WO2006112487A1 - ピッチ系炭素繊維、マットおよびそれらを含む樹脂成形体 - Google Patents
ピッチ系炭素繊維、マットおよびそれらを含む樹脂成形体 Download PDFInfo
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- WO2006112487A1 WO2006112487A1 PCT/JP2006/308250 JP2006308250W WO2006112487A1 WO 2006112487 A1 WO2006112487 A1 WO 2006112487A1 JP 2006308250 W JP2006308250 W JP 2006308250W WO 2006112487 A1 WO2006112487 A1 WO 2006112487A1
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- Prior art keywords
- pitch
- fiber
- carbon fiber
- based carbon
- carbon
- Prior art date
Links
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
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- H—ELECTRICITY
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- H05K3/4611—Manufacturing multilayer circuits by laminating two or more circuit boards
- H05K3/4641—Manufacturing multilayer circuits by laminating two or more circuit boards having integrally laminated metal sheets or special power cores
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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
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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
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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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
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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
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- Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer
Definitions
- the present invention relates to a mixture of pitch-based carbon short fibers having different fiber diameters, a carbon fiber mat containing pitch-based carbon short fibers, a strong resin molded product containing them, and uses of the molded product.
- High-performance carbon fibers can be classified into PAN-based carbon fibers made from polyacrylonitrile (PAN) and pitch-based carbon fibers made from a series of pitches.
- PAN polyacrylonitrile
- Carbon fiber is used widely in aerospace / space applications, architecture / civil engineering applications, and sports / leisure applications, taking advantage of the fact that its strength and elastic modulus are significantly higher than those of ordinary synthetic polymers.
- carbon fibers have a higher thermal conductivity than ordinary synthetic polymers, but further improvements in thermal conductivity are being investigated.
- the thermal conductivity of commercially available PAN-based carbon fibers is usually lower than 200 WZ (m-K).
- pitch-based carbon fibers are generally recognized as being more likely to achieve higher thermal conductivity than PAN-based carbon fibers.
- carbon fiber in order for carbon fiber to actually act as a heat conducting material, it is necessary to improve the thermal conductivity when formed into a molded body.
- the filler mainly responsible for heat conduction forms a network in three dimensions.
- the filler network in the molded body depends on the dispersion state, but if the dispersion is uniform, percolation Behavior. Therefore, in order to obtain sufficient thermal conductivity, it is necessary to add more filler than a certain amount.
- the conventional composite material made from a woven fabric made of a fiber and made into a composite material has improved the in-plane thermal conductivity, but the thermal conductivity in the thickness direction is a carbon fiber network. It is difficult to say that it is good because it cannot be formed sufficiently.
- Japanese Patent Application Laid-Open No. 5-175993 discloses a heat conductive molded article having high mechanical strength in which carbon fiber aligned in one direction is impregnated with black lead powder and a thermosetting resin.
- Japanese Patent Application Laid-Open No. 2-2 4 2 9 1 9 discloses that physical properties such as thermal conductivity are improved by improving the physical properties of the carbon fiber, but the thermal physical properties of the molded body are clear. It is not clear about performance improvement.
- the average fiber diameter is in the range of 5 m or more and less than 10 m, the ratio of the fiber diameter dispersion to the average fiber diameter is 0.05 to 0.2, and the fiber length is in the range of 20 to 6, OOO ⁇ m.
- the average fiber diameter is in the range of 10 m to 20 m
- the ratio of the fiber diameter dispersion to the average fiber diameter is 0.05 to 0.2
- the fiber length is in the range of 20 to 6,000 m.
- a weight ratio of the first pitch-based carbon fiber to the second pitch-based carbon fiber is in the range of 1:99 to 99: 1, and is achieved by a pitch-based carbon short fiber mixture characterized in that Is done.
- the pitch-based carbon short fibers are dispersed in the gaps of the pitch-based carbon fiber mat, and the weight ratio of the pitch-based carbon fiber mat to the pitch-based carbon short fibers is 30:70 to 95: 5. In the range of
- a carbon fiber reinforced resin molded article comprising the pitch-based carbon short fiber mixture of the present invention and a matrix resin, and the pitch-based carbon short fiber mixture occupies 3 to 60% by volume based on the total of both. Achieved by:
- the pitch-based carbon fibers used in the pitch-based carbon short fiber mixture of the present invention will be described first.
- this pitch-based carbon short fiber for example, a material made from a condensed heterocyclic compound such as naphthenolene or phenanthrene, condensed polycyclic hydrocarbon compounds, petroleum-based pitch or coal-based pitch is preferable.
- condensed polycyclic hydrocarbon compounds such as naphthalene and phenanthrene are preferable
- optically anisotropic pitch that is, mesophase pitch is particularly preferable.
- mesophase pitch is particularly preferable.
- the softening point of the raw material pitch can be obtained by the Mettler method, and is preferably 2550 ° C. or higher and 35 ° C. or lower. When the softening point is lower than 250 ° C., fusion of fibers and large heat shrinkage occur during infusibility. On the other hand, when the temperature is higher than 350 ° C, the pitch is thermally decomposed and is not easily formed into a filament.
- the raw material pitch is spun by the melt blow method, and then becomes a pitch-based carbon short fiber filler by infusibilization, firing, milling, sieving, and graphitization. Each process will be described below.
- the shape of the spinning nozzle of the pitch fiber used as the raw material for the pitch-based carbon short fiber is not particularly limited, but the nozzle hole length to hole diameter ratio is preferably smaller than 3, more preferably smaller than 1.5. Things are used.
- the temperature of the nozzle at the time of spinning is not particularly limited, and the temperature at which a stable spinning state can be maintained, that is, the temperature at which the spinning pitch viscosity is 2 to 80 Pa ⁇ S, preferably 5 to 30 Pa ⁇ S. If it is.
- the pitch fiber drawn from the nozzle hole is heated to 100 to 35 ° C., and the gas with a linear velocity of 100 to 100 m / min. It is shortened by spraying.
- the gas to be blown can be used as the gas to be blown, but air is desirable from the viewpoint of cost performance.
- the pitch fibers are collected on a wire mesh belt to form a continuous mat, A web with a certain basis weight is obtained by slap.
- the web made of pitch fibers thus obtained is infusibilized by a known method and fired at 700 to 900 ° C.
- the infusibilization is performed at 20 ° C. to 3500 ° C. using air or a gas obtained by adding ozone, nitrogen dioxide, nitrogen, oxygen, iodine, bromine to air, for example. Considering safety and convenience, it is desirable to carry out in air.
- the infusible pitch fiber is fired in a vacuum or in an inert gas such as nitrogen, argon or krypton. It is preferably carried out under normal pressure and in low-cost nitrogen.
- the web consisting of pitch fibers that has been fired is milled and sieved to make the fibers even shorter.
- a powder mill such as a Victory mill, a jet mill, a high-speed rotary mill, or a cutting machine can be used.
- a cutting machine In order to perform milling efficiently, it is appropriate to cut the fiber in a direction perpendicular to the fiber axis by rotating the mouth attached with the blade at high speed.
- the average length of carbon fiber produced by milling can be controlled by adjusting the number of rotor rotations, blade angle, and the like.
- the pitch-based carbon short fibers used in the present invention are graphitized by heating the pitch fibers, which have been subjected to the baking after the sieving, to 2,300 to 3,500 ° C. Graphite soot is carried out in a non-oxidizing atmosphere.
- the length of the pitch-based carbon short fiber is determined by the above-described sieving, but the fiber diameter and the dispersion of the fiber diameter are almost uniquely determined by the spinning process.
- the fiber diameter of the pitch-based carbon short fiber is 1 to 2 / m smaller than the fiber diameter of the original yarn when it is spun.
- CV which is the ratio of the fiber diameter dispersion degree to the average fiber diameter, is defined by the following formula and directly reflects the value of the raw yarn produced by the Melt-Blow method. ⁇
- Si can be obtained by the following formula.
- D is the fiber diameter of each of the n fibers, is the average value of the n fiber diameters, and n is the number of fibers.
- the pitch-based carbon short fibers have an average fiber diameter in the range of 5 m to less than 10 m, and the first fiber pitch short carbon fibers having a CV of 0.05 to 0.02 and an average fiber diameter of 10 im. It is in the range of 20 m or less and is obtained as a mixture of second pitch carbon short fibers having a CV of 0.05 to 0.2.
- the filling rate of the carbon short fibers can be improved at the time of forming a molded body.
- the average fiber diameter is in the range of 5 nm to less than 10 ULm, more preferably 6-9 m short fibers and the average fiber diameter is in the range of 10 m to 20 m, more preferably 11-16 / xm.
- a mixture obtained by mixing these short fibers is suitable for improving the thermal conductivity of the molded product. If the average fiber diameter is less than 5 ⁇ m, the web created immediately after spinning cannot maintain its shape and productivity is poor.
- the average fiber diameter is larger than 20 m, there is no problem in the web shape, but the diameter of the raw yarn is 21-22, which causes unevenness in infusibilization, and the fibers are fused after firing.
- the ratio is high, and very large diameters are likely to occur.
- CV is less than 5% Fibers are not preferable for improving the filling rate because the randomness of the fiber diameter becomes small. Further, fibers having a CV of more than 20% are not preferable because too many thick fibers become a problem when infusible. More preferably, it is 7 to 15%, and further preferably 7 to 12%.
- the mixing ratio of the first and second pitch-based carbon short fibers can be in the range of 1:99 to 99: 1 by weight, more preferably 10:90 to 90:10.
- the true density of the first and second pitch-based short carbon fibers strongly depends on the graphitization temperature, but both are preferably in the range of 1.5 to 2.5 g / cc. More preferably, it is 1.6 to 2.5 g / cc.
- the thermal conductivity in the fiber axis direction of the first and second pitch-based carbon short fibers is 200 W / (m-K) or more, more preferably 30 OWZ (m ⁇ K) or more. .
- At least one of the first pitch-based carbon short fibers and the second pitch-based carbon short fibers has a crystallite size in the hexagonal network direction of 5 nm or more.
- the crystallite size derived from the growth direction of the hexagonal network surface can be determined by a known method, and can be determined by diffraction lines from the (110) plane of the carbon crystal obtained by the X-ray diffraction method.
- the reason why the crystallite size is important is that heat conduction is mainly handled by phonon, and it is crystal that generates phonon.
- the crystallite size is more desirably 20 nm or more, and further desirably 30 nm or more.
- the first and second pitch-based carbon short fibers may be surface treated and then sizing agent may be added to the short fibers in an amount of 0.1 to 15% by weight, preferably 0.4 to 7.5% by weight. Any commonly used sizing agent can be used. Specifically, an epoxy compound, a water-soluble polyamide compound, a saturated polyester, an unsaturated polyester, vinyl acetate, water, alcohol, glycol alone or a mixture thereof should be used. Can do.
- the matrix resin may be any of a thermosetting resin, a thermoplastic resin, or a thermoplastic elastomer resin.
- thermoplastic resins include polycarbonate, polyethylene terephthalate, polyethylene 1,6-naphthalene dicarboxylate, polyamide, polypropylene, polyethylene, polyepoxyetherketone, polyphenylene sulfide, and each of these polymers. A copolymer is used.
- thermoplastic resins more specifically, polyethylene-polypropylene, ethylene-olefin copolymers such as ethylene-propylene copolymer, polymethylpentene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate , Ethylene vinyl acetate copolymer, Polyvinyl alcohol, Polyacetal, Fluororesin (Polyvinyl fluoride, Polytetrafluoroethylene, etc.), Polyethylene terephthalate, Polypropylene terephthalate, Polyethylene naphthaleate, Polystyrene, Polyacrylonitrile, Styrene monoacrylonitrile copolymer, ABS resin, Polyphenylene ether (PPE) resin, Modified PPE resin, Aliphatic polyamide, Aromatic polyamide, Polyimide, Polyamideimide, Polymeric acrylic acid Polymerase evening acrylic acid esters of methacrylic Sanme chill etc.), polyacrylic acids, polycarbonate, Porifue two Reni
- thermoplastic elastomer resin for example, a polyester elastomer is preferable, and as the polyester elastomer, a block copolymer composed of a hard segment and a soft segment is preferable.
- the melting point of such a polyester elastomer is preferably 180 ° C to 230 ° C, more preferably 190 ° C to 210 ° C.
- the preferred elastic modulus is 1, OO OMPa or less.
- thermoplastic polyester elastomer resins are commercially available such as TR-EKV, B 4032 AT B4063AC, P4140DT, etc. manufactured by Teijin Chemicals Limited. It is. In particular, P 4 1 40 DT and B 4 0 3 2 AT, in which water absorption is suppressed, are preferable.
- a stabilizer or the like may be added to improve the stability of the thermoplastic polyester elastomer resin.
- thermosetting resin examples include an epoxy resin, a phenol resin, a silicone resin, a polyurethane resin, a polyimide resin, a thermosetting polyphenylene ether resin, or a thermosetting modified polyphenylene ether resin. It can. These may be used alone or in appropriate combination of two or more.
- matrix resin a thermoplastic resin and a thermosetting shelf can be appropriately mixed and used in order to develop desired physical properties in the carbon fiber reinforced plastic molded article.
- a mixing device or a kneading device such as a mixer, a blender, a roll or an extruder may be used.
- the molding production method examples include an injection molding method, a press molding method, a calendar molding method, an extrusion molding method, a casting molding method, and a blow molding method.
- the volume fraction of the pitch-based carbon short fiber mixture in the carbon fiber-reinforced resin molded body prepared by mixing the pitch-based carbon short fiber mixture and the matrix resin is preferably 3 to 60% by volume. More preferably, it is 5 to 50% by volume. When it is less than 3% by volume, it is difficult to create a path for heat conduction, and the addition of carbon fiber is not meaningful. Addition of 60% by volume or more causes a phenomenon of powder falling in which the carbon fibers are detached from the molded body, which deteriorates the quality of the molded body.
- the carbon fiber reinforced resin molded article of the present invention preferably has a high thermal conductivity as a molded article, but preferably has a thermal conductivity calculated from thermal diffusion to the front and back of 1 WZ (m-K). More preferably, it is 2 W / (m-K) or more, more preferably 5 W / (m ⁇ K) or more.
- the carbon fiber reinforced plastic molded article of the present invention can be used as a heat sink for electronic parts or a part of a heat exchanger. More specifically, it can be molded into a heat sink, a semiconductor package component, a heat sink, a heat spreader, a die pad, a printed wiring board, a cooling fan component, a heat pipe, a case, and the like.
- the carbon fiber mat containing the pitch-based carbon short fibers of the present invention will be described.
- the raw material of the carbon fiber constituting the pitch-based carbon fiber mat used in the present invention the same raw material as that used for producing the pitch-based carbon short fiber of the pitch-based carbon short fiber mixture described above can be used. .
- the raw material pitch is spun by the melt-pro method, then infusibilized and fired to form a three-dimensional random matte carbon fiber.
- each process will be described.
- the pitch fibers obtained by spinning from the raw material pitch are collected on a wire mesh belt and become a mat having a continuous three-dimensional random shape.
- a pitch fiber mat having the three-dimensional random shape thus obtained is infusibilized by a known method and fired at 1, 00 to 3,500 ° C. to have a three-dimensional random shape.
- a pitch-based carbon fiber mat is obtained.
- Infusibilization is achieved at 200 to 350 ° C. using air or a gas obtained by adding ozone, nitrogen dioxide, nitrogen, oxygen, iodine or bromine to the air. Considering safety and convenience, it is desirable to carry out in air.
- the infusible pitch fiber is fired in vacuum or in an inert gas such as nitrogen, argon, krypton, etc., but it is preferably carried out in nitrogen at normal pressure and at low cost. .
- the firing temperature is preferably set to 2, 300 to 3,500 ° C., and is set to 2,500 to 3,500. More preferably. It is preferable to place it in a graphite container during firing because it can block external physical and chemical effects.
- the pitch-based carbon fiber mat obtained in this way is formed by randomly distributing the carbon fibers constituting it in a three-dimensional direction in the space defining the mat.
- the obtained carbon fiber reinforced composite material tends to be able to conduct heat equally in all directions, which is preferable for achieving the object of the present invention.
- a carbon fiber bundle (UD material) in which each fiber is oriented in a specific direction When a carbon fiber reinforced composite material is used to produce heat, it is easy to conduct heat in a specific direction, but in other directions, there is a problem that heat conduction is extremely bad, which is not preferable.
- the carbon fibers constituting the pitch-based carbon fiber mat preferably have a crystallite size of 5 nm or more in the hexagonal network direction.
- the crystallite size derived from the growth direction of the hexagonal mesh plane can be obtained by a known method, and can be obtained by diffraction lines from the (1 1 0) plane of the carbon crystal obtained by the X-ray diffraction method.
- the reason why the crystallite size is important is that heat conduction is mainly borne by phonon, and it is the crystal that generates phonon.
- the crystallite size is more preferably 20 nm or more, and even more preferably 30 nm or more.
- the fiber diameter of the carbon fibers that make up the pitch-based carbon fiber pine cake is: It is preferably ⁇ 20 m. If the length is less than 1 m, the mat shape may not be maintained, resulting in poor productivity. When the fiber diameter exceeds 20 xm, unevenness in the infusibilization process becomes large, and a part of the fusion occurs. More preferably, it is 3 to 17 m, and more preferably 5 to 15 im.
- the CV value is desirably 0.2 or less. More desirably, it is 0.17 or less. If the CV value exceeds 0.2, the shape may change during firing, which is not preferable.
- the fiber length of the carbon fibers constituting the pitch-based carbon fiber mat is preferably from 0.01 to: 1,00 mm. If it is less than 0.0 l mm, handling as a fiber becomes difficult. On the other hand, if it exceeds 1,00,000 mm, the entanglement of the fiber increases remarkably and handling becomes difficult. More preferably, it is 1 to 900 mm, and still more preferably 10 to 800 mm.
- Examples of the raw material for the short carbon fiber used together with the pitch-based carbon short fiber in the present invention include the same condensed heterocyclic compounds as described above as the raw material for the pitch-based carbon fiber mat.
- the pitch-based carbon short fiber can be obtained by grinding the pitch-based carbon fiber obtained by a conventionally known manufacturing method or the pitch-based carbon fiber mat.
- the powdering method is not particularly limited.
- a pulverizer such as a Victory mill, a jet mill, or a high-speed rotary mill, or a cutting machine is preferably used.
- a low speed blade equipped with a blade is rotated at high speed. It is appropriate to cut the fiber in a direction perpendicular to the fiber axis.
- the average length of the carbon fiber produced by the powder is controlled by adjusting the number of rotations of the rotor, the angle of the blade, and the like.
- the pitch fiber after the sieving may be further heated to 2,300 to 3,500 ° C. to be graphitized to obtain a final short carbon fiber.
- the length of the short carbon fiber is determined by the above-described sieving, but the average fiber diameter and the fiber diameter dispersion are almost uniquely determined by the spinning process.
- the fiber diameter of the short carbon fiber is 1 to 2 zm smaller than the fiber diameter of the original yarn when it is spun.
- the CV value reflects the raw yarn value as it is spun.
- the short carbon fiber used in the present invention has an average fiber diameter.
- the mat shape may not be maintained, resulting in poor productivity. If the fiber diameter exceeds 20 xm, unevenness in the infusibilization process will increase and partial fusion will occur. More desirably, the thickness is 3 to 17 mm, and more desirably 5 to 15 m.
- the CV value should be 0.2 or less. More desirably, it is 0.17 or less. If the CV value exceeds 0.2, the shape may change during firing, which is not preferable.
- the mixing ratio of pitch-based carbon fiber mat to pitch-based carbon short fiber is in the range of 30:70 to 95: 5 by weight. Preferably, it is 50: 50-90: 10. If the mixing ratio of the pitch-based carbon fiber mat is less than 30% by weight, the thermal conductivity in the thickness direction is not sufficiently exhibited, and if it exceeds 95% by weight, the filling rate cannot be increased.
- the true density of the pitch-based carbon fiber mat depends strongly on the firing temperature, but it is 1.5-2.
- the range of 5 gZc c is preferable, and more preferably 1.6 to 2.5 gZc c.
- the thermal conductivity in the fiber axis direction of the pitch-based carbon fiber constituting the pitch-based carbon fiber mat is preferably 200 WZ (m-K) or more, more preferably 300 W / (m ⁇ K) or more. It is.
- Preferred embodiments of the present invention include the following (i), (i i) and (i i i).
- the carbon fibers constituting the pitch-based carbon fiber mat have an average fiber diameter in the range of 1 to 202 m, and the fiber diameter dispersion with respect to the average fiber diameter is in the range of 0.05 to 0.2.
- Both the carbon fibers and the pitch-based carbon short fibers constituting the pitch-based carbon fiber mat have a true density of 1.5 to 2.5 gZc c.
- pitch-based short fiber reinforcing material provides a carbon fiber-reinforced composite material obtained by impregnating a matrix resin therein. Can do.
- thermosetting resins thermoplastic resins
- thermoplastic elastomers thermoplastic elastomers
- Thermoplastic resins can be preferably used from the viewpoint of shape flexibility and productivity.
- the ratio of the pitch-based carbon fiber reinforcement in the carbon fiber reinforced composite material is preferably 3 to 60% by volume, more preferably 5 to 50% by volume. If the proportion of the pitch-based carbon fiber reinforcement is less than 3% by volume, the desired thermal conductivity cannot be obtained, and if it exceeds 60% by volume, molding becomes extremely difficult.
- the carbon fiber reinforced composite material should have a high thermal conductivity as a composite material, but the thermal conductivity calculated from the thermal diffusion to the front and back is 1WZ (m-K) or more. More preferably, it is 2 WZ (m-K) or more, more preferably 5 WZ (m-K) or more.
- the carbon fiber reinforced composite material is advantageously obtained by predispersing pitch-based short carbon fibers in a pitch-based carbon fiber mat or matrix resin and then impregnating the matrix resin in the pitch-based carbon fiber mat. .
- pitch-based carbon fiber mat The pitch-based carbon fiber mat, pitch-based carbon short fiber, and matrix resin are the same as those described above.
- the method for dispersing the pitch-based carbon short fibers into the pitch-based carbon fiber mat is not particularly limited, but is a method of dry blending to the pitch-based carbon fiber mat, or the pitch of the carbon short fibers after being dispersed in the solvent. It can be carried out by a method of immersing a carbon fiber mat and then removing the solvent.
- the method for dispersing the short carbon fibers in the matrix resin is not particularly limited.
- the matrix t fat is liquid at room temperature, it can be applied by a kneading apparatus such as a mixer.
- the matrix resin is solid at room temperature, it can be melted by heating and can be carried out by a kneading apparatus such as a twin screw extruder.
- the molding method for obtaining the carbon fiber strong composite material includes injection molding, press molding, calendar molding, extrusion molding, cast molding, and blow molding. However, the following two methods can be implemented. As the first method,
- short carbon fibers are dispersed in a matrix resin by the above method, and then the matrix resin in which the short carbon fibers are dispersed is introduced into a pitch-based carbon fiber mat.
- the matrix resin is liquid at room temperature
- carbon fiber reinforcement is achieved by introducing it into the pitch-based carbon fiber mat pre-loaded in the mold using the RIM or RTM methods and curing the matrix resin.
- a composite material can be obtained.
- the carbon short fibers are dispersed in the matrix resin by the above method, and then injected into a pitch-based carbon fiber mat that has been charged in advance in the mold.
- a fiber reinforced composite material can be obtained.
- a matrix resin in which short carbon fibers are dispersed is processed into a sheet shape in advance and press-molded in a state of being laminated with a pitch-based carbon fiber mat.
- a carbon fiber reinforced composite material can be obtained.
- vacuum press molding it is preferably performed in a vacuum state for the purpose of suppressing the generation of voids.
- the matrix resin When the matrix resin is liquid at room temperature, it is introduced into the pitch-based carbon fiber mat in which short carbon fibers previously charged in the mold are dispersed by the RIM method, RTM method, etc., and the matrix resin is hardened. By letting it evaporate, a carbon fiber reinforced composite material can be obtained.
- a carbon fiber reinforced composite material can be obtained by injection molding a pitch-based carbon fiber mat in which short carbon fibers previously charged in a mold are dispersed.
- a carbon fiber reinforced composite material can be obtained by processing the matrix resin into a sheet-like shape in advance and press-molding it in a state of being laminated with a pitch-based carbon fiber mat in which short carbon fibers are dispersed.
- vacuum press molding it is preferably performed in a vacuum state for the purpose of suppressing the generation of voids.
- the pitch-based carbon fiber mat and Z or carbon short fiber may be surface-treated and then a sizing agent may be attached thereto.
- the surface may be modified by an oxidation treatment such as electrolytic oxidation or a treatment with a force pulling agent or a sizing agent.
- an oxidation treatment such as electrolytic oxidation or a treatment with a force pulling agent or a sizing agent.
- methods such as electroless plating, electrolytic plating, physical vapor deposition such as vacuum deposition, sputtering, and ion plating, chemical vapor deposition, painting, dipping, and mechanochemical methods for mechanically fixing fine particles.
- the surface may be coated with metal or ceramics.
- the sizing agent is used in an amount of 0.1 to 15% by weight, preferably 0.4 to 7.5% by weight, based on the pitch-based carbon fiber mat and Z or short carbon fiber.
- Sizing agent Any of those usually used can be used, and specifically, an epoxy compound, a water-soluble polyamide compound, a saturated polyester, an unsaturated polyester, vinyl acetate, water, an alcohol, glycol alone or a mixture thereof can be used.
- the carbon fiber reinforced composite material is preferably used for a heat radiating plate for electronic parts or a heat exchanger.
- heat dissipation members heat transfer members, or constituent materials for effectively dissipating the heat generated by electronic components such as semiconductor elements, power supplies, and light sources to the outside, for heat sinks and semiconductor packages It can be molded into parts, heat sinks, heat spreaders, die pads, printed wiring boards, cooling fan parts, heat pipes, casings, etc.
- the thermal conductivity of the carbon fiber composite sheet can be measured by a known method, it is desirable to use the laser flash method particularly because it aims to improve the thermal conductivity in the thickness direction of the carbon fiber composite sheet.
- the thermal conductivity of carbon fiber itself is several hundred WZ (mK), but when it is formed, the thermal conductivity decreases rapidly due to the occurrence of defects, air contamination, and unexpected voids. To do. Therefore, it has been considered difficult for the carbon fiber composite sheet to have a thermal conductivity substantially exceeding 1 WZ (m-K).
- this is solved by using a carbon fiber mat, and the carbon fiber composite sheet is made 1 WZ (m-K) or more. More preferably, it is 2 W / (m-K) or more, and more preferably 5 WZ (m-K) or more.
- the carbon fiber reinforced composite material thus obtained can be suitably used for the purpose of thermal management.
- the average fiber diameter and fiber diameter dispersion of pitch-based carbon short fibers were obtained by photographing 10-field images of the graphitized fiber under a scanning electron microscope at 800x magnification.
- ⁇ represents the thermal conductivity W / ( ⁇ ⁇ ⁇ ) of the carbon fiber
- ER represents the electrical specific resistance ⁇ of the carbon fiber
- the thermal conductivity of the molded body was obtained by a laser flash method (using LFA 447 manufactured by NETZCH) using a carbon fiber reinforced plastic molded product molded into a 1 mm thick sheet as a sample.
- the density of the pitch-based carbon short fibers was determined using a specific gravity method.
- the crystal size of the carbon fiber was determined by the Gakushin method by measuring the reflection from the (1 10) plane appearing in X-ray diffraction.
- the diameter of the three-dimensional random mat-like carbon fiber was obtained by photographing the fired fiber using a scanning electron microscope at 800x and extracting any 10 fields of view.
- Pitch made of condensed polycyclic hydrocarbon compound was used as the main raw material. This pitch had an optical anisotropy ratio of 100% and a softening point of 285 ° C.
- heated air is ejected from the slit at a linear velocity of 5,000 m / min to produce a pitch-type short fiber with an average diameter of 10 m by pulling the melt pitch. did.
- the spun fibers are collected on a belt to form a mat, which is further weighted by cross wrapping 2
- the web was made of 50 g / m 2 pitch-based short fibers.
- the web was infusibilized by raising the temperature from 170 ° C to 29 ⁇ in air at an average heating rate of :: min.
- the infusibilized web was fired at 800 ° C, milled, and sieved to a length of 50 to 500 m. Then, it was graphitized by heating to 3,000 ° C in a non-oxidizing atmosphere furnace.
- the average fiber diameter was 8.5 m and the CV was 15%. This was designated as pitch-based carbon short fiber A.
- the thermal conductivity was 480 W / (m ⁇ K).
- pitch-based short fibers having an average diameter of 13 m were produced by pulling the melt pitch.
- the spun fibers were collected on a belt to make a mat, and then a web consisting of pitch-based short fibers having a basis weight of 300 gZm 2 by cross-rubbing.
- the web was heated in air from 170 ° C to 295 ° C at an average rate of temperature increase of 5 ° CZ for infusibilization.
- the infusibilized web was fired at 800 ° C, milled, and sieved to 50-500 zm length. After that, it was graphitized by heating to 3,000 ° C in an Atchison furnace in a non-oxidizing atmosphere.
- the average fiber diameter was 11.5 m and the CV was 13%.
- pitch-based carbon short fiber B This was designated as pitch-based carbon short fiber B.
- the thermal conductivity was 480WZ (m-K).
- the mixture was added at a volume ratio of 30% to the polystrength Ponate resin, and a flat plate was produced by injection molding.
- the thermal conductivity in the thickness direction of the flat plate was 1.5 WZ (m * K).
- a pitch-based carbon short fiber mixture prepared by mixing carbon short fibers A and B prepared in Example 1 at a weight ratio of 50:50 was prepared, and 30% by volume ratio was added to the polyphenylene sulfide resin.
- a flat plate was produced. The density of the mixture was 2. O gZc c, and the thermal conductivity in the thickness direction of the flat plate was 3.3 W / (m-K).
- a flat plate was produced. The density of the mixture was 2.0 g / c c, and the thermal conductivity in the thickness direction of the flat plate was 2.9 WZ (m ⁇ K).
- Example 1 Only the short carbon fibers A produced in Example 1 were used as pitch-based carbon short fibers, and 30% by volume was added to the polycarbonate resin, and a flat plate was produced by injection molding.
- the density of carbon short fiber A was 2.0 gZc c, and the thermal conductivity in the thickness direction of the flat plate was 0.8 ⁇ / (m ⁇ K).
- Example 7 Only the short carbon fibers B produced in Example 1 were used as pitch-based short carbon fibers, and 30% by volume was added to the polyphenylene sulfide resin, and a flat plate was produced by injection molding.
- the density of the short carbon fiber B was 2.0 gZcc, and the thermal conductivity in the thickness direction of the flat plate was 0.6 WZ (m ⁇ K).
- Example 7 When the flat plate produced in Example 1 was replaced with a case made of only a single polyponate and a mass of stainless steel heated to 80 ° C was added as a heat source, it was confirmed that the increase in internal temperature was suppressed. .
- Example 4 When the flat plate produced in Example 4 was replaced with a casing made of only polycarbonate, and a lump of stainless steel heated to 80 ° C was added as a heat source, it was confirmed that the rise in internal temperature was suppressed.
- a pitch made of a condensed polycyclic hydrocarbon compound was used as a main raw material.
- This pitch had an optical anisotropy ratio of 100% and a softening point of 285 ° C.
- heated air is ejected from the slit at a linear velocity of 5,000 m / min, and the pitch is melted to draw pitch-based short fibers with an average diameter of 11 m.
- the spun fibers were collected on a belt to form a mat, and further to a pitch fiber mat having a three-dimensional random shape with a cross wrapping weight of 250 gZm 2 .
- the pitch fiber mat was infusibilized by raising the temperature from 17'0 ° C to 300 ° C in air at an average heating rate of 5 ° C Z min. An infusible pitch fiber mat was fired at 3,000 ° C to obtain a pitch-based carbon fiber mat A having a three-dimensional random shape.
- the average fiber diameter of pitch-based carbon fibers constituting pitch-based carbon fiber mat A was 9 m, and CV was 18%.
- the average fiber length was 10 Omm.
- the crystallite size was 46 nm.
- the thermal conductivity was 595 WZ (m ⁇ K).
- Short fiber B was obtained.
- Short carbon fiber B had an average fiber diameter of 9/2 m and CV of 18%. The average fiber length was 0.5 mm.
- a pitch made of a condensed polycyclic hydrocarbon compound was used as a main raw material.
- the optical anisotropy ratio of this pitch was 100%, and the softening point was 285 ° C.
- heated air is ejected from the slit at a linear velocity of 4,800 m / min to produce a pitch-type short fiber with an average diameter of 12 m by pulling the melt pitch. did.
- the spun fibers were collected on a belt to form a mat, and then a pitch fiber mat having a three-dimensional random shape with a basis weight of 250 g / m 2 by cross wrapping.
- the pitch fiber mat was infusibilized by raising the temperature from 170 ° C to 300 ° C in air at an average heating rate of 5 ° C Z min.
- the infusible pitch fiber mat was fired at 3,000 ° C to obtain a pitch-based carbon fiber mat A having a three-dimensional random shape.
- the average fiber diameter of pitch-based carbon fibers constituting the pitch-based carbon fiber mat A was 10 xm, and CV was 19%.
- the average fiber length was 15 Omm.
- the crystallite size was 47 nm.
- the thermal conductivity was 61 OW / (m ⁇ K).
- the short fiber B had an average fiber diameter of 10 zm and a CV of 19%.
- the average fiber length was 0.2 mm.
- Teijin Kaisei Co., Ltd. polystrength Ponate resin was used as the matrix resin, and using a twin screw extruder equipped with a film forming die, 100 parts by weight of polycarbonate resin and short carbon fiber B 20 After melt-kneading the weight parts, a film-like molded product was obtained.
- Pitch made of condensed polycyclic hydrocarbon compound was used as the main raw material.
- This pitch had an optical anisotropy ratio of 100% and a softening point of 285 ° C.
- heated air is ejected from the slit at a linear velocity of 5,000 m / min, pulling the melt pitch, and pitch-based short fibers with an average diameter of 10 / m Was made.
- the spun fibers were collected on a belt to form a mat, and further, a pitch fiber mat having a three-dimensional random shape with a basis weight of 250 gZm 2 by cross wrapping.
- the pitch fiber mat was infusibilized by raising the temperature from 170 ° C to 295 ° C in air at an average heating rate of 7 ° C / min.
- the infusible 3D random mat was fired at 800 ° C.
- the average fiber diameter of pitch-based carbon fibers constituting the pitch-based carbon fiber mat after firing was 9 HI and CV was .18%.
- the average fiber length was 40 mm.
- the crystallite size was 3 nm.
- the thermal conductivity was 35 WZ (m ⁇ K).
- Example 9 instead of the carbon fiber reinforced composite material, a maleic acid-modified polypropylene resin single body was used as a molded body, and the thermal conductivity was measured to be less than 1 WZ (m-K).
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- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Inorganic Fibers (AREA)
- Nonwoven Fabrics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007528179A JP4538502B2 (ja) | 2005-04-18 | 2006-04-13 | ピッチ系炭素繊維、マットおよびそれらを含む樹脂成形体 |
DE200660016766 DE602006016766D1 (de) | 2005-04-18 | 2006-04-13 | Pechbasierte carbonfasern sowie sie enthaltende matte und formkörper |
EP20060732108 EP1873283B1 (en) | 2005-04-18 | 2006-04-13 | Pitch-derived carbon fibers, mat, and molded resin containing these |
US11/911,912 US7651767B2 (en) | 2005-04-18 | 2006-04-13 | Pitch-based carbon fiber, web and resin molded product containing them |
CN2006800130297A CN101163825B (zh) | 2005-04-18 | 2006-04-13 | 沥青类碳纤维、毡以及含有它们的树脂成型体 |
US12/622,999 US7767302B2 (en) | 2005-04-18 | 2009-11-20 | Pitch-based carbon fiber, web and resin molded product containing them |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005-119537 | 2005-04-18 | ||
JP2005119537 | 2005-04-18 | ||
JP2005156894 | 2005-05-30 | ||
JP2005-156894 | 2005-05-30 |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US11/911,912 A-371-Of-International US7651767B2 (en) | 2005-04-18 | 2006-04-13 | Pitch-based carbon fiber, web and resin molded product containing them |
US12/622,999 Division US7767302B2 (en) | 2005-04-18 | 2009-11-20 | Pitch-based carbon fiber, web and resin molded product containing them |
Publications (1)
Publication Number | Publication Date |
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WO2006112487A1 true WO2006112487A1 (ja) | 2006-10-26 |
Family
ID=37115199
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2006/308250 WO2006112487A1 (ja) | 2005-04-18 | 2006-04-13 | ピッチ系炭素繊維、マットおよびそれらを含む樹脂成形体 |
Country Status (8)
Country | Link |
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US (2) | US7651767B2 (ja) |
EP (2) | EP2180094B1 (ja) |
JP (1) | JP4538502B2 (ja) |
KR (1) | KR20080000592A (ja) |
CN (2) | CN101163825B (ja) |
AT (2) | ATE510946T1 (ja) |
DE (1) | DE602006016766D1 (ja) |
WO (1) | WO2006112487A1 (ja) |
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JP2007084649A (ja) * | 2005-09-21 | 2007-04-05 | Teijin Ltd | 炭素繊維複合シート及びその製造方法 |
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WO2008023777A1 (fr) * | 2006-08-22 | 2008-02-28 | Kureha Corporation | Article moulé stratifié contenant une fibre de carbone et son procédé de fabrication |
US8962500B2 (en) | 2006-08-22 | 2015-02-24 | Kureha Corporation | Molded article containing stacked carbon fiber and method for producing same |
JP4889741B2 (ja) * | 2006-08-22 | 2012-03-07 | 株式会社クレハ | 炭素繊維含有積層成型体及びその製造方法 |
JP2008069474A (ja) * | 2006-09-13 | 2008-03-27 | Teijin Ltd | 補強材・放熱材に適する炭素繊維集合体 |
JP2008189866A (ja) * | 2007-02-07 | 2008-08-21 | Teijin Ltd | 炭素繊維補強熱硬化性樹脂放熱材 |
JP2008189867A (ja) * | 2007-02-07 | 2008-08-21 | Teijin Ltd | 炭素繊維補強熱可塑性樹脂複合材料 |
JP2008208490A (ja) * | 2007-02-27 | 2008-09-11 | Teijin Ltd | ピッチ系炭素繊維及び炭素繊維強化複合材料 |
JP2008208316A (ja) * | 2007-02-28 | 2008-09-11 | Teijin Ltd | 炭素繊維複合材料 |
JP2008214543A (ja) * | 2007-03-06 | 2008-09-18 | Teijin Ltd | 炭素繊維複合材及びその製造方法 |
JPWO2008108482A1 (ja) * | 2007-03-06 | 2010-06-17 | 帝人株式会社 | ピッチ系炭素繊維、その製造方法および成形体 |
US7846543B2 (en) | 2007-03-06 | 2010-12-07 | Teijin Limited | Pitch-based carbon fibers, and manufacturing method and molded product thereof |
WO2008108482A1 (ja) * | 2007-03-06 | 2008-09-12 | Teijin Limited | ピッチ系炭素繊維、その製造方法および成形体 |
JP2009108119A (ja) * | 2007-10-26 | 2009-05-21 | Teijin Ltd | 熱伝導性フィラー及びそれを用いた成形体 |
JP2009108118A (ja) * | 2007-10-26 | 2009-05-21 | Teijin Ltd | ピッチ系炭素短繊維フィラー及びそれを用いた成形体 |
WO2010024462A1 (ja) * | 2008-09-01 | 2010-03-04 | 帝人株式会社 | ピッチ系黒鉛化短繊維及びそれを用いた成形体 |
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JP2013010859A (ja) * | 2011-06-29 | 2013-01-17 | Mitsubishi Chemicals Corp | 熱可塑性エラストマー組成物 |
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CN101935919A (zh) | 2011-01-05 |
JP4538502B2 (ja) | 2010-09-08 |
ATE510946T1 (de) | 2011-06-15 |
CN101935919B (zh) | 2011-09-14 |
US20100068496A1 (en) | 2010-03-18 |
US20090075054A1 (en) | 2009-03-19 |
CN101163825B (zh) | 2011-09-14 |
EP1873283A4 (en) | 2009-09-16 |
EP2180094A1 (en) | 2010-04-28 |
DE602006016766D1 (de) | 2010-10-21 |
EP2180094B1 (en) | 2011-05-25 |
CN101163825A (zh) | 2008-04-16 |
ATE480653T1 (de) | 2010-09-15 |
KR20080000592A (ko) | 2008-01-02 |
US7767302B2 (en) | 2010-08-03 |
EP1873283B1 (en) | 2010-09-08 |
JPWO2006112487A1 (ja) | 2008-12-11 |
EP1873283A1 (en) | 2008-01-02 |
US7651767B2 (en) | 2010-01-26 |
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