WO2006120803A1 - Materiau composite extremement thermoconducteur - Google Patents

Materiau composite extremement thermoconducteur Download PDF

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Publication number
WO2006120803A1
WO2006120803A1 PCT/JP2006/305738 JP2006305738W WO2006120803A1 WO 2006120803 A1 WO2006120803 A1 WO 2006120803A1 JP 2006305738 W JP2006305738 W JP 2006305738W WO 2006120803 A1 WO2006120803 A1 WO 2006120803A1
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WIPO (PCT)
Prior art keywords
composite material
high thermal
fibrous carbon
conductive composite
thermal conductive
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PCT/JP2006/305738
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English (en)
Japanese (ja)
Inventor
Kazuaki Katagiri
Atsushi Kakitsuji
Toyohiro Sato
Terumitsu Imanishi
Akiyuki Shimizu
Katsuhiko Sasaki
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Sumitomo Precision Products Co., Ltd
Osaka Prefectural Government
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Application filed by Sumitomo Precision Products Co., Ltd, Osaka Prefectural Government filed Critical Sumitomo Precision Products Co., Ltd
Priority to JP2007526827A priority Critical patent/JP5288441B2/ja
Publication of WO2006120803A1 publication Critical patent/WO2006120803A1/fr

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Definitions

  • the present invention provides a fibrous form such as carbon nanotubes (CNT) and vapor-grown carbon fibers (VGCF) contained in a sintered body made of the powder.
  • CNT carbon nanotubes
  • VGCF vapor-grown carbon fibers
  • the present invention relates to a high thermal conductive composite material provided with excellent electrical conductivity, thermal conductivity, and strength characteristics by a carbon material, and a method for producing the same.
  • metal compounds (boride: TiB, WB, MoB, CrB, A1B2, MgB, carbide: WC, nitride: TiN, etc.) and car
  • Patent Document 2 There has been proposed a resin molded article that has both moldability and conductivity by blending an appropriate amount of bon nanotubes.
  • Patent Document 1 JP-A-2002-363716
  • Patent Document 2 JP 2003-34751 A
  • Patent Document 3 JP 2000-223004
  • the carbon nanotubes to be dispersed in the above-mentioned resin or aluminum alloy are used as short as possible in consideration of the manufacturability of the resulting composite material and obtaining the required formability. Therefore, the dispersibility is improved, and it is not intended to effectively utilize the excellent electrical and thermal conductivity characteristics of the carbon nanotube itself.
  • the present invention is a composite that has corrosion resistance, heat resistance, and has the characteristics of a metal material having versatility, ductility, etc. purely and imparts or improves electrical conductivity and thermal conductivity.
  • the metallic powder base material itself or ceramics to be further added, and the characteristics of the ceramic powder base material itself, as well as the excellent electrical conductivity inherent to the fibrous carbon material itself For the purpose of providing a high thermal conductive composite material that effectively utilizes thermal conductivity and strength properties and its manufacturing method!
  • the composite material similarly has high thermal conductivity and can be plastically deformed such as rolling.
  • the thermal conductivity is low and at the interface due to plastic deformation such as rolling. Delamination occurs and the function as a composite material is lost.
  • the high thermal conductive composite material of the present invention has been completed based on these findings, and is based on a metal powder, a mixed powder of metal and ceramic, or a discharge plasma sintered body having a ceramic powder force.
  • a fibrous carbon material such as an ultra-thin tubular structure composed of single-layer or multi-layer darafen is distributed and integrated in the base material.
  • Graphene is a marker composed of six carbon atoms arranged regularly in two dimensions. It is a net with a net structure and is also called a carbon hexagonal mesh surface, and this graphite layered with regularity is called a graphite.
  • the single-layer or multi-layered and ultrathin tube-like structure composed of darafen is a fibrous carbon material used in the present invention, and includes both single-bonn nanotubes and vapor-grown carbon fibers.
  • the carbon nanotube is a seamless tube in which graphene is rounded into a cylindrical shape, and there are a single-walled tube and a multi-walled tube that is concentrically stacked.
  • Single-walled ones are called single-walled nanotubes
  • multiple-walled ones are called multi-walled nanotubes.
  • Vapor-grown carbon fiber also has a single-layer or multiple-layer dalafen tube whose carbon is rounded into a cylindrical shape, that is, a carbon nanotube in the core, and the core is multi-layered and polygonal.
  • Graphite is stacked in the radial direction of the graphene tube so as to surround it, and it is also called super multi-walled carbon nanotube due to its structure.
  • the single-layer or multi-layer carbon tube present at the center of the vapor-grown carbon fiber is a carbon nanotube.
  • the method for producing the fibrous carbon material is not particularly limited! Although any of an arc discharge method, a laser evaporation method, a thermal decomposition method, a chemical vapor deposition method and the like may be used, the vapor grown carbon fiber is manufactured by a chemical vapor deposition method.
  • VGCF which stands for vapor growth carbon fiber, is an abbreviation for Vapor Growth Carbon Fiber.
  • the fibrous carbon material can be dispersed and contained in the base material, or it can be formed into a sheet and alternately laminated with the powder layer to constitute a laminate.
  • the fibrous carbon material can also be oriented in the substrate.
  • orientation There are two types of orientation, one is a three-dimensional orientation in which the fibrous carbon material is oriented in a specific position, and the other is oriented in a direction parallel to a specific plane.
  • Random two-dimensional orientation Non-orientation is a three-dimensional random form in which the fibrous carbon material is oriented in a random direction in three dimensions.
  • a sheet made of a fibrous carbon material can be easily oriented in the direction parallel to the surface, and can be easily oriented in the same direction. By the orientation of the fibrous carbon material, the thermal conductivity in the orientation direction can be improved in the carbon material-containing metal material.
  • the spark plasma sintered body can be subjected to plastic casing.
  • Plastic working eg rolling
  • the carbon nanotubes at the powder boundaries and grain boundaries are oriented by the repetitive stress caused by, and the self-organization is also promoted by dislocation accumulation.
  • the thermal conductivity may decrease due to plastic working.
  • one is a step of kneading and dispersing metal powder, mixed powder of metal and ceramic, or ceramic powder and fibrous carbon material. And a step of performing discharge plasma sintering of the kneaded dispersion material.
  • the other is a metal powder layer, a mixed powder layer of metal powder and ceramic powder, or a ceramic powder layer, and a fibrous shape.
  • the method includes a step of alternately laminating sheets made of a carbon material, and a step of spark plasma sintering the obtained laminate.
  • a high thermal conductive composite material in which a fibrous carbon material is dispersed and contained in a discharge plasma sintered body of a metal powder, a mixed powder of metal and ceramics, or a ceramic powder. Is manufactured.
  • the latter production method has a laminated structure in which sheets of fibrous carbon material are arranged at predetermined intervals in a discharge plasma sintered body of metal powder, mixed powder of metal and ceramics, or ceramic powder. High thermal conductivity composite materials are produced.
  • the fibrous carbon material dispersed in the spark plasma sintered body can be oriented in a specific direction.
  • the fibrous carbon material constituting the sheet can be oriented in a direction parallel to the sheet surface.
  • the fibrous carbon material may be oriented in the same direction within the plane as when it is random. As described above, the orientation of the fibrous carbon material improves the thermal conductivity in the orientation direction of the carbon material-containing metal material.
  • this orientation operation can be performed by orienting the fibrous carbon material in the kneaded dispersion material before sintering in a specific direction.
  • this orientation operation can be performed at the stage of producing a sheet of fibrous carbon material.
  • a method for orienting the fibrous carbon material in a predetermined direction a method of preparing a dispersion of the fibrous carbon material and solidifying the dispersion in a magnetic field or an electric field is simple and preferable for orientation.
  • An oriented sheet can also be produced by pushing down the fibrous carbon material in one direction over a planar fiber assembly in which the extremely short V and fibrous carbon material are gathered two-dimensionally in the radial direction.
  • the metal powder used in the present invention is versatile and versatile in which one or more of aluminum, aluminum alloy, titanium, titanium alloy, copper, copper alloy, and stainless steel are preferred. This makes it possible to produce industrial products having various properties and excellent characteristics.
  • the metal powder has an average particle size of 200 ⁇ m or less, and the ceramic powder has an average particle size of 10 m or less.
  • Ceramic powders include oxides such as alumina and zirconium, nitrides such as aluminum nitride, titanium nitride and silicon nitride, carbides such as silicon carbide, titanium carbide, tantalum carbide and tungsten carbide, and borides.
  • borides such as titanium, zirconium boride and chromium boride are preferred.
  • This ceramic powder can constitute a base material alone.
  • mixing with metal powder improves grain boundary sliding during rolling, making it possible to produce industrial products with various characteristics with excellent versatility and versatility.
  • the content of the fibrous carbon material is preferably 20 wt% or less by weight. This makes it possible to easily obtain the desired characteristics with excellent sinterability and ductility. However, when the carbon material-containing metal material is a laminated structure of a powder layer and a sheet-like carbon material, the content of 50 wt% or less is allowed unless plastic processing is required.
  • the weight ratio is 2 Owt% or less. Become.
  • Examples of plastic working include rolling, press forming, and the like, and the rolling may be any of cold rolling, warm rolling, and hot rolling. Annealing can be performed after the plastic cage. Select the most appropriate rolling method according to the ceramic species mixed with metal species, the type and amount of fibrous carbon material, etc., and further reduce the residual stress of the resulting metal material by annealing to further improve the rolling effect Thus, it becomes possible to easily obtain the desired characteristics.
  • the fibrous carbon material before blending into the substrate can be preliminarily subjected to a discharge plasma treatment, thereby significantly improving the uniform dispersibility of the fibrous carbon material in the metal substrate. It is out.
  • fibrous carbon materials are short, and the length of carbon nanotubes is several hundred ⁇ m.
  • the growth carbon fiber is at most 2 to 3 cm.
  • the fibers are usually connected to each other to form a long chain, and these fibers are entangled or further formed into a lump-like lump, or only the fibrous carbon material is subjected to a discharge plasma treatment.
  • the carbon nanotubes and the vapor-grown carbon fibers have been developed to be relatively long and straight, and the shape is not particularly limited.
  • the kneading and dispersing step it is important to unravel the lumps of fibrous carbon material that are intertwined like cocoons and mix them uniformly with the powder.
  • the dispersion may be wet-dispersed using a dispersant.
  • kneading and dispersing can be carried out efficiently to ensure uniform dispersion of the fibrous carbon material into the metal substrate.
  • a dispersion medium to rotate and knead and disperse the container containing the powder and fibrous carbon material, kneading and dispersing can be efficiently performed according to the metal species, the ceramic species to be mixed, and the amount of fibrous carbon material. Can be implemented.
  • the container containing the powder and the fibrous carbon material is rotated and kneaded and dispersed without using a dispersion medium, so that the kneading and dispersing are performed according to the metal species, the ceramic species to be mixed, and the amount of the fibrous carbon material. Can be implemented efficiently.
  • the two-stage process of performing low-temperature plasma discharge under low pressure and then performing low-temperature discharge plasma sintering under high pressure is a long-chain fibrous carbon material. It is effective to obtain a good sintered body while ensuring the dispersibility of the material.
  • the high thermal conductive composite material of the present invention uses a sintered body of a metal powder or a ceramic powder of pure aluminum, aluminum alloy, titanium or the like excellent in corrosion resistance and heat dissipation as a base.
  • the carbon nanotube itself has excellent electrical conductivity and heat by combining and integrating the fibrous carbon material. Combined with conduction characteristics and strength, the required properties can be enhanced, synergistic effects, or new functions can be exhibited.
  • the highly heat-conductive composite material of the present invention is obtained by obtaining a required shape material such as a metal powder sintered body plate, bar material, or block material containing a fibrous carbon material, and then pressing it into a required shape by press molding. Can be crafted. In addition, it is possible to obtain a form according to the intended use such as a thin wire rod by rolling.
  • the high thermal conductive composite material of the present invention can disperse, for example, ceramic powders such as alumina and zirconium oxide which are excellent in corrosion resistance and heat resistance when obtaining the above-mentioned sintered body.
  • the characteristics of the substrate and ceramics can be combined or synergized, such as corrosion, electrodes and heating elements in high temperature environments, wiring materials, heat exchangers with improved thermal conductivity, heat sink materials, brake components, or fuel. It can be applied as a battery electrode separator. Further, by dispersing fine particles such as silicon carbide and silicon nitride when obtaining the above-mentioned sintered body, the grain boundary sliding during plastic deformation is improved, and superplasticity can be exhibited.
  • pure aluminum, a known aluminum alloy, titanium, a titanium alloy, copper, a copper alloy, stainless steel, or the like can be used as the metal powder to be used.
  • a known functional metal capable of sintering and plastic deformation and exhibiting necessary functions such as corrosion resistance, thermal conductivity and heat resistance may be employed.
  • the particle size of the metal powder is approximately 100 m or less, more preferably 50 m or less, having a sinterability capable of forming a necessary sintered body and a pulverizing ability when kneading and dispersing with a fibrous carbon material. It is also possible to use large and small particle sizes that are preferred for particles with different particle sizes, and it is possible to adopt a configuration in which there are multiple powder types and different particle sizes. preferable. In addition to the spheres, the powders can be appropriately used in the form of fibers, indeterminate shapes, cocoons, and various forms. Aluminum and the like are preferably 50 m to 150 m.
  • ceramic powders used include oxides such as alumina and zirconium oxide, nitrides such as aluminum nitride, titanium nitride, and silicon nitride, silicon carbide, titanium carbide, tantalum carbide,
  • Use ceramics with various known mechanical functions such as carbides such as tungsten carbide, boride such as titanium boride, zirconium boride, and chromium boride, and a function that improves the intergranular sliding during plastic deformation. be able to.
  • a well-known functional ceramic that exhibits necessary functions such as corrosion resistance and heat resistance may be employed.
  • the particle size of the ceramic powder considering the sinterability capable of forming a necessary sintered body, considering the crushing ability when kneading and dispersing with carbon nanotubes, and the grain boundary during plastic deformation Decided considering the sliding ability, but about 10 m or less is preferable. It is also possible to adopt a configuration in which there are a plurality of powder types and different particle sizes. In the case of a single powder, it is preferably 5 ⁇ m or less, more preferably 1 ⁇ m or less. In addition to spheres, the powders can be used in a fibrous, indeterminate or various form as appropriate.
  • the content of the high thermal conductive composite material is not particularly limited as long as a sintered body having a required shape and strength can be formed.
  • the seed and particle size of the metal powder it is possible to contain, for example, 20 wt% or less by weight.
  • the content of fibrous carbon material is reduced to 3 wt% or less, and if necessary, to about 0.05 wt%. It is necessary to devise a dispersion method.
  • the ceramic content is 20 wt% or less by weight.
  • a method of producing a metal material containing a carbon material in which a fibrous carbon material is dispersed in a metal powder, a mixed powder of metal and ceramics, or a discharge plasma sintered body of a ceramic powder is provided.
  • a step of wet-dispersing the powder and the carbon nanotube using a dispersant that is, a step of preparing and solidifying a dispersion.
  • the long-chain fibrous carbon material described above is dispersed in ceramic powder, metal powder, or a mixed powder of ceramic and metal, and then loosened and crushed. is important.
  • various mills, crushers, and shaker devices for performing known crushing, crushing, and crushing can be used as appropriate, and the mechanisms are also rotary impact type, rotary shear type, rotary impact shear type, medium stirring type
  • Well-known mechanisms such as a stirring type, a stirring type without a stirring blade, and an airflow grinding type can be used as appropriate.
  • the ball mill has a misalignment structure as long as it is crushed and crushed using a medium such as a ball such as a known horizontal type, planetary type, or stirring type mill. Even available. Further, the material and particle size of the media can be appropriately selected. In the case where only the carbon nanotubes are preliminarily subjected to the discharge plasma treatment, it is necessary to set conditions for improving the crushing ability especially by selecting the powder particle size and the ball particle size.
  • the planetary mill is configured such that the rotation and revolution of the storage container are performed at the same time, and usually pulverized and crushed using a medium such as a ball.
  • a medium is used.
  • the wet-dispersing step is performed by adding a known nonionic dispersant or cationic anionic dispersant to the above-mentioned various mills and crashers including an ultrasonic dispersing device and a ball mill.
  • a known nonionic dispersant or cationic anionic dispersant to the above-mentioned various mills and crashers including an ultrasonic dispersing device and a ball mill.
  • the dispersion can be performed using a shaker device, and the dry dispersion time can be shortened and high efficiency can be achieved.
  • a known heat source or a spin method can be appropriately employed as a method of drying the slurry after the wet dispersion.
  • the kneading and dispersing step and the wet-dispersing step include a dry kneading dispersion followed by a wet dispersion, a wet dispersion followed by a dry kneading dispersion, or a dry, wet, dry
  • Various kneading and dispersing process patterns such as combining with can be employed.
  • the carbon nanotubes and ceramics can be kneaded and dispersed first, and then the metal powder can be kneaded and dispersed, or the kneading and dispersing can be repeated for each particle size of the powder.
  • a fibrous carbon material and ceramics are first wet-kneaded and dispersed, and then dried into a metal powder.
  • Various kneading and dispersing process patterns such as dry kneading and dispersing can be adopted.
  • the step of orienting the fibrous carbon material in the kneading dispersion material uses, for example, the above-described wet dispersion step. Specifically, a dispersion liquid of a mixed dispersion material in which a fibrous carbon material is mixed and dispersed in a metal powder, a mixed powder of metal and ceramics, or a ceramic powder is prepared. Gelatin etc. are blended in the dispersion as a binder for solidification. This dispersion is placed in a strong magnetic field of 3000 gauss in a solution state (heated state) and solidified by cooling. A strong magnetic field of 3000 gauss can be formed by neodymium iron boron magnets.
  • a mixed powder solid in which the fibrous carbon material is dispersed in the metal powder, the mixed powder of metal and ceramics, or in the ceramic powder, and the fibrous carbon material is oriented in a specific direction. It is formed.
  • an electric field can be used.
  • a method of applying a magnetic field or an electric field using a dispersion liquid can be similarly used.
  • physical methods such as placing the dispersion in an injection machine such as a syringe and pushing out several rows in one direction, flowing the dispersion on a standing plate, and immersing the plate in the dispersion
  • a sheet in which the fibrous carbon material is oriented in a specific direction can be formed by any method.
  • a dry kneaded dispersion powder or solid is loaded between a carbon die and a punch, and is added by upper and lower punches.
  • Compressive force Joule heat is generated in the die, punch, and material to be processed by applying a direct current pulse current, and the kneaded dispersion material is sintered.
  • a pulse current powder, powder, and fiber are sintered. Sintering proceeds smoothly by actions such as the generation of discharge plasma between the carbonaceous materials, the disappearance of powder and impurities on the surface of the fibrous carbon materials, and the like.
  • the discharge plasma treatment conditions to be applied only to the fibrous carbon material are not particularly limited.
  • the temperature is 200 to 1400 ° C
  • the time is about 1 to 2 hours
  • the pressure is 0 to: the range of LOMPa. can do.
  • the knead-dispersed material obtained by the dry method or the wet method or both is further subjected to a discharge plasma treatment. This step is performed before the spark plasma sintering step, and the kneading and dispersing material is further crushed, and effects such as carbon nanotube stretching, surface activation, and powder diffusion occur. As the discharge plasma sintering proceeds smoothly, the thermal conductivity and conductivity imparted to the sintered body are improved.
  • the discharge plasma treatment conditions for the kneaded dispersion are not particularly limited, but considering the sintering temperature of the material to be treated, for example, the temperature is 200 to 1400 ° C, and the time is 1 to 15 minutes.
  • the degree and pressure are 0 to:
  • the range of LOMPa can be selected as appropriate.
  • the discharge plasma sintering is preferably performed at a temperature lower than the normal sintering temperature of the ceramic powder or metal powder to be used.
  • a low temperature plasma discharge is performed under a low pressure, and then a low temperature discharge plasma sintering is performed under a high pressure. It is also preferable to do. It is also possible to use precipitation hardening after sintering and phase transformation by various heat treatments. Note that the pressure and temperature levels are relative between the two processes, and it is sufficient if a difference in height can be set between the two processes!
  • the step of plastically deforming the obtained discharge plasma sintered body which is one of the characteristics of the present invention, includes any known rolling method, any rolling method of cold rolling, warm rolling, and hot rolling. It may be.
  • the optimum rolling method is selected according to the metal type of the sintered metal, the type of ceramic to be mixed, and the amount of fibrous carbon material. Further, when performing multiple passes of rolling, for example, cold rolling and warm rolling can be combined.
  • Cold rolling is a process in which the obtained block-like, plate-like, and linear-shaped sintered bodies are rolled as they are, and a plate material or a thin plate having a required thickness by repeating one pass to a plurality of passes at a required reduction ratio.
  • the rolling reduction ratio, total rolling reduction ratio, rolling roll diameter, etc. are appropriately selected so that cracks do not occur in the rolled material depending on the metal species, the ceramic species to be mixed and the amount of fibrous carbon material! .
  • Warm or hot press forming or rolling can be appropriately selected according to the required form and material, for example, cold rolling is not easy depending on the properties of the sintered metal! ! Can be used for the purpose of improving rolling efficiency.
  • the heating temperature of the material is appropriately selected in consideration of the rolling reduction ratio, total rolling reduction ratio, number of passes, and rolling roll diameter.
  • the annealing process after press molding and rolling is performed as necessary.
  • an optimal rolling method and combination according to the metal species, the ceramic species to be mixed, and the amount of carbon nanotubes, The rolling conditions are selected, but the selected rolling method, combination, rolling conditions, etc., for the purpose of further improving the rolling effect by reducing the residual stress of the rolled metal material and easily obtaining the required characteristics, etc.
  • the annealing time, temperature conditions, number of times, etc. are selected accordingly.
  • the metal material of the present invention that has been plastically deformed or plastically deformed and annealed is easy to machine, can be processed into various shapes according to the intended use and form, and further processed metal material. It is also possible to join different materials with a brazing material or the like.
  • seat of a fibrous carbon material is produced first.
  • a sheet is made from a cocoon by unraveling a lump of fibers that have been strengthened in a cocoon shape, making a dispersion thereof, and solidifying it thinly.
  • the fibers can be oriented by applying a magnetic field or an electric field to the dispersion.
  • the kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and subjected to discharge plasma sintering at 575 ° C for 60 minutes. At that time, the rate of temperature increase was 100 ° C / min, and a 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 about 200 WZmK (198 W / mK). Note that the thermal conductivity of the solidified body obtained by subjecting only the aluminum alloy powder to spark plasma sintering under the above conditions was 157 WZmK, and the thermal conductivity of the composite material according to the present invention increased by about 21%. I understand.
  • Example 1 Average particle size 30
  • the kneaded dispersion 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 was sintered in a discharge plasma sintering apparatus at 600 ° C. for 5 minutes. At that time, the rate of temperature rise was set to 100 ° CZmin, and a pressure of 50 MPa was continuously applied.
  • Example 1 3 In kneading and pulverization of aluminum powder having an average particle diameter of 30 ⁇ m and 0.25 wt% long-chain carbon nanotubes, only the carbon nanotubes were previously contained in the die of the discharge plasma sintering apparatus.
  • the kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and subjected to discharge plasma treatment at 400 ° C for 5 minutes. Thereafter, the kneaded dispersion was sintered in a discharge plasma sintering apparatus at 600 ° C. for 5 minutes.
  • FIG. 5 shows an electron micrograph of the forced fracture surface of the obtained composite material.
  • Fig. 5B shows an electron micrograph of a net-like carbon nanotube when the scale of Fig. 5A with an order of 100 m is expanded to the order of 5.0 m.
  • FIGS. 6A and 6B show electron micrographs of the aluminum particles before kneading and crushing.
  • FIG. 7A shows an electron micrograph of the aluminum particles after kneading and pulverizing with a planetary high-speed mill
  • FIG. 7B shows an enlarged electron micrograph of the concave portion shown in FIG. 7A on the order of 10 m.
  • enlarged electron micrographs of the 1 ⁇ m order and 500 nm order of the recesses shown in FIG. 7A are shown in FIGS. 8A and 8B.
  • 9A, 9B, and 10 show enlarged electron micrographs of the smoothed portion shown in FIG. 7A on the order of 10 m, 1 m, and 500 nm.
  • the obtained spark plasma sintered body was a short cylindrical body having a height of 10 mm and an outer diameter of 60 mm. This was cold-rolled in two passes until the thickness reached 1 mm.
  • Fig. 1A shows a state photograph after rolling of an aluminum sintered body containing 0.05 wt% of carbon nanotubes
  • Fig. 1B shows an enlarged electron micrograph of a 2 m order structure of the rolled structure. It is clear that good rolling was achieved with the metal materials of the examples.
  • the production method is the same as in Example 2-1, except that the sintered material was rolled under different rolling conditions (rolling direction), and the carbon nanotube content was 0.05 wt%, 0.5 wt%, 0.25 wt%.
  • Four types of rolled metal materials of samples R2, R3, R4, and R5 with%, 0.25 wt%, and 0.25 wt% were prepared.
  • the test pieces shown in Fig. 2 were cut out from the four types of samples R2, R3, R4, and R5 with different production conditions by aligning the test piece axes in the rolling direction and width direction, and subscripting symbols T and L, respectively. .
  • Example 2-3 The four types of rolled metal materials R2, R3, R4, and R5 manufactured in Example 2-2 were annealed at a temperature of 400 ° C. for 1 hour.
  • the maximum stress due to annealing was compared with the stress-strain relationship for the specimens without annealing in Fig. 3 in the rolling direction and width direction as shown in Fig. 4. It can be seen that it has decreased and the overall growth has increased. This is thought to be because the residual stress / strain produced during rolling was recovered by annealing.
  • sample R2 having a low carbon nanotube content is significantly increased by annealing.
  • sample R3 with a high content does not show a large difference before and after annealing. In other words, it is considered that the smaller the content, the larger the rate of increase in total elongation due to annealing.
  • Pure titanium powder with an average particle size of 10 to 20 m and 0.1 to 0.25 wt% long-chain carbon nanotubes (CNTs) are used in a planetary mill using a titanium container and dispersed media is used. Without mixing, kneading dispersion was performed by combining various time units of 2 hours or less and the rotation speed of the container in a dry state.
  • CNTs carbon nanotubes
  • the obtained kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and subjected to discharge plasma sintering at 900 ° C for 10 minutes. At that time, the rate of temperature increase was 100 ° C / min, and a pressure of 60 MPa was continuously applied.
  • FIG. 11 shows an electron micrograph of the forced fracture surface of the obtained composite material (CNT: 0.25 wt% added).
  • FIG. 11B shows an electron micrograph of the net-like carbon nanotubes when FIG. 11A with a scale of 10 / z m order is enlarged to 1.0 m order.
  • thermal conductivity of the obtained composite material As a result of measuring the thermal conductivity of the obtained composite material, it was 18.4 WZmK.
  • the thermal conductivity of the solidified body obtained by spark plasma sintering of pure titanium powder only under the above conditions was 13.8 WZmK, and the thermal conductivity of the composite material according to the present invention increased by about 30%. I understand.
  • the kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and subjected to discharge plasma sintering at 900 ° C for 10 minutes. At that time, the rate of temperature increase was 100 ° C / min, and a pressure of 60 MPa was continuously applied. As a result of measuring the thermal conductivity of the obtained composite material, it was 17.2 WZmK when only the carbon nanotube was previously subjected to the discharge plasma treatment.
  • FIGS. 12A and 12B show electron micrographs of titanium particles before kneading and crushing and titanium particles after kneading and crushing with a planetary high-speed mill.
  • Fig. 13A and Fig. 13B show magnified electron micrographs of the 1 m order and 500 nm order of the titanium particle surface shown in Fig. 12B after kneading and crushing with a planetary high-speed mill. From the electron micrographs in Figs. 12 to 13, the carbon nanotubes are evenly and standing on the surface of the titanium particles by kneading and crushing with a planetary high-speed mill. It is clear that they are physically and vertically attached.
  • a spark plasma titanium sintered body having a carbon nanotube content of 0.05 wt%, 0.25 wt%, and 0.5 wt% obtained in Example 3-2 is a short cylinder having a height of 10 mm and an outer diameter of 60 mm. Met. This was cold-rolled for 4 passes until the thickness reached 8 mm. When the sintered state of the titanium sintered body and the structure after rolling were observed with an electron microscope in the order of 1 to 5 ⁇ m, it was confirmed that the metal material of the example achieved good rolling.
  • An oxygen-free copper powder (Mitsui Metal atomized powder) with an average particle size of 20-30 m and 0.5 wt% long-chain carbon nanotubes in a planetary mill using a stainless steel container, using dispersion media Without mixing, kneading dispersion was performed by combining various time units of 2 hours or less and the rotation speed of the container in a dry state.
  • the kneaded dispersion 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. After that, the kneading dispersion material is 800 in a spark plasma sintering apparatus. C, spark plasma sintering for 15 minutes. At that time, the temperature rising rate was 100 ° CZmin, and a 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 a net-like carbon nanotube when the scale of Fig. 14A is enlarged to the order of 1.0 ⁇ m.
  • FIGS. Fig. 16A and Fig. 16B show the enlarged electron micrographs of the 1 m order and 500 nm order of the copper particle surface shown in Fig. 15B after kneading and crushing with a planetary high-speed mill. From the electron micrographs in Figs. 15 to 16, carbon nanotubes are evenly and three-dimensionally and vertically attached to the copper particle surface by kneading and crushing with a planetary high-speed mill. It is clear that he is wearing.
  • the discharge plasma copper sintered body having a carbon nanotube content of 0.5 wt% obtained in Example 41 was a short cylinder having a height of 10 mm and an outer diameter of 60 mm. This was cold-rolled for 3 passes until the thickness reached 8 mm. When the state of the copper sintered body after rolling and the structure after rolling were observed with an electron microscope in the order of 1 to 5 m, it was confirmed that the metal material of the example achieved good rolling.
  • the kneaded and dispersed 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 kneading dispersion material is 900 in a spark plasma sintering apparatus. C, spark plasma sintering for 10 minutes. At that time, the rate of temperature rise was 100 ° CZmin, and a pressure of 60 MPa was continuously applied.
  • the composite material according to the present invention has a thermal conductivity of only about stainless steel powder obtained by spark plasma sintering under the above conditions. Increased by 18%.
  • the electrical resistivity of the solidified body obtained by spark plasma sintering of only the stainless steel powder under the above conditions was compared with that of the present invention.
  • the electrical resistivity of the composite material was approximately 60% (conductivity increased approximately 1.65 times).
  • Example 6-1 The discharge plasma SUS sintered body having a carbon nanotube content of 0.5 wt% obtained in Example 5-1 was a short cylindrical body having a height of 10 mm and an outer diameter of 60 mm. This was cold-rolled for 5 passes until the thickness reached 8 mm. The state of the SUS sintered body after rolling and the structure after rolling were observed with an electron microscope in the order of 1 to 5 ⁇ m. As a result, it was confirmed that the metal material of the example achieved good rolling. [0106] Example 6-1
  • a mixture of pure aluminum powder with an average particle size of 100 ⁇ m and alumina powder with an average particle size of 0.6 ⁇ m (95 wt%, aluminum powder: alumina powder 95; 5) Carbon nanotubes (5 wt%) were dispersed in a planetary mill using an alumina container.
  • the kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus, and plasma solidified at 500 to 600 ° C for 7 minutes. At that time, the rate of temperature increase was 100 ° CZmin and 230 ° CZmin, and a pressure of 14-40 MPa was continuously applied. When the thermal conductivity of the obtained composite material was measured, it was 300 to 450 WZmK.
  • the spark plasma metal composite sintered body having a carbon nanotube content of 0.5 wt% obtained by the same method as in Example 6-1 was a short cylindrical body having a height of 10 mm and an outer diameter of 60 mm. This was cold-rolled for 5 passes until the thickness reached 8 mm. The state of the sintered body after rolling and the structure after rolling were observed with an electron microscope on the order of 1 to 5 ⁇ m. As a result, it was confirmed that the metal material of the example achieved good rolling.
  • a mixed powder of oxygen-free copper powder (Mitsui Metal atomized powder) with an average particle diameter of 50 ⁇ m and alumina powder with an average particle diameter of 0.6 ⁇ , and 10 wt% long-chain carbon nanotubes It was dispersed with a planetary mill using a vessel made of stainless steel. First, carbon nanotubes are combined, and a mixed powder of oxygen-free copper powder and alumina powder that has been sufficiently dispersed in advance is blended, and these powders are in a dry state without using a dispersion medium. Then, kneading and dispersion were performed by combining various time units of 2 hours or less and the rotation speed of the container.
  • the kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and subjected to discharge plasma sintering at 700 to 900 ° C for 5 minutes. At that time, the temperature rising rate is 250 ° CZmin, and lOMPa pressure is applied. Continued to add. As a result of measuring the thermal conductivity of the two types of composite materials obtained, both were 500-8 OOWZmK.
  • the discharge plasma metal composite sintered body having a carbon nanotube content of 0.5 wt% obtained by the same method as in Example 7-1 was a short cylinder having a height of 10 mm and an outer diameter of 60 mm. This was cold-rolled for 8 passes until the thickness reached 8 mm. The state of the sintered body after rolling and the structure after rolling were observed with an electron microscope on the order of 1 to 5 ⁇ m. As a result, it was confirmed that the metal material of the example achieved good rolling.
  • the content of the fibrous carbon material was varied in the range of 2.5 wt% or more and 30 wt% or less by adjusting the adhesion amount of the aluminum powder adhered to both surfaces of the circular sheet. That is, by increasing the adhesion amount of the aluminum powder, the content of the fibrous carbon material is reduced, and the number of laminated circular sheets in the cylindrical laminate is also reduced. On the other hand, by reducing the adhesion amount of the aluminum powder, the content of the fibrous carbon material is increased, and the number of laminated circular sheets in the cylindrical laminate is increased. As a result, the number of stacked circular sheets in the columnar laminate changed in the range of about 100 to 250 sheets. When stacking circular sheets, care was taken that the fiber orientation direction was the same.
  • the manufactured composite material had a diameter of 10 mm and a height of about 11 to 12 mm due to shrinkage during the pressure sintering process.
  • the fibers in the carbon fiber layer are parallel to the layer surface (perpendicular to the center line of the composite material) and oriented in the same direction.
  • a disk-shaped specimen was taken in the direction perpendicular to the composite material force.
  • the test piece has a diameter of 10 mm and a thickness of 2 to 3 mm.
  • the center line of the test piece is perpendicular to the center line of the composite material and coincides with the fiber orientation direction in the fiber layer. That is, in each test piece, the fiber layer force parallel to the center line is laminated at a predetermined interval in a direction perpendicular to the center line, and the fiber orientation direction in each fiber layer coincides with the center line direction of the test piece. It is.
  • A1-Si alloy powder containing lwt% of silicon powder in aluminum powder was used as the metal powder.
  • the composite material manufactured in this example has vapor-grown carbon fibers oriented in one direction as a fibrous carbon material, surpassing the thermal conductivity of aluminum at a practical level at all fiber contents, The thermal conductivity tends to increase as the fiber content increases, with a maximum of 600 WZm A result exceeding K is obtained.
  • Example 8 in order to measure the thermal conductivity in the fiber orientation direction, a composite material having a multilayer structure in which a large number of fiber sheets were laminated was manufactured. In many cases, a small number of sheets such as one or several sheets are laminated. Thin composite materials with a small number of laminated fiber sheets are more versatile. Use value is also great. The same applies to the following embodiments.
  • Example 8 a composite material with a fibrous carbon material content of 2.5 wt% was manufactured as a cylindrical rolling test composite material with a diameter of 60 mm and a height of 10 mm. did.
  • the manufacturing method is the same as in Example 8.
  • carbon fiber layers perpendicular to the center line are laminated in layers at predetermined intervals in the center line direction in the cylindrical aluminum powder sintered body.
  • the fibers in the carbon fiber layer are oriented in the same direction.
  • the produced cylindrical composite material having a height of 60 mm was rolled in the fiber orientation direction in the carbon fiber layer until the thickness became 1 mm.
  • a 25 mm square sample was taken from a lmm thick plate after rolling, with two parallel sides parallel to the rolling direction (fiber orientation direction) and the other two parallel sides perpendicular to the rolling direction (fiber orientation direction).
  • the thermal conductivity of the sample was measured in two directions, the direction perpendicular to the rolling direction (fiber orientation direction) and the rolling direction (fiber orientation direction).
  • the thermal conductivity in the rolling direction was 237 WZmK, and the thermal conductivity in the direction perpendicular to the rolling direction (fiber orientation direction) was 212 WZmK.
  • the thermal conductivity in the fiber orientation direction before rolling is about 330 WZmK, which exceeds 300 WZmK.
  • the thermal conductivity after rolling surpasses the thermal conductivity of aluminum at the practical level and is in a direction perpendicular to the fiber orientation direction. Even the thermal conductivity surpasses that of aluminum at this practical level.
  • Lumps of vapor-grown carbon fibers with a length of 2 to 3 mm that were entangled were loosened with a shaker mill and separated.
  • Aluminum powder was mixed in the shaker mill, and both were kneaded. Both The mixing ratio was adjusted so that the content of the vapor-grown carbon fiber varied in the range of 2.5 to 15 wt%.
  • Example 8 In the same manner as in Example 8, the obtained powdered kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and pressurized in the height direction. In this state, the knead-dispersed material in the die was subjected to spark plasma sintering under conditions of 575 ° C ⁇ 60 minutes. At that time, the temperature rising rate was 100 ° CZmin, and the pressure of 50 MPa was continuously applied. As a result, a composite material of aluminum and fibrous carbon material in which the fibrous carbon material was uniformly dispersed in a cylindrical aluminum powder sintered body having a diameter of 10 mm and a height of l to 12 mm was produced.
  • Vapor-grown carbon fibers in the kneaded and dispersed material fall sideways by compression in the height direction of the kneaded and dispersed material in the die of the spark plasma sintering apparatus. There are various ways to fall. For this reason, in the manufactured composite material, the vapor-grown carbon fiber is not oriented, but tends to be oriented along a plane perpendicular to the center line. In other words, the vapor-grown carbon fiber in the composite material does not have a high degree of orientation but exhibits a two-dimensional orientation along a plane perpendicular to the center line.
  • the specimen has a diameter of 10 mm and a thickness of 2 to 3 mm.
  • the center line of the specimen is perpendicular to the center line of the composite material.
  • the thermal conductivity in the center line direction of the test piece was measured. The results are indicated by X in Figure 17.
  • ⁇ in FIG. 17 represents an average value of the thermal conductivity of a plurality of composite materials produced for each content of the fibrous carbon material.
  • Examples 8 to 10 are production examples of fiber-oriented composite materials using vapor-grown carbon fibers as fibrous carbon materials.
  • Examples 1 to 7 use carbon nanotubes as fibrous carbon materials, and all are production examples of fiber non-oriented composite materials. is there. Therefore, in this example, an example of manufacturing a fiber-oriented composite material using carbon nanotubes as a fibrous carbon material is shown.
  • a carbon nanotube assembly sheet with a thickness of several nanometers / zm is prepared by two-dimensionally closely gathering linear carbon nanotubes with a length of several ⁇ m in the radial direction. did. A number of carbon nanotubes in the carbon nanotube aggregate sheet were pushed down in one direction by a roller to produce a thin fiber sheet in which the carbon nanotubes were oriented in one specific direction parallel to the surface.
  • a large number of circular fiber sheets having a diameter of 10 mm were punched from this fiber sheet. While attaching aluminum powder with an average particle size of 30 m as metal powder to both sides of these circular fiber sheets, circular sheets are laminated in the thickness direction to produce a cylindrical laminate with a diameter of 10 mm x height of 20 mm. did. At this time, the content of carbon nanotubes was adjusted to 1.5 wt% by adjusting the amount of aluminum powder adhered to both surfaces of the circular sheet. When stacking circular sheets, care was taken that the fiber orientation direction was the same.
  • the produced cylindrical laminate was loaded into a die of a discharge plasma sintering apparatus and pressurized in the height direction. This compressed the cylindrical stack in the die to a height of approximately 15 mm.
  • the cylindrical laminate in the die was spark plasma sintered at 575 ° C. for 60 minutes. At that time, the temperature rising rate was 100 ° CZmin, and the pressure of 50 MPa was continuously applied.
  • the produced composite material had a diameter of 10 mm and a height of about 11 to 12 mm due to shrinkage during the pressure sintering process.
  • the fibers in the carbon fiber layer are carbon nanotubes, and they are oriented in the same direction and parallel to the layer surface (perpendicular to the center line of the composite material).
  • a disk-shaped test piece was taken in the direction perpendicular to the composite material force.
  • the test piece has a diameter of 10 mm and a thickness of 2 to 3 mm.
  • the center line of the test piece is perpendicular to the center line of the composite material and coincides with the fiber orientation direction in the fiber layer. That is, in each test piece, the fiber layer force parallel to the center line is laminated at a predetermined interval in a direction perpendicular to the center line, and the fiber orientation direction in each fiber layer is the center line of the test piece. It is consistent with the direction.
  • the thermal conductivity of the test piece was measured in the center line direction, that is, the fiber orientation direction. The results are indicated by ⁇ in FIG.
  • This carbon nanotube-oriented composite material showed a thermal conductivity of 274 WZmK when the carbon nanotube content was 1.5 wt%.
  • the performance is comparable.
  • high-quality linear carbon nanotubes are very expensive at present, and considering the cost performance, the use of vapor-grown carbon fibers is not comprehensive. Meaningful.
  • a non-oriented type composite material was manufactured using a linear high quality carbon nanotube having a length of several meters as the fibrous carbon material. Specifically, aluminum powder having an average particle diameter of 30 ⁇ m and linear carbon nanotubes having a length of several ⁇ m were kneaded by a shaker mill. The carbon nanotube content was 0.5 wt%.
  • the obtained powdery kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus and pressurized in the height direction.
  • the kneaded dispersion material in the die was subjected to spark plasma sintering under the condition of 575 ° C. ⁇ 60 minutes.
  • the rate of temperature increase was 100 ° C / min, and a pressure of 50 MPa was continuously applied. This produced a disc-shaped composite material with a diameter of 10 mm and a height of 2-3.
  • the carbon nanotubes are uniformly dispersed in the disc-shaped aluminum powder sintered body. Since carbon nanotubes are very short, orientation does not substantially occur even when subjected to compression in the center line direction. For this reason, a thin disc-shaped composite material (diameter 10 mm x thickness 2 to 3 mm) with a size for measuring thermal conductivity was directly manufactured. The thermal conductivity in the direction of the center line was 240 WZmK as shown by ⁇ in FIG. 17 (the black circle in the center). Considering that the carbon nanotube content is 0.5 wt%, this performance is good.
  • the substrate is a metal powder sintered body or a mixed powder sintered body of metal and ceramics.
  • a composite material of a ceramic base material and a vapor growth fiber was manufactured.
  • the obtained powdery kneaded dispersion was loaded into a die of a discharge plasma sintering apparatus in the same manner as in Example 8 and Example 10, and pressurized in the height direction.
  • the kneaded dispersion material in the die was subjected to spark plasma sintering under the condition of 1400 ° C. ⁇ 3 minutes.
  • the temperature rising rate was 100 ° CZmin, and the pressure of 30 MPa was continuously applied.
  • a composite material of alumina and fibrous carbon material in which vapor-grown carbon fibers were uniformly dispersed in a cylindrical alumina powder sintered body having a diameter of 10 mm and a height of l to 12 mm was produced.
  • the vapor-grown carbon fibers in the kneaded and dispersed material fall sideways due to the compression in the height direction of the kneaded and dispersed material in the die of the discharge plasma sintering apparatus. There are various ways to fall. For this reason, in the manufactured composite material, the vapor-grown carbon fiber is not oriented, but tends to be oriented along a plane perpendicular to the center line. In other words, the vapor-grown carbon fiber in the composite material does not have a high degree of orientation but exhibits a two-dimensional orientation along a plane perpendicular to the center line.
  • Example 8 and Example 10 Thereafter, in the same manner as in Example 8 and Example 10, a disk-shaped test piece was collected from the composite material in the orthogonal direction.
  • the specimen has a diameter of 10 mm and a thickness of 2-3 mm, and the specimen centerline is perpendicular to the composite centerline.
  • the measured thermal conductivity in the direction of the center line of the test piece was 243 WZmK. Since the thermal conductivity of the sintered alumina powder itself is about 25 W ZmK, the composite with the fibrous carbon material increased the thermal conductivity by about 10 times. The performance is not inferior even in comparison.
  • a composite material using carbon fiber as a fibrous carbon material was manufactured.
  • the manufacturing method was the same as in Example 10. In other words, a lump of entangled carbon fiber was loosened with a shaker mill and separated. Aluminum powder was mixed in the shaker mill, and both were kneaded. The carbon fiber content was 15 wt%.
  • the obtained powdery kneading dispersion was treated with a discharge plasma sintering apparatus in the same manner as in Examples 8 and 10.
  • a discharge plasma sintering apparatus in the same manner as in Examples 8 and 10.
  • the kneaded dispersion material in the die was subjected to spark plasma sintering under conditions of 575 ° C. X 60 minutes.
  • the rate of temperature increase was 100 ° CZmin, and the pressure of 5 OMPa was continuously applied.
  • a composite material of aluminum and fibrous carbon material was produced in which carbon fibers were uniformly dispersed in a cylindrical aluminum powder sintered body having a diameter of 10 mm and a height of ll to 12 mm.
  • the carbon fiber in the kneaded dispersion falls down sideways due to the compression in the height direction of the kneaded dispersion in the die of the spark plasma sintering apparatus. For this reason, the carbon fiber in the manufactured composite material does not have a high degree of orientation, but exhibits a two-dimensional orientation along a plane perpendicular to the center line.
  • the thermal conductivity was 208WZmK.
  • the thermal conductivity is about 350 WZmK.
  • the fibrous carbon material used in the present invention is far superior to carbon fiber as a contained material in the composite material.
  • the high thermal conductive composite material of the present invention can produce a heat exchanger, a heat sink, a fuel cell separator, etc. excellent in high thermal conductivity using metal powder such as aluminum alloy and stainless steel, Furthermore, electrode materials, heating elements, wiring materials, heat exchangers, fuel cells, etc. with excellent corrosion resistance and high temperature resistance characteristics can be manufactured using metal powder and ceramic powder.
  • FIG. 1A is a state photograph after rolling of an aluminum sintered body containing carbon nanotubes in a dispersed manner
  • FIG. 1B is an enlarged electron micrograph of a 2 m order yarn and weave after rolling. .
  • FIG. 2 (a) to (d) show the test piece cutouts of four types of rolled metal materials R2, R3, R4, and R5.
  • FIG. 1 (a) to (d) show the test piece cutouts of four types of rolled metal materials R2, R3, R4, and R5.
  • FIG. 3 (a) to (d) are graphs showing the stress-strain relationship for each of the four types of rolled metal materials R2, R3, R4, and R5 (without annealing).
  • FIG. 4 (a) to (d) are graphs showing the stress-strain relationship for each of the four types of rolled metal materials R2, R3, R4, and R5 (with annealing).
  • FIG. 5A is an electron micrograph of a forced fracture surface of a carbon nanotube-dispersed composite material using aluminum as a 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 pulverization.
  • FIG. 6A shows a scaler on the order of 20 ⁇ m
  • FIG. 6B shows an order on the order of 10 m.
  • Fig. 7 is an electron micrograph of aluminum particles after kneading and pulverization.
  • Fig. 7A is an enlarged electron with a scale of the order of 30 ⁇ m
  • Fig. 7B is an enlarged electron with an order of 10 ⁇ m of the recess shown in Fig. 7A.
  • FIG. 7A is an electron micrograph of aluminum particles after kneading and pulverization.
  • Fig. 7A is an enlarged electron with a scale of the order of 30 ⁇ m
  • Fig. 7B is an enlarged electron with an order of 10 ⁇ m of the recess shown in Fig. 7A.
  • FIG. 8A is an enlarged electron micrograph of 1 m order of the recess shown in FIG. 7A
  • FIG. 8B is an enlarged electron micrograph of the order of 500 nm.
  • FIG. 9A is an enlarged electron micrograph of the smooth portion shown in FIG. 7A on the order of 10 m
  • FIG. 9B is an enlarged electron micrograph of the order of 1 ⁇ m.
  • FIG. 10 is an enlarged electron micrograph of the smooth part shown in FIG. 7A on the order of 500 nm.
  • FIG. 11A is an electron micrograph of a forced fracture surface of a 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 crushing
  • FIG. 12B is an electron micrograph of titanium particles after kneading and crushing.
  • FIG. 13A is an enlarged electron micrograph of the order of 1 m of the titanium particle surface shown in FIG. 12B
  • FIG. 13B is an enlarged electron micrograph of the order of 500 nm.
  • FIG. 14A is an electron micrograph of a forced fracture surface of a 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 copper particles before kneading and pulverization
  • FIG. 15A shows a scale of 10 ⁇ m order
  • FIG. 15B shows a order of 50 ⁇ m.
  • FIG. 16A is an enlarged electron micrograph of the L m order on the copper particle surface after kneading and pulverization
  • FIG. 16B is an enlarged electron micrograph of the order of 500 nm.
  • Fig. 17 is a graph showing the relationship between the carbon material content and the thermal conductivity in a composite material of aluminum and carbon material.

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Abstract

La présente invention concerne un matériau composite pouvant utiliser efficacement les propriétés d’un matériau de base de poudre de métal en soi ou un matériau en céramique et céramique ajoutée en soi, une excellente conductivité électrique et une conductibilité thermique et des propriétés de résistance présentées par un matériau carboné fibreux formé de graphène. A cette fin, on procède à l’incorporation d’un matériau carboné fibreux formé de graphène, tel que des nanotubes de carbone ou des fibres de carbone produites en phase vapeur, puis à un frittage par décharge plasma pour l’intégration en vue de produire un frittage métal ou un frittage mixte composé d’un frittage métallique et céramique ou d’un frittage céramique. L’incorporation du matériau carboné fibreux formé de graphène peut améliorer différentes propriétés comme la conductibilité thermique et la conductivité électrique que possède le métal. Bien que le coefficient de roulement du frittage soit inférieur à celui d’un matériau exempt de matériau carboné fibreux, il est possible de rouler le frittage. Une fois prise en considération la sélection des différentes conditions, par exemple les conditions de roulement comme la direction de roulement et la réduction de roulement et le nombre de cycles de roulement, et le recuit faisant suite au roulement, il est possible de réguler le module de Young et l’étirement, la contrainte résiduelle ou d’autres propriétés ductiles ainsi que de nombreuses autres propriétés, sans provoquer de modification dans la résistance à la traction après le roulement.
PCT/JP2006/305738 2005-05-10 2006-03-22 Materiau composite extremement thermoconducteur WO2006120803A1 (fr)

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