de déchets de batterie secondaire
WO2018194418A1 (fr) Composition de graphite, mélange maître comprenant ladite composition, et matériau composite à base de graphite ainsi réalisé
WO2011034408A2 (fr) Procédé de préparation d'un liquide de dispersion de nanocarbone, liquide de dispersion de nanocarbone préparé selon ce procédé, procédé d'évaluation de nanocarbones, procédé de production de matériaux en nanocarbone et procédé de production de matières solides en nanocarbone
WO2020096400A1 (fr) Composition de résine concentrée conductrice, composition de résine polyamide conductrice, son procédé de fabrication et produit moulé
JP2019206459A (ja) 熱伝導性酸化物及びその製造方法
WO2023013834A1 (fr) Composition de peinture pour dissipateur thermique, son procédé de préparation, film de revêtement pour dissipateur thermique formé à partir de celle-ci, et dissipateur thermique le comprenant
WO2016047988A1 (fr) Nitrure de bore modifié en surface, composition ayant des particules de celui-ci dispersées en son sein, et câble revêtu de la composition
Zhang et al. Investigation of polyimide–mica hybrid films for cryogenic applications
WO2018182111A1 (fr) Solution de type dispersion de nanotubes de carbone et son procédé de préparation
TW202235498A (zh) 四氟乙烯系聚合物組合物之製造方法、組合物、金屬箔積層體及延伸片材
WO2017018599A1 (fr) Poudre de carbure de silicium, corps fritté en carbure de silicium, suspension épaisse de carbure de silicium, et procédé de préparation
WO2020141925A1 (fr) Procédé de fabrication d'une feuille de dissipation de chaleur
WO2010120153A2 (fr) Composition de solution à base de nanocarbone, composition de résine à base de nanocarbone, produit solide à base de nanocarbone, produits résiniques à base de nanocarbone, et leurs procédés de fabrication
EP4148091A1 (fr) Composition de résine thermoconductrice et feuille de dissipation de chaleur

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 10817477

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 10817477

Country of ref document: EP

Kind code of ref document: A2