WO2005040065A1 - カーボンナノチューブ分散複合材料の製造方法 - Google Patents
カーボンナノチューブ分散複合材料の製造方法 Download PDFInfo
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- WO2005040065A1 WO2005040065A1 PCT/JP2004/016494 JP2004016494W WO2005040065A1 WO 2005040065 A1 WO2005040065 A1 WO 2005040065A1 JP 2004016494 W JP2004016494 W JP 2004016494W WO 2005040065 A1 WO2005040065 A1 WO 2005040065A1
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- H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
- H01L23/492—Bases or plates or solder therefor
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
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- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3733—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon having a heterogeneous or anisotropic structure, e.g. powder or fibres in a matrix, wire mesh, porous structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5284—Hollow fibers, e.g. nanotubes
- C04B2235/5288—Carbon nanotubes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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- C—CHEMISTRY; METALLURGY
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- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
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- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention relates to a composite material that utilizes the inherent characteristics of corrosion-resistant and heat-resistant ceramics such as silicon carbide and imparts electrical and thermal conductivity and excellent strength characteristics.
- the present invention relates to a method for producing a carbon nanotube-dispersed composite material in which nanotubes are dispersed in a sintered body of ceramics or metal powder in a net shape.
- carbon nanotubes with an average diameter of l to 45 nm and an average aspect ratio of 5 or more carbon fiber, metal-coated carbon fiber, carbon Proposal of processing and molding a resin composition containing a carbon fiber dispersed in a resin such as an epoxy resin or an unsaturated polyester resin in which fillers such as powder and glass fiber are kneaded (JP 2003-12939) Have been.
- At least one of the components contained in the aluminum alloy material, Si, Mg, and Mn, is combined with the carbon nanofiber to form the carbon nanofiber.
- An aluminum alloy material contained in an aluminum base material has been proposed.
- carbon nanofibers are mixed into a molten aluminum alloy material of 0.1 to 5 vol% and kneaded to form a billet, which is provided as an extruded material of an aluminum alloy material obtained by extruding the billet (Japanese Unexamined Patent Application Publication No. 363716).
- metal compounds can be added to thermoplastic resins with excellent fluidity such as PPS and LCP. , CrB, A1B 2, MgB, carbides: WC, nitrides: TiN, etc.
- thermoplastic resins with excellent fluidity such as PPS and LCP.
- carbon nanotubes Chikaraichi proposed moldability and conductivity of the resin molded article obtained by both elevation (JP 2003- 34751).
- carbon nanotubes are compounded in the matrix of organic polymers such as thermoplastic resins, curable resins, rubber, and thermoplastic elastomers.
- organic polymers such as thermoplastic resins, curable resins, rubber, and thermoplastic elastomers.
- a composite molded article that is oriented in a magnetic field, aligned in a certain direction, and molded in a composite state has been proposed.
- carbon nanotubes It has been proposed to apply various treatments such as a degreasing treatment and a washing treatment to the surface in advance (Japanese Patent Application Laid-Open No. 2002-273741).
- conductive metals such as metal alloys of nanotube wetting elements such as indium, bismuth or lead, and relatively soft and ductile metal powders such as Ag, Au or Sn Press molding of material powder and carbon nanotubes, cutting or polishing, forming protruding nanotubes on the surface, etching the surface to form nanotube tips, and then re-dissolving the metal surface to align the protruding nanotubes
- JP-A-2000-223004 A method of manufacturing the same has been proposed (JP-A-2000-223004).
- the ceramic composite nanostructure is to be composed of multiple polyvalent metal element oxides selected for a certain function.
- it is proposed to select a production method in which different kinds of metal elements are bonded via oxygen, and to produce a columnar body having a short-axis cross section with a maximum diameter of 500 mn or less by various known methods (Japanese Patent Application Laid-Open 2003-238120).
- the above-mentioned carbon nanotubes that are to be dispersed in a resin or an aluminum alloy are required in consideration of the manufacturability of the resulting composite material and the required formability.
- a material having a length as short as possible is used to improve dispersibility, and does not attempt to effectively utilize the excellent electrical and thermal conductivity characteristics of the carbon nanotube itself.
- the present invention takes advantage of the characteristics of ceramics such as silicon carbide and alumina, which are insulative, but have corrosion resistance and heat resistance, as well as metals having versatility and ductility, for example.
- ceramics such as silicon carbide and alumina
- metals having versatility and ductility, for example.
- the aim is to provide a method for producing carbon nanotube dispersed composite materials that makes full use of the characteristics and strength characteristics.
- the present inventors have developed a composite material in which carbon nanotubes are dispersed in a base material, which was previously developed based on the development commission of the Japan Science and Technology Agency, and developed the electrical, thermal, and strength properties of carbon nanotubes.
- a composite material in which carbon nanotubes are dispersed in a base material, which was previously developed based on the development commission of the Japan Science and Technology Agency, and developed the electrical, thermal, and strength properties of carbon nanotubes.
- long-chain carbon nanotubes were mixed and kneaded with a ceramic or metal powder that can be fired using a ball mill, or wet-dispersed with a dispersant, and the resulting dispersion was obtained. It has been found that by integrating the materials by spark plasma sintering, the carbon nanotubes can be wrapped around the sintered body in a net-like manner, and the above object can be achieved.
- the inventors have found that in the above process, the disintegration is improved by using a ball mill for kneading and dispersing the carbon nanotubes and the ceramics.
- a container holds an appropriate amount of carbon nanotubes and ceramics and revolves at high speed and revolves at high gravity.
- the dispersion and crushing proceed favorably, and the distribution and uniformity of the reticulated carbon nanotubes dispersed and integrated in the obtained sintered body are improved, and the desired electric power is obtained.
- the inventors have found that conductivity, heat conductivity, and strength are further improved, and have completed the present invention.
- the present invention relates to a ceramic powder or a metal (including an alloy thereof) powder.
- a method for producing a carbon nanotube-dispersed composite material comprising: a step of subjecting the obtained kneading / dispersing material to discharge plasma treatment; and a step of subjecting the dispersing material to discharge plasma sintering.
- the composite material according to the present invention is a sintered body of ceramic powder such as alumina and zirconium having excellent corrosion resistance and heat resistance, and a metal powder such as pure aluminum, aluminum alloy and titanium having excellent corrosion resistance and heat dissipation.
- ceramic powder such as alumina and zirconium having excellent corrosion resistance and heat resistance
- metal powder such as pure aluminum, aluminum alloy and titanium having excellent corrosion resistance and heat dissipation.
- the material itself inherently has corrosiveness and excellent durability in a high-temperature environment, and the long-chain carbon nanotubes are uniformly dispersed therein.
- the required properties can be enhanced, a synergistic effect, or a new function can be exhibited by combining the excellent electrical and thermal conductivity properties and strength of the carbon nanotube itself.
- the composite material according to the present invention is obtained by pulverizing a ceramic powder or a metal powder or a mixed powder of a ceramic and a metal and a long-chain carbon nanotube by a known pulverization method. It can be manufactured by a relatively simple manufacturing method of applying a high gravity without using a media such as a crushing mill or Shii force and mixing and dispersing by applying high gravity, and sintering the dispersing material by discharge plasma.For example, corrosion, high temperature environment It can be used as an electrode, a heating element, a wiring material, a heat exchanger or a heat sink material with improved thermal conductivity, a brake component, or an electrode-separator of a fuel cell.
- FIG. 1 is a graph showing the relationship between the plasma sintering temperature and the electric conductivity.
- FIG. 2 is a graph showing the relationship between the sintering pressure and the electrical conductivity.
- FIG. 3 is an electron micrograph of a cocoon-shaped carbon nanotube according to the present invention.
- FIG. 4 is a schematic view of an electron micrograph of a carbon nanotube dispersed composite material using alumina as a matrix according to the present invention.
- FIG. 5A is an electron micrograph of the forced fracture surface of the aluminum nanoparticle dispersed composite material having an aluminum matrix according to the present invention
- FIG. 5B is an enlarged electron micrograph of the forced fracture surface.
- FIG. 6 is an electron micrograph of aluminum particles before kneading and disintegration.
- FIG. 6A shows a scale of 20 ⁇ order
- FIG. 6 ⁇ shows a scale of 1 ⁇ order.
- Fig. 7 is an electron micrograph of the aluminum particles after kneading and disintegration.
- Fig. 7 ⁇ is a scale electron micrograph of the order of 30 ⁇ , and
- Fig. 7 ⁇ is an enlarged electron micrograph of the depression shown in Fig. 7 ⁇ on the order of ⁇ .
- FIG. 8A is an enlarged electron micrograph of the concave portion shown in FIG. 7 on the order of ⁇
- FIG. 8 is an enlarged electron micrograph on the order of 500 nm.
- FIG. 9A is an enlarged electron micrograph of the smooth portion shown in FIG. 7A in the order of ⁇
- FIG. 9 ⁇ ⁇ is an enlarged electron micrograph of the order of ⁇
- FIG. 10 is an enlarged electron micrograph of the order of 500 nm of the smooth portion shown in FIG. 7A.
- FIG. 11A is an electron micrograph of a forced fracture surface of the carbon nanotube dispersed composite material using titanium as a matrix according to the present invention
- FIG. 11B is an enlarged electron micrograph of the forced fracture surface.
- FIG. 12A is an electron micrograph of titanium particles before kneading and disintegration
- FIG. 12B is an electron micrograph of titanium particles after kneading and disintegration.
- FIG. 13A is an enlarged electron micrograph of the order of ⁇ on the titanium particle surface shown in FIG. 12B
- FIG. 13B is an enlarged electron micrograph of the order of 500 ⁇ .
- FIG. 14A is an electron micrograph of the forced fracture surface of the carbon nanotube dispersed composite material using copper as a matrix according to the present invention
- FIG. 14B is an enlarged electron micrograph of the forced fracture surface.
- FIG. 15 is an electron micrograph of the copper particles before kneading and disintegration.
- FIG. 15A shows a scale of 1 ⁇
- FIG. 15 ⁇ shows a scale of 50 ⁇ .
- FIG. 16A is a ⁇ order magnification electron micrograph of the surface of the copper particles after kneading and disintegration
- FIG. 16B is a magnification electron micrograph on the order of 500 nm.
- FIG. 7 is an electron micrograph of the forced fracture surface of the carbon nanotube dispersed composite material having a zirconium matrix according to the present invention
- FIG. 17B is an enlarged electron micrograph of the forced fracture surface.
- FIG. 18 is an electron micrograph of the zirconia particles before kneading and disintegration.
- FIG. 18A shows a scale of 50 ⁇ order
- FIG. 18B shows a scale of 500 nm order.
- FIG. 19A is an enlarged electron micrograph of the order of 30 ⁇ on the surface of the zirconia particles after kneading and crushing
- FIG. 19B is an enlarged electron micrograph of the order of 500 nm
- Fig. 20 is an electron micrograph of silicon carbide particles before kneading and crushing.
- Fig. 20A shows a scale on the order of 5pm
- Fig. 20 ⁇ shows a scale on the order of 500nm.
- FIG. 21A is an enlarged electron micrograph of the order of 5 ⁇ on the surface of the silicon carbide particles after kneading and crushing
- FIG. 21B is an enlarged electron micrograph of the order of 500 nm.
- the ceramic powder to be used known ceramics having high functions and various functions such as alumina, zirconium, aluminum nitride, silicon carbide and silicon nitride can be adopted.
- a well-known functional ceramic that exhibits required functions such as corrosion resistance and heat resistance may be used.
- the particle size of the ceramic powder is determined in consideration of the sintering property capable of forming a required sintered body or the crushing ability at the time of kneading and dispersing with a carbon nanotube. The following are preferred, for example, it is possible to use several kinds of particles having different particle sizes, and it is also possible to adopt a configuration in which a plurality of powder types have different particle sizes. In addition to the spheres, fibrous, amorphous and various forms of powder can be used as appropriate.
- the metal powder to be used pure aluminum, a known aluminum alloy, titanium, a titanium alloy, copper, a copper alloy, stainless steel, or the like can be used.
- a known functional metal exhibiting required functions such as corrosion resistance, thermal conductivity, and heat resistance may be used.
- the particle size of the metal powder should be approximately ⁇ or less, and more preferably 50 ⁇ or less, which has the sintering property capable of forming the required sintered body and the crushing ability during kneading and dispersion with carbon nanotubes. It is also preferable to employ a composition in which a plurality of powder types are used, and a configuration in which a plurality of powder types have different particle sizes can be employed. In the case of a single powder, the particle size is preferably ⁇ ⁇ or less. In addition to the spheres, fibrous, amorphous, tree-like or various forms of powder can be used as appropriate. 50 ⁇ for aluminum etc.! ⁇ 150 ⁇ is preferred.
- the long-chain carbon nanotubes to be used are literally formed by connecting carbon nanotubes to form a long chain.
- a cocoon or net-like material obtained by discharge plasma treatment of carbon nanotubes alone is used.
- the structure of the carbon nanotube itself can be either single-walled or multi-walled.
- the content of carbon nanotubes is not particularly limited as long as a sintered body having a required shape and strength can be formed. By appropriate selection, it is possible to contain, for example, 90 wt% or less by weight.
- the homogeneity of the composite material for example, reduce the content of carbon nanotubes to 3 wt% or less and, if necessary, to about 0.05 wt%, and devise kneading conditions such as selection of particle size and kneading dispersion method. There is a need to.
- the method for producing a carbon nanotube-dispersed composite material according to the present invention comprises:
- the above-mentioned long-chain carbon nanotubes are converted into a ceramic powder, a metal powder, or a mixed powder of ceramic and metal. It is important to disintegrate.
- various known mills, crushers and shakers for pulverizing, crushing and crushing can be appropriately employed, and the mechanism is also a rotary shock type, a rotary shear type, a rotary shock shear type, and a medium stirring.
- a well-known mechanism such as a stirring type, a stirring type, a stirring type without a stirring blade, and an air-flow crushing type can be appropriately used.
- planetary mills rotate and revolve storage containers at the same time, and usually use a medium such as a ball to perform crushing and disintegration.
- the container capacity is reduced without using media.
- the carbon nanotubes, ceramics, the particle size and amount of metal, etc., and the rotation speed (gravity applied) of the container By appropriately selecting the amount to be stored, the carbon nanotubes, ceramics, the particle size and amount of metal, etc., and the rotation speed (gravity applied) of the container, the carbon nanotubes can be applied to the ceramics and metal particles. Dispersion and adhesion can be performed efficiently and reliably. That is, the applied gravity is appropriately selected along with the processing time according to the storage amount in the container capacity, the particle size and amount of carbon nanotubes, ceramics, and metal, and the rotation speed of the container.
- the wet dispersing step is performed by adding a known nonionic dispersing agent, a positive / negative dispersing agent, and using an ultrasonic dispersing device, a ball mill, and the above-described various mills, crushers, and shaker devices. Dispersion can be performed, and the above-mentioned dry dispersion time can be reduced and efficiency can be improved.
- a known heat source or a spin method can be appropriately employed as a known heat source or a spin method.
- the steps of kneading and dispersing and the step of wet dispersing include various methods such as wet-dispersing after dry-kneading and dispersing, kneading and dispersing after wet-dispersing, and combining with dry, wet and dry. Can be employed.
- kneading and dispersing in the same dry state for example, carbon nanotubes and ceramics can be kneaded and dispersed first, and then metal powder can be kneaded and dispersed therein, or kneading and dispersing can be repeated for each particle size of the powder. .
- various kneading and dispersing steps such as wet kneading and dispersing the carbon nanotubes and ceramics first, and then dry kneading and dispersing the metal powder in the dried dispersing material are performed.
- a dry kneading and dispersing material is loaded between a carbon die and a punch, and a direct pulse current is applied while pressurizing the upper and lower punches.
- Joule heat is generated in the material to be processed, the punch, and the material to be processed, and the kneading and dispersing material is sintered.
- discharge plasma is generated between the powder, the powder, and the carbon nanotube. Re-sintering proceeds smoothly due to the activation of the powder and impurities on the surface of the carbon nanotube, for example.
- the discharge plasma treatment conditions applied only to the carbon nanotubes are not particularly limited.
- the temperature is appropriately selected from the range of 200 ° C to 1400 ° C, the time is about 1 minute to 15 minutes, and the pressure is 0 to 10 MPa. Can be.
- the process of further subjecting the kneaded and dispersed material obtained by the dry method or the wet method or both to discharge plasma treatment is performed before the discharge plasma sintering process. Effects such as stretching action, surface activation, and diffusion of powder are produced, and the thermal conductivity and conductivity imparted to the sintered body are improved with the smooth progress of the subsequent discharge plasma sintering.
- the discharge plasma treatment conditions for the kneading and dispersing material are not particularly limited, but considering the sintering temperature of the material to be treated, for example, the temperature is 200 ° C to 1400 ° C, the time is about 1 minute to 15 minutes, The pressure can be appropriately selected from the range of 0 to 10 MPa.
- the spark plasma sintering is preferably performed at a temperature lower than the normal sintering temperature of the ceramic powder or metal powder to be used.
- the step of spark plasma sintering of the kneading and dispersing material it is also preferable to perform two steps of first performing low-temperature plasma discharge under low pressure and then performing low-temperature discharge plasma sintering under high pressure. Precipitation hardening after sintering, phase transformation by various heat treatments It is also possible to use. The levels of pressure and temperature are relative between the two steps, and it is only necessary to set a difference in level between the two steps.
- the composite material according to the present invention can be manufactured by the above-described relatively simple manufacturing method, and is provided with electrodes, heating elements, wiring materials, heat exchangers and heat sink materials with improved thermal conductivity, and brakes under corrosion, high temperature environment. Although it can be applied as a part, it is possible to obtain a thermal conductivity of 800 W / mK or more, as shown in the examples. It can be easily fired into a shape and is ideal for heat exchanger applications.
- Alumina powder having an average particle diameter of 0.6 ⁇ and long-chain carbon nanotubes were dispersed in a ball mill using an alumina bowl and balls. First, 5 wt% of carbon nanotubes were blended, alumina powder which had been sufficiently dispersed in advance was blended, and these powders were kneaded and dispersed in a dry state for 96 hours.
- a nonionic surfactant Triton X-100, lwt% was added as a dispersant, and the mixture was wet-dispersed by applying ultrasonic waves for 2 hours or more. The resulting slurry was filtered and dried.
- the dried kneading and dispersing material is loaded into a die of a discharge plasma sintering apparatus,
- Plasma solidification was performed at 1300 ° C to 1500 ° C for 5 minutes. At that time, the heating rate is
- the temperature was set to 100 ° C / Min and 230 ° C / Min, and a pressure of 15 to 40 MPa was continuously applied.
- the electrical conductivity of the obtained composite material was measured, and the results shown in FIGS. 1 and 2 were obtained.
- FIG. 3 shows an electron micrograph of the obtained cocoon-shaped carbon nanotube.
- Alumina powder having an average particle diameter of 0.5 ⁇ and the carbon nanotubes were dispersed in a ball mill using an alumina bowl and balls.
- 5 wt% of carbon nanotubes were blended, and then sufficiently dispersed alumina powder was blended and kneaded and dispersed for 96 hours in a dry state. Further, the same ultrasonic wet dispersion as in Example 1 was performed. The resulting slurry was filtered and dried.
- the dried kneading and dispersing material was loaded into a die of an electric discharge plasma sintering apparatus and solidified by plasma at 1400 ° C. for 5 minutes. At that time, the temperature was raised at a rate of 200 ° C / Min, and a pressure of 15 MPa was applied first, followed by a pressure of 30 MPa.
- the electric conductivity of the obtained composite material was in the same range as in Example 1. An electron micrograph of the obtained composite material is shown in FIG. Example 2-1
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and discharge plasma sintering was performed at 575 ° C for 60 minutes. At that time, the heating rate was 100 ° C / Min, and the pressure of 50 MPa was continuously applied.
- the thermal conductivity of the obtained composite material As a result of measuring the thermal conductivity of the obtained composite material, it was 198 W / mK.
- the thermal conductivity of the solidified body obtained by spark plasma sintering only the aluminum alloy powder under the above conditions was 157 W / mK, and the thermal conductivity of the composite material according to the present invention increased by about 21%. You can see that.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus and subjected to a discharge plasma treatment at 800 ° C for 5 minutes. Thereafter, the kneaded dispersion material was subjected to discharge plasma sintering at 600 ° C for 5 minutes in a discharge plasma sintering apparatus. At that time, the heating rate was 100 ° C / Min, and the pressure of 50 MPa was continuously applied.
- the thermal conductivity of the solidified body obtained by discharge plasma sintering without performing the discharge plasma treatment on the carbon nanotubes and the kneaded dispersion material under the above conditions was 94.1 W / mK.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus and subjected to a discharge plasma treatment at 400 ° C for 5 minutes. Thereafter, the kneaded and dispersed material was subjected to discharge plasma sintering at 600 ° C. for 5 minutes in a discharge plasma sintering apparatus.
- FIG. 5 shows an electron micrograph of the forced fracture surface of the obtained composite material.
- An electron micrograph of the reticulated carbon nanotube when the scale shown in Fig. 5A on the order of ⁇ is enlarged to the order of 5.0 ⁇ is shown in Fig. 5 ⁇ .
- Figures 6A and 6B show electron micrographs of aluminum particles before kneading and disintegration.
- Fig. 7A shows an electron micrograph of aluminum particles after kneading and disintegrating with a planetary high-speed mill
- Fig. 7B shows an enlarged electron micrograph of the order of ⁇ of the recess shown in Fig. 7A.
- Figures 8 ⁇ and 8 ⁇ show magnified electron micrographs of the concave part shown in Fig.
- Figures 9 ⁇ , 9 ⁇ , and 10 show magnified electron micrographs of the order of ⁇ and ⁇ on the order of nm ⁇ and the order of 500 nm, respectively, of the smoothed part shown in Fig. 7 ⁇ .
- the carbon nanotubes uniformly adhere to the surface of the aluminum particles by kneading and disintegrating with a planetary high-speed mill, and in particular, as shown in Figs. It is clear that the aluminum particles are attached three-dimensionally vertically and horizontally to the surface of the aluminum particles.
- CNT carbon nanotubes
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and discharge plasma sintering was performed at 900 ° C for 10 minutes. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied.
- FIG. 11 shows an electron micrograph of a forced fracture surface of the obtained composite material (containing 0.25 wt% of CNT).
- Fig. 11B shows an electron micrograph of the reticulated nanotube when the scale of Fig. 11A of the order of ⁇ is enlarged to the order of ⁇ .
- Example 3-2 As a result of measuring the thermal conductivity of the obtained composite material, it was 18.4 W / mK.
- the thermal conductivity of a solid obtained by spark plasma sintering of pure titanium powder alone under the above conditions is 13.8 W / mK, and the thermal conductivity of the composite material according to the present invention is increased by about 30%.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and discharge plasma sintering was performed at 900 ° C for 10 minutes. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied. As a result of measuring the thermal conductivity of the obtained composite material, it was 17.2 W / inK when only the carbon nanotube was previously subjected to the discharge plasma treatment.
- Figures 12A and 12B show electron micrographs of titanium particles before kneading and disintegration and titanium particles after kneading and disintegrating in a planetary high-speed mill.
- Figs. 13A and 13B show magnified electron micrographs of the order of 500 ⁇ m on the order of ⁇ on the surface of the titanium particles shown in Fig. 12B after being kneaded and disintegrated by a planetary high-speed mill. From the electron micrographs in Figs. 12 and 13, it is clear that the carbon nanotubes are uniformly and three-dimensionally attached to the titanium particle surface by kneading and disintegrating with a planetary high-speed mill.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and discharge plasma sintering was performed at 1400 ° C for 5 minutes. At that time, the heating rate was 100 ° C / Min, and a pressure of 20 MPa was first applied, and then a pressure of 60 MPa was continued.
- the thermal conductivity of the obtained composite material As a result of measuring the thermal conductivity of the obtained composite material, it was 50 W / mK when only the carbon nanotubes were previously subjected to the discharge plasma treatment, and was 30 W / mK without the discharge plasma treatment.
- the thermal conductivity of a solid obtained by spark plasma sintering of pure alumina powder alone under the above conditions was 25 W / mK.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus and subjected to a discharge plasma treatment at 575 ° C. for 5 minutes.
- the kneaded and dispersed material was subjected to discharge plasma sintering at 800 ° C. for 15 minutes in a discharge plasma sintering apparatus. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied.
- FIG. 14 shows an electron micrograph of the forced fracture surface of the obtained composite material.
- FIG. 14B shows an electron micrograph of the reticulated carbon nanotube when the scale shown in FIG. 14A with a scale of the order of 50 ⁇ is magnified to the order of ⁇ .
- FIGS. 16A and 16B show magnified electron micrographs on the order of ⁇ on the order of 500 nm on the copper particle surface shown in Fig. 15B after kneading and disintegration with a planetary high-speed mill. From the electron micrographs in Figs. 15 and 16, it is clear that the carbon nanotubes are uniformly and three-dimensionally attached to the copper particle surface by kneading and pulverizing with a planetary high-speed mill.
- Zirconia powder having an average particle diameter of 0.5 ⁇ manufactured by Sumitomo Osaka Cement Co.
- lwt% long-chain carbon nanotubes were dispersed in a planetary mill using a zirconia container.
- carbon nanotubes are blended, zirconia powders that have been sufficiently dispersed in advance are blended, and the powders are dried in a dry state without using a dispersing medium. Kneading and dispersing were performed using a combination of the minute unit and the rotation speed of the container.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and was plasma-solidified at 1200 ° C for 5 minutes. At that time, the heating rate was 100 ° C / Min, and the pressure of 50 MPa was continuously applied.
- the electrical resistivity of the composite material according to the present invention was found to be the electrical resistivity of the solidified body obtained by subjecting only the zirconia powder to discharge plasma sintering under the above conditions. About 72% (conductivity increased about 1.4 times).
- Zirconia powder having an average particle size of 0.5 ⁇ (Sumitomo Osaka Cement Co., Ltd.) and pre-loaded into the die of a discharge plasma sintering device, and subjected to discharge plasma treatment at 575 ° C for 5 minutes 0.05wt ⁇ 3 ⁇ 4 ⁇ 0.5wt % Of long-chain carbon nanotubes in a dry state in a planetary mill using a container made of zirconia, in a dry state without using dispersing media, kneading and dispersing by combining various minute units of 60 minutes or less and the rotation speed of the container. Was done.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus and subjected to a discharge plasma treatment at 575 ° C for 5 minutes. Thereafter, the kneaded dispersion material was subjected to discharge plasma sintering at 1350 ° C for 5 minutes in a discharge plasma sintering apparatus. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied.
- FIG. 9 shows an electron micrograph of the forced fracture surface of the obtained composite material.
- Fig. 7 ⁇ shows an electron micrograph of the reticulated carbon nanotube when the scale shown in Fig. 7 with a scale of ⁇ order is enlarged to the order of ⁇ . ⁇ .
- Figures 18A and 18B show electron micrographs of the zirconia particles before kneading and disintegration, and their enlarged electron micrographs on the order of 500 nm.
- Figures 19A and 19B show electron micrographs of the zirconium particles after kneading and disintegration with a planetary high-speed mill and enlarged electron micrographs on the order of 500 nm. From the electron micrographs in Figs. 18 to 19, it is clear that carbon nanotubes are uniformly and three-dimensionally attached to the surface of the zirconia particles by kneading and disintegrating with a planetary high-speed mill.
- Carbonized t, elemental powder having an average particle diameter of 0.3 ⁇ and long-chain carbon nanotubes of 2 wt% were dispersed in a planetary mill using an alumina container.
- carbon nanotubes are blended, silicon carbide powders that have been sufficiently dispersed in advance are blended, and these powders are dried in a dry state without using a dispersing medium. Kneading and dispersing were performed using a combination of hour and minute units and the rotation speed of the container.
- the kneading and dispersing material was charged into a die of a spark plasma sintering apparatus, and plasma-solidified at 1850 ° C for 5 minutes. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied.
- the electric resistivity of the composite material according to the present invention was compared with the electric resistivity of the solidified body obtained by discharge plasma sintering only the carbonized powder and the elementary powder under the above conditions.
- the resistivity was about 93% (the conductivity increased to about 1.08 times).
- Figures 20A and 20B show electron micrographs of carbonized L and elementary particles before kneading and disintegration, and their enlarged electron micrographs at 500 nm order.
- Figures 21 ⁇ and 21 ⁇ show electron micrographs of silicon carbide after being kneaded and disintegrated by a planetary high-speed mill and its enlarged electron micrographs on the order of 500 mn. From the electron micrographs of FIGS. 20 to 21, it is clear that the carbon nanotubes are uniformly and three-dimensionally attached to the silicon carbide surface by kneading and pulverizing with a planetary high-speed mill.
- Silicon carbide powder having an average particle diameter of 0.3 ⁇ and long-chain carbon nanotubes of 0.25 wt% were dispersed in a planetary mill using an alumina container.
- carbon nanotubes are blended, carbonized which has been sufficiently dispersed in advance, and raw powders are blended.
- the powders are dried in a dry state without using dispersing media for 2 hours or less in a dry state. Kneading and dispersing were carried out by combining various time and minute units and the rotation speed of the container.
- the kneading and dispersing material was charged into a die of a spark plasma sintering apparatus, and plasma-solidified at 1850 ° C for 5 minutes. At that time, the heating rate was 100 ° C / Min, and a pressure of 100 MPa was applied to open.
- Silicon nitride powder (Ube Industries, Ltd.) having an average particle diameter of 0.5 ⁇ and long-chain carbon nanotubes of 0.25 wt% were dispersed in a planetary mill using an alumina container. First, carbon nanotubes are blended, silicon nitride powder that has been sufficiently dispersed in advance is blended, and these powders are dried in a dry state without using a dispersing medium. And kneading and dispersing using a combination of the number of rotations of the container.
- the dried kneading and dispersing material is loaded into a die of a discharge plasma sintering apparatus,
- Plasma solidification was performed at 1500 ° C to 1600 ° C for 5 minutes. At that time, the heating rate is
- the temperature was set to 100 ° C / Min and 230 ° C / Min, and the pressure of 20 to 60 MPa was continuously applied.
- the electric conductivity of the obtained composite material was measured, it was 450 to 500 Siemens / m.
- a mixture of pure aluminum powder with an average particle size of ⁇ and alumina powder with an average particle size of 0.6 ⁇ (90 wt%) and long-chain carbon nanotubes (10 wt%) are packed in an alumina container. Dispersed in the used planetary mill. First, carbon nanotubes are combined, and a mixed powder of pure aluminum powder (95 wt%) and alumina powder (5 wt%), which has been sufficiently dispersed in advance, is blended, and these powders are dispersed in a dry state. Without using media, kneading and dispersing were performed in a dry state by combining various time and minute units of 2 hours or less and the number of rotations of the container.
- a nonionic surfactant Triton X-100, lwt% was added as a dispersant, and the mixture was wet-dispersed by applying ultrasonic waves for 2 hours or more. The resulting slurry was filtered and dried.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and was plasma-solidified at 500 ° C. to 600 ° C. for 5 minutes. At that time, the heating rates were 100 ° C / Min and 230 ° C / Min, and a pressure of 15 to 40 MPa was continuously applied. When the thermal conductivity of the obtained composite material was measured, it was 250 to 400 W / mK.
- a mixture of pure aluminum powder with an average particle size of ⁇ and alumina powder with an average particle size of 0.6 ⁇ (95 wt%, aluminum powder: alumina powder 95: 5) and a long-chain carbon nanotube ( 5 wt%) was dispersed in a planetary mill using an alumina container.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and was plasma-solidified at 500 ° C. to 600 ° C. for 5 minutes. At that time, the heating rates were 100 ° C / Min and 230 ° C / Min, and a pressure of 15 to 40 MPa was continuously applied. When the thermal conductivity of the obtained composite material was measured, it was 300 to 450 W / mK.
- a carbon nanotube is compounded, a mixed powder of oxygen-free copper powder and alumina powder, which have been sufficiently dispersed in advance, is mixed, and the powders are dried in a dry state without using a dispersion medium. In the dry state, kneading and dispersing were performed in combination of various time units of 2 hours or less and the rotation speed of the container.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus, and discharge plasma sintering was performed at 700 ° C to 900 ° C for 5 minutes. At that time, the heating rate was 250 ° C / Min and the pressure of lOMPa Continued to apply force. As a result of measuring the thermal conductivity of the obtained two types of composite materials, both became 500 to 800 W / mK.
- Stainless steel powder (SUS316L) with an average particle size of 20 ⁇ to 30 ⁇ and 0.5wt% long-chain carbon nanotubes are dried in a planetary mill using a stainless steel container without using dispersion media. The kneading and dispersing were performed by combining various time units of 2 hours or less and the rotation speed of the container.
- the kneading and dispersing material was loaded into a die of a discharge plasma sintering apparatus and subjected to a discharge plasma treatment at 575 ° C. for 5 minutes. Thereafter, the kneaded and dispersed material was subjected to discharge plasma sintering at 900 ° C for 10 minutes in a discharge plasma sintering apparatus. At that time, the heating rate was 100 ° C / Min, and the pressure of 60 MPa was continuously applied.
- the thermal conductivity of the obtained composite material was measured, and as a result, the composite material according to the present invention was about 18% Rose.
- the electrical resistivity of the solidified material obtained by spark plasma sintering only the stainless steel powder under the above conditions was compared with the electrical resistivity of the composite material according to the present invention.
- the electrical resistivity was about 60% (the conductivity increased to about 1.65 times).
- the carbon nanotube-dispersed composite material according to the present invention uses, for example, ceramic powder to produce an electrode material, a heating element, a wiring material, a heat exchanger, a fuel cell, etc. having excellent corrosion resistance and high temperature resistance. be able to.
- heat exchangers, heat sinks, fuel cell separators, and the like with excellent high thermal conductivity can be manufactured by using metal powders such as ceramic powders, aluminum alloys, and stainless steels.
Abstract
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Also Published As
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US20070057415A1 (en) | 2007-03-15 |
JP4593473B2 (ja) | 2010-12-08 |
JPWO2005040068A1 (ja) | 2007-03-08 |
JPWO2005040065A1 (ja) | 2007-03-01 |
WO2005040068A1 (ja) | 2005-05-06 |
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