WO2021043051A1 - High-performance heat conducting interface material and application thereof - Google Patents

High-performance heat conducting interface material and application thereof Download PDF

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Publication number
WO2021043051A1
WO2021043051A1 PCT/CN2020/111612 CN2020111612W WO2021043051A1 WO 2021043051 A1 WO2021043051 A1 WO 2021043051A1 CN 2020111612 W CN2020111612 W CN 2020111612W WO 2021043051 A1 WO2021043051 A1 WO 2021043051A1
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powder
parts
interface material
thermally conductive
microns
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PCT/CN2020/111612
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French (fr)
Chinese (zh)
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范勇
程亚东
唐正华
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上海阿莱德实业股份有限公司
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Publication of WO2021043051A1 publication Critical patent/WO2021043051A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/28—Nitrogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5425—Silicon-containing compounds containing oxygen containing at least one C=C bond
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0812—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/28—Nitrogen-containing compounds
    • C08K2003/282—Binary compounds of nitrogen with aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/004—Additives being defined by their length
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Definitions

  • the invention belongs to the technical field of thermally conductive materials, and specifically relates to a high-performance thermally conductive interface material and its application.
  • thermal conductive materials with light weight, good mechanical properties, strong electrical insulation, and low price have become the trend of future development.
  • Electronic industry products such as LEDs, microelectronic packaging materials and semiconductor devices continue to develop in the direction of miniaturization, lightness and thinness, and intelligence. Therefore, people have put forward higher requirements for the thermal conductivity of the materials.
  • Thermally conductive materials used in electronic devices such as high heat dissipation materials, electronic packaging materials, etc., often need to have excellent electrical insulation and high breakdown voltage properties to meet the requirements of use.
  • the heat generated by the product has also increased significantly.
  • the continuous rise of operating temperature will reduce the stability and reliability of electronic equipment, and shorten the service life of the product.
  • the first aspect of the present invention provides a high-performance thermal interface material, which is characterized in that, in parts by weight, the preparation raw materials include: 13-20 parts of liquid silica gel, 27-35 parts of metal powder , 7-13 parts of metal oxides, 20-30 parts of carbon materials, 0.1-0.5 parts of alkenyl-containing siloxane;
  • the metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
  • the metal powder is composed of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns.
  • the weight ratio of the 1-10 micron metal powder to the 30-50 micron metal powder is (0.8-1.2):1.
  • the molecular formula of the metal oxide is M x O y , where M is selected from one of Zn, Cu, Al, Ag, Ni, Fe, and Mg, x is 1-2, y For 1-3.
  • the average particle size of the metal oxide is 400-800 nm.
  • the carbon material is selected from at least one of carbon fibers, carbon nanotubes, carbon nanowires, graphene, and graphene oxide.
  • the average length of the carbon fiber is 50-200 microns.
  • the average length of the carbon fiber is 150 microns.
  • the thermally conductive interface material further includes 11-20 parts of ceramic materials.
  • the second aspect of the present invention provides an application of the thermally conductive interface material, which is used for heat dissipation of electronic products.
  • the thermally conductive interface material of the present invention has superior thermal conductivity, suitable hardness, and can be well applied to heat dissipation in the field of electronic products.
  • the above-mentioned range is regarded as continuous, and includes the minimum and maximum values of the range, and every value between such minimum and maximum values. Further, when the range refers to an integer, it includes every integer between the minimum value and the maximum value of the range.
  • the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein. For example, a specified range from "1 to 10" should be regarded as including any and all sub-ranges between the minimum value of 1 and the maximum value of 10. Exemplary sub-ranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
  • the present invention provides a high-performance thermally conductive interface material.
  • the preparation raw materials include: 13-20 parts of liquid silica gel, 27-35 parts of metal powder, 7-13 parts of metal oxide, and carbon 20-30 parts of materials, 0.1-0.5 parts of alkenyl-containing siloxane.
  • the thermal interface material prepares raw materials including: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, and alkenyl-containing silica 0.32 parts of alkane.
  • the liquid silica gel mentioned in this application includes two types: one type is liquid silica gel with functional groups at both ends of the molecular structure; the other type is liquid silica gel with active functional groups randomly distributed in the main chain.
  • the liquid silica gel has fast flow, The advantages of mild curing conditions, safety and environmental protection.
  • the liquid silica gel includes hydroxyl-modified polydimethylsiloxane-type silica gel, carboxyl-modified polydimethylsiloxane-type silica gel, and silicon-hydrogen bond-containing polydimethylsiloxane-type silica gel. At least one of them.
  • the viscosity of the liquid silica gel is 500-1000 mPa ⁇ s.
  • the viscosity test of the liquid silica gel refers to the standard ISO3219, and the temperature is 25 degrees Celsius.
  • the model of the liquid silica gel is Waker-9212 A/B, which was purchased from Wacker, Germany.
  • the thermal conductivity of aluminum is 190k/W ⁇ (m ⁇ K) -1
  • the thermal conductivity of zinc is 121k/W ⁇ (m ⁇ K) -1
  • the thermal conductivity of copper is 398k/W ⁇ (m ⁇ K) -1
  • the thermal conductivity of silver is 471k/W ⁇ (m ⁇ K) -1 .
  • the metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
  • the metal powder is aluminum powder.
  • the metal powder is a spherical structure powder.
  • the shape and size of the metal particles affect their distribution in the polymer and the way they are stacked between the particles, thereby affecting the ability to build a heat conduction channel inside the polymer, and affecting its thermal conductivity and other properties.
  • the average particle size of the metal powder is 1-70 microns; preferably, the average particle size of the metal powder is 5-40 microns;
  • the metal powder is composed of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns;
  • the weight ratio of the 1-10 micron metal powder to the 30-50 micron metal powder is (0.8-1.2):1.
  • the weight ratio of the 5 micron metal powder to the 40 micron metal powder is (0.8-1.2):1.
  • the weight ratio of the 5 micron metal powder to the 40 micron metal powder is 1:1.
  • the metal powder described in the present application forms a thermally conductive network structure in the liquid silica gel, and improves the thermal conductivity of the silica gel with the help of free electron and phonon vibration.
  • the thermal conductivity of the metal oxide described in this application is lower than that of metal powder, but it has good electrical insulation, good wear resistance, and high hardness.
  • the molecular formula of the metal oxide is M x O y , where M is selected from one of Zn, Cu, Al, Ag, Ni, Fe, and Mg, x is 1-2, and y is 1. -3.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1.
  • the metal oxide is a powder with a spherical structure.
  • the average particle size of the metal oxide is 400-800 nm.
  • the average particle size of the metal oxide is 600 nm.
  • the carbon material is selected from at least one of carbon fibers, carbon nanotubes, carbon nanowires, graphene, and graphene oxide.
  • the carbon material is carbon fiber.
  • the average length of the carbon fiber is 50-200 microns.
  • the average length of the carbon fiber is 150 microns.
  • the carbon fiber described in this application has ultra-high thermal conductivity and mechanical strength, and the thermal conductivity can reach 700W/(m ⁇ K).
  • the special microcrystalline graphite structure of the carbon fiber makes it play a huge heat dissipation advantage in the heat conduction process.
  • the metal powder, metal oxide, carbon material, etc. have high thermal conductivity, but due to the lack of active groups, the surface energy is low, and the compatibility with liquid silica gel is poor, which will affect the thermal conductivity of the material. Its thermal conductivity, hardness and other properties.
  • the surface treatment of metal powders, metal oxides, and carbon materials is performed by adding alkenyl-containing siloxane to increase the compatibility between each other and improve the interfacial adhesion.
  • the alkenyl-containing siloxane is selected from 1-vinyl-1,1,3,3,3-pentamethyldisiloxane, 1,3,5-trivinyl -1,1,3,5,5-pentamethyltrisiloxane, vinyltris(dimethylsiloxane)silane, 1,3-divinyltetraethoxydisiloxane, methyl At least one of acryloyloxypentamethyldisiloxane, vinyltris(trimethylsiloxy)silane, and vinyltrimethoxysilane.
  • the alkenyl-containing siloxane is vinyltrimethoxysilane.
  • model number of the alkenyl-containing siloxane is KH171.
  • the thermally conductive interface material further includes 11-20 parts of ceramic materials.
  • the thermally conductive interface material further includes 15.31 parts of ceramic materials.
  • the ceramic material described in this application has an atomic crystal form and a dense structure, mainly conducts heat conduction by phonons, and has a high thermal conductivity.
  • the ceramic material is selected from one or more of silicon carbide, aluminum nitride, silicon nitride, aluminum silicate, and zirconium oxide.
  • the ceramic material is aluminum nitride.
  • the aluminum nitride is a covalent bond compound with a hexagonal wurtzite structure, white or off-white, and Al atoms and adjacent N atoms form a dismutated (AIN 4 ) tetrahedron.
  • AIN has a theoretical density of 3.269, a Mohs hardness of 7-8, and decomposes at 2200-22500 degrees Celsius. It has good stability and thermal shock resistance in a high-temperature non-oxidizing atmosphere within 2000 degrees Celsius.
  • the aluminum nitride has the characteristics of not being corroded by aluminum and other molten metals and gallium arsenide, and aluminum nitride also has excellent electrical insulation and dielectric properties.
  • the aluminum nitride is a powder with a spherical structure.
  • the average particle size of the aluminum nitride is 0.5-5 microns
  • the aluminum nitride is composed of aluminum nitride with an average particle size of 0.5-2 microns and aluminum nitride with an average particle size of 4-6 microns;
  • the weight ratio of the 0.5-2 micron aluminum nitride to the 4-6 micron aluminum nitride is (0.9-1.3):1.
  • the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is (0.9-1.3):1.
  • the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
  • the applicant has found through painstaking research that when metal powders, metal oxides, ceramics When the weight ratio of the material is: (2-4):1:(1-2), and the metal powder is composed of metal powder with an average particle size of 1-10 microns and an average particle size of 30-50 microns When the aluminum nitride is composed of aluminum nitride with an average particle size of 0.5-2 microns and aluminum nitride with an average particle size of 4-6 microns, the performance of the material is optimized.
  • the particle size of the metal powder, metal oxide or ceramic material is small, the specific surface area is larger; when the particle size of the metal powder, metal oxide or ceramic material is large, the thermal conductivity is better, and the particle size is different
  • the filler is distributed in the silica gel, it is limited by the particle size and kinetic energy of the filler.
  • Fillers with different particle sizes and different thermal conductivity contact each other to form a thermal conductive chain.
  • the thermal conductive material system is equivalent to forming multiple "parallel circuits”. Heat flow passes through multiple "parallel circuits" to improve thermal conductivity.
  • the solution properties of liquid silicone rubber, the incompatibility of filler surface energy, and the large viscosity of the mixture are improved.
  • the hardness of the interface material obtained is in the range of 30-50 ShoreOO, which has a good performance.
  • the processing performance is very suitable for heat dissipation in various electronic product fields.
  • the preparation method of the thermally conductive interface material includes the following steps:
  • step S2 Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, and the planetary vacuum is stirred for 5-20 minutes;
  • step S3 Add half of the carbon material to the mixture obtained in step S2, and stir the planetary vacuum for 1-30 min;
  • step S4 Add the remaining carbon material to the mixture obtained in step S3, and stir the planetary vacuum for 1-30 min;
  • step (1) Put the mixed material obtained in step (1) into the hydraulic injection extruder, spit it out through the needle nozzle, and arrange it neatly in a rectangular parallelepiped container. After it is stacked to a height of 1/2-1/4, the material is mixed in a vibrating compactor Vibrate, a total of 2-4 times.
  • step (2) Put the rectangular parallelepiped container in step (2) in a vacuum drying oven to evacuate to ⁇ -0.098MPa, 1-5 minutes later, release the vacuum, tap the material in a vibrating compactor, repeat at least once; then place the weights together Vacuum in the vacuum drying box to ⁇ -0.098MPa, release the vacuum after 1-5 minutes, repeat at least once;
  • the force applied by the weight to the container in step (3) and step (4) is 100-500 kgf.
  • the force applied by the weight to the container in step (3) and step (4) is 300 kgf.
  • the preparation method of the thermally conductive interface material includes the following steps:
  • step S2 Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, vacuum and stir for 5-20 minutes on the planet, then shovel the paddle and the material on the pot wall and continue to vacuum and stir for 1-10 minutes, and then add the paddle Shovel the material on the pot wall and continue to vacuum and stir for 1-10min;
  • step S3 Add half of the carbon material to the mixture obtained in step S2, vacuum the planetary for 1-10min, then shovel the material on the paddle and the pot wall and continue to vacuum and stir for 1-10min, and then put the paddle and the pot wall on Continue to vacuum and stir for 1-10min under the shovel;
  • step S4 Add the remaining carbon material to the mixture obtained in step S3, vacuum and stir for 1-10min on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 1-10min, and then shovel the material on the paddle and pot wall Continue to vacuum and stir for 1-10min, then shovel the paddle and the material on the pot wall and continue to vacuum and stir for 1-10min
  • step (1) Put the mixed material obtained in step (1) into a hydraulic injection extruder and spit it out through a needle nozzle.
  • the diameter of the needle nozzle is 2.5mm. They are arranged neatly in a rectangular parallelepiped container and stacked to 1/2-1/4 height. , The material is vibrated in the vibrating compaction machine for a total of 2-4 times.
  • step (2) Put the rectangular parallelepiped container in step (2) in a vacuum drying oven to evacuate to ⁇ -0.098MPa, 1-5 minutes later, vacuum, and vibrate the material with a vibrating compactor; then put it in a vacuum drying oven to evacuate to ⁇ -0.098 MPa, 1-5 minutes later, vacuum, vibrating compactor to compact the material; after pressing the heavy objects, put them in a vacuum drying oven and vacuum to ⁇ -0.098MPa, 1-5 minutes after the vacuum, after pressing the heavy objects Then put it in a vacuum drying oven to evacuate to ⁇ -0.098MPa, and then release the vacuum after 1-5 minutes.
  • (2) in the orientation process put the mixed material obtained in step (1) into a hydraulic injection extruder, and spit it out through a needle nozzle with a diameter of 2.5mm, which is arranged neatly in a rectangular parallelepiped container and stacked After reaching 1/3 height, vibrate the material in a vibrating compactor for a total of 3 times.
  • the dimensions of the length, width, and height of the container are 250 mm, 150 mm, and 150 mm, respectively.
  • the specific operation is: put the mixed material obtained in step S1 into a hydraulic injection extruder and spit it out through a needle nozzle.
  • the diameter of the needle nozzle is 2.5mm.
  • the material is compacted by the compactor.
  • the compaction time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm; after continuing to stack to 2/3 height, the material is compacted by the vibrating compactor.
  • the compaction time is 40 minutes, and the vibration frequency It is 5Hz and the amplitude is 5mm; after continuing to pile up to the height of 3/3, the material is tapped by a vibrating compactor, the tapping time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm.
  • the second aspect of the present invention provides an application of the thermally conductive interface material, which is used for heat dissipation of electronic products.
  • the electronic products can be listed as watches, smart phones, telephones, televisions, video disc players (VCD, SVCD, DVD), video recorders, camcorders, radios, radio cassette recorders, combined speakers, compact disc players (CD), computers, games Machine waiting.
  • VCD video disc players
  • SVCD SVCD
  • DVD video recorders
  • camcorders radios
  • radio cassette recorders combined speakers
  • compact disc players (CD) computers, games Machine waiting.
  • a thermal interface material, by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
  • the liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
  • the metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 1:1.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
  • the carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
  • the model number of the alkenyl-containing siloxane is KH171.
  • the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
  • the preparation method of the thermally conductive interface material includes the following steps:
  • step S2 Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, vacuum and stir for 10 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, and then put the paddle and pot wall on Continue to vacuum and stir for 5 minutes under the shovel;
  • step S3 Add half of the carbon material to the mixture obtained in step S2, vacuum and stir for 5 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, and then shovel the material on the paddle and pot wall to continue Vacuum and stir for 5 minutes;
  • step S4 Add the remaining carbon material to the mixture obtained in step S3, vacuum and stir for 5 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, then shovel the material on the paddle and pot wall to continue vacuuming Stir for 5 minutes, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes;
  • step S1 Put the mixed material obtained in step S1 into a hydraulic injection extruder and spit it out through a needle nozzle.
  • the diameter of the needle nozzle is 2.5mm.
  • the material is arranged neatly in the container and stacked to 1/3 of the height. Then the material is removed in a vibrating compactor.
  • Tap the tap time is 40 minutes, the vibration frequency is 5 Hz, and the amplitude is 5 mm; after continuing to pile up to 2/3 height, the material is tapped by a vibrating compactor.
  • the tap time is 40 minutes, the vibration frequency is 5 Hz, and the amplitude It is 5mm; after continuing to pile up to a height of 3/3, the material is tapped in a vibrating compactor.
  • the tapping time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm.
  • the dimensions of the length, width, and height of the container are 250 mm, 150 mm, and 150 mm, respectively.
  • step (2) Put the rectangular parallelepiped container in step (2) in a vacuum drying box to evacuate to ⁇ -0.098MPa, then release the vacuum after 2 minutes, and tap the material with a vibrating compactor; then put it in the vacuum drying box to evacuate to ⁇ -0.098MPa, After 2 minutes, put the vacuum on, and the material will be compacted in the vibrating compactor; after pressing the heavy objects, put them in a vacuum drying oven to vacuum to ⁇ -0.098MPa, and put the vacuum after 2 minutes, then put the heavy objects in the vacuum drying box together Evacuate the vacuum to ⁇ -0.098MPa, and release the vacuum after 2 minutes.
  • the force applied by the weight to the container in step (3) and step (4) is 300 kgf.
  • a thermal interface material, by weight, the preparation raw materials include: 13 parts of liquid silica gel, 27 parts of metal powder, 7 parts of metal oxide, 20 parts of carbon material, 0.1 part of alkenyl-containing siloxane, and 11 parts of ceramic material .
  • the liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
  • the metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 0.8:1.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
  • the carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
  • the model number of the alkenyl-containing siloxane is KH171.
  • the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.3:1.
  • a thermal interface material based on parts by weight, the preparation raw materials include: 20 parts of liquid silica gel, 35 parts of metal powder, 13 parts of metal oxides, 30 parts of carbon materials, 0.5 parts of alkenyl-containing siloxane, and 20 parts of ceramic materials. .
  • the liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
  • the metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 1.2:1.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
  • the carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
  • the model number of the alkenyl-containing siloxane is KH171.
  • the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 0.9:1.
  • a thermal interface material based on parts by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
  • the liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
  • the metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 0.4:1.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
  • the carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
  • the model number of the alkenyl-containing siloxane is KH171.
  • the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
  • a thermal interface material based on parts by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
  • the liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
  • the metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 3:1.
  • the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
  • the carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
  • the model number of the alkenyl-containing siloxane is KH171.
  • the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
  • a thermally conductive interface material The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 0.5:1.
  • a thermally conductive interface material The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 3:1.
  • thermally conductive interface material the specific components are the same as in Example 1, except that the model number of the alkenyl-containing siloxane is KH560.
  • a thermal interface material the specific composition is the same as that of Example 1, the difference is that the molecular formula of the metal oxide is M x O y , where M is Al, x is 2, and y is 3; The average particle size is 600nm.
  • a thermal interface material the specific composition is the same as that of Example 1, the difference is that the metal powder is composed of aluminum powder with an average particle size of 10 microns and aluminum powder with an average particle size of 40 microns; The weight ratio of powder to 40 micron aluminum powder is 1:1.
  • a thermally conductive interface material The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 3 microns and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 1.1:1.
  • the test method refers to the standard ASTM D5470 to test the thermal conductivity of the thermally conductive material along the fiber orientation direction, unit: W/(m ⁇ K)
  • Hardness Test with a Shore OO hardness tester, put the thermal interface material under the needle insertion device of the hardness tester, wait for the device to make a beep 3 seconds later, and the data is stable, and record the data (the average value of five different positions) ), Unit: Shore OO. See Table 1 for details.
  • Example Thermal Conductivity hardness Example 1 50 49 Example 2 46 47 Example 3 48 49 Example 4 31 48 Example 5 25 38 Example 6 34 48
  • Example 7 28 35 Example 8 36 31 Example 9 33 49 Example 10 35 34 Example 11 37 32

Abstract

A high-performance heat conducting interface material and an application thereof, raw materials for the preparation thereof comprising, by weight proportions: 13-20 parts liquid silica gel, 27-35 parts metal powder, 7-13 parts metal oxide, 20-30 parts carbon material and 0.1-0.5 parts alkanyl-containing siloxane; the metal powder comprises at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder and tin powder.

Description

一种高性能导热界面材料及其应用A high-performance thermal interface material and its application 技术领域Technical field
本发明属于导热材料技术领域，具体涉及一种高性能导热界面材料及其应用。The invention belongs to the technical field of thermally conductive materials, and specifically relates to a high-performance thermally conductive interface material and its application.
背景技术Background technique
材料科学的不断发展使得导热材料在国防工业和民用材料中的应用比例逐年增大，具有质量轻、力学性能好、电绝缘性强、价格低等特点的导热材料成为未来发展的趋势，在电子工业发展迅速的今天有着很广泛的应用前景。电子工业产品如LED、微电子封装材料和半导体器件不断的向小型化、轻薄化和智能化方向发展，因此人们对材料的导热性能提出了更高的要求。The continuous development of material science has made the application proportion of thermal conductive materials in the defense industry and civil materials increase year by year. Thermal conductive materials with light weight, good mechanical properties, strong electrical insulation, and low price have become the trend of future development. Today, the industry is developing rapidly and has a wide range of application prospects. Electronic industry products such as LEDs, microelectronic packaging materials and semiconductor devices continue to develop in the direction of miniaturization, lightness and thinness, and intelligence. Therefore, people have put forward higher requirements for the thermal conductivity of the materials.
电子设备所使用的导热材料比如高散热材料、电子封装材料等往往需要具备优良的电绝缘性及高击穿电压等性能才得以满足使用要求。随着笔记本电脑、移动通讯等小型化电子设备体积不断减小，性能不断提高，产品发热量也随之显著增加。工作温度持续上升会使电子设备的稳定性和可靠性下降，并且缩短产品的使用寿命。为保证电子设备高效平稳地运行，制备高导热率、合适硬度的材料将设备内部产生的热量快速、有效地导出成为亟待解决的问题。Thermally conductive materials used in electronic devices, such as high heat dissipation materials, electronic packaging materials, etc., often need to have excellent electrical insulation and high breakdown voltage properties to meet the requirements of use. As the volume of miniaturized electronic devices such as notebook computers and mobile communications continues to decrease and their performance continues to improve, the heat generated by the product has also increased significantly. The continuous rise of operating temperature will reduce the stability and reliability of electronic equipment, and shorten the service life of the product. In order to ensure the efficient and stable operation of electronic equipment, it is an urgent problem to prepare materials with high thermal conductivity and suitable hardness to quickly and effectively dissipate the heat generated inside the equipment.
发明内容Summary of the invention
为了解决上述技术问题，本发明的第一个方面提供了一种高性能导热界面材料，其特征在于，按重量份计，制备原料包括：液体硅胶13-20份、金属粉体27-35份、金属氧化物7-13份、碳材料20-30份、含烯基硅氧烷0.1-0.5份；In order to solve the above technical problems, the first aspect of the present invention provides a high-performance thermal interface material, which is characterized in that, in parts by weight, the preparation raw materials include: 13-20 parts of liquid silica gel, 27-35 parts of metal powder , 7-13 parts of metal oxides, 20-30 parts of carbon materials, 0.1-0.5 parts of alkenyl-containing siloxane;
所述金属粉体包括铜粉、铝粉、银粉、铁粉、锌粉、镍粉、锡粉中的至少一种。The metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
作为一种优选的技术方案，所述金属粉体由平均粒径为1-10微米的金属粉体和平均粒径为30-50微米的金属粉体组成。As a preferred technical solution, the metal powder is composed of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns.
作为一种优选的技术方案，所述1-10微米金属粉体和30-50微米金属粉体的重量比为(0.8-1.2)：1。As a preferred technical solution, the weight ratio of the 1-10 micron metal powder to the 30-50 micron metal powder is (0.8-1.2):1.
作为一种优选的技术方案，所述金属氧化物的分子式为M xO y，其中M选自Zn、Cu、Al、Ag、Ni、Fe、Mg中的一种，x为1-2，y为1-3。 As a preferred technical solution, the molecular formula of the metal oxide is M x O y , where M is selected from one of Zn, Cu, Al, Ag, Ni, Fe, and Mg, x is 1-2, y For 1-3.
作为一种优选的技术方案，所述金属氧化物的平均粒径为400-800nm。As a preferred technical solution, the average particle size of the metal oxide is 400-800 nm.
作为一种优选的技术方案，所述碳材料选自碳纤维、碳纳米管、碳纳米线、石墨烯、氧化石墨烯中的至少一种。As a preferred technical solution, the carbon material is selected from at least one of carbon fibers, carbon nanotubes, carbon nanowires, graphene, and graphene oxide.
作为一种优选的技术方案，所述碳纤维的平均长度为50～200微米。As a preferred technical solution, the average length of the carbon fiber is 50-200 microns.
作为一种优选的技术方案，所述碳纤维的平均长度为150微米。As a preferred technical solution, the average length of the carbon fiber is 150 microns.
作为一种优选的技术方案，按重量份计，所述导热界面材料还包括陶瓷材料11-20份。As a preferred technical solution, based on parts by weight, the thermally conductive interface material further includes 11-20 parts of ceramic materials.
本发明的第二个方面提供了所述导热界面材料的应用，所述界面材料用于电子产品的散热。The second aspect of the present invention provides an application of the thermally conductive interface material, which is used for heat dissipation of electronic products.
有益效果：本发明所述导热界面材料，具有优越的导热性能，合适的硬度，能够很好的应用于电子产品领域的散热。Beneficial effects: The thermally conductive interface material of the present invention has superior thermal conductivity, suitable hardness, and can be well applied to heat dissipation in the field of electronic products.
具体实施方式detailed description
为了下面的详细描述的目的，应当理解，本发明可采用各种替代的变化和步骤顺序，除非明确规定相反。此外，除了在任何操作实例中，或者以其他方式指出的情况下，表示例如说明书和权利要求中使用的成分的量的所有数字应被理解为在所有情况下被术语“约”修饰。因此，除非相反指出，否则在以下说明书和所附权利要求中阐述的数值参数是根据本发明所要获得的期望性能而变化的近似值。至少并不是试图将等同原则的适用限制在权利要求的范围内，每个数值参数至少应该根据报告的有效数字的个数并通过应用普通舍入技术来解释。For the purpose of the following detailed description, it should be understood that various alternative changes and step sequences may be adopted in the present invention, unless the contrary is clearly specified. In addition, except in any operating examples, or where otherwise indicated, all numbers indicating amounts of ingredients used in, for example, the specification and claims should be understood as modified by the term "about" in all cases. Therefore, unless stated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximate values that vary according to the desired performance to be obtained in the present invention. At least it is not an attempt to limit the application of the principle of equivalence to the scope of the claims. Each numerical parameter should at least be interpreted based on the number of significant figures reported and through the application of ordinary rounding techniques.
尽管阐述本发明的广泛范围的数值范围和参数是近似值，但是具体实例中列出的数值尽可能精确地报告。然而，任何数值固有地包含由其各自测试测量中发现的标准偏差必然产生的某些误差。Although the numerical ranges and parameters that illustrate the broad range of the present invention are approximations, the numerical values listed in the specific examples are reported as accurately as possible. However, any numerical value inherently contains certain errors that inevitably result from the standard deviation found in its respective test measurement.
当本文中公开一个数值范围时，上述范围视为连续，且包括该范围的最小值及最大值，以及这种最小值与最大值之间的每一个值。进一步地，当范围是指整数时，包括该范围的最小值与最大值之间的每一个整数。此外，当提供多个范围描述特征或特性时，可以合并该范围。换言之，除非另有指明，否则本文中所公开之所有范围应理解为包括其中所归入的任何及所有的子范围。例如，从“1至10”的指定范围应视为包括最小值1与最大值10之间的任何及所有的子范围。范围1至10的示例性子范围包括但不限于1至6.1、3.5至7.8、5.5至10等。When a numerical range is disclosed herein, the above-mentioned range is regarded as continuous, and includes the minimum and maximum values of the range, and every value between such minimum and maximum values. Further, when the range refers to an integer, it includes every integer between the minimum value and the maximum value of the range. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be combined. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all sub-ranges subsumed therein. For example, a specified range from "1 to 10" should be regarded as including any and all sub-ranges between the minimum value of 1 and the maximum value of 10. Exemplary sub-ranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
为了解决上述问题，本发明提供了一种高性能导热界面材料，按重量份计，制备原料包括：液体硅胶13-20份、金属粉体27-35份、金属氧化物7-13份、碳材料20-30份、含烯基硅氧烷0.1-0.5份。In order to solve the above problems, the present invention provides a high-performance thermally conductive interface material. Based on parts by weight, the preparation raw materials include: 13-20 parts of liquid silica gel, 27-35 parts of metal powder, 7-13 parts of metal oxide, and carbon 20-30 parts of materials, 0.1-0.5 parts of alkenyl-containing siloxane.
作为一种优选的实施方式，所述导热界面材料，按重量份计，制备原料包括：液体硅胶15.92份、金属粉体31.45份、金属氧化物10.36份、碳材料26.64份、含烯基硅氧烷0.32份。As a preferred embodiment, the thermal interface material, based on parts by weight, prepares raw materials including: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, and alkenyl-containing silica 0.32 parts of alkane.
液体硅胶Liquid silicone
本申请中所述液体硅胶包括两个类型：一类是官能团处于分子结构两端液体硅胶；另一类是活性官能团在主链中呈无规分布的液体硅胶，所述液体硅胶具有流动快、固化条件温和、安全环保等优点。The liquid silica gel mentioned in this application includes two types: one type is liquid silica gel with functional groups at both ends of the molecular structure; the other type is liquid silica gel with active functional groups randomly distributed in the main chain. The liquid silica gel has fast flow, The advantages of mild curing conditions, safety and environmental protection.
作为一种实施方式，所述液体硅胶包括羟基改性聚二甲基硅氧烷型硅胶、羧基改性聚二甲基硅氧烷型硅胶、含硅氢键聚二甲基硅氧烷型硅胶中的至少一种。As an embodiment, the liquid silica gel includes hydroxyl-modified polydimethylsiloxane-type silica gel, carboxyl-modified polydimethylsiloxane-type silica gel, and silicon-hydrogen bond-containing polydimethylsiloxane-type silica gel. At least one of them.
作为一种优选的实施方式，所述液体硅胶的粘度为500-1000mPa·s。As a preferred embodiment, the viscosity of the liquid silica gel is 500-1000 mPa·s.
所述液体硅胶的粘度测试参考标准ISO3219，温度为25摄氏度。The viscosity test of the liquid silica gel refers to the standard ISO3219, and the temperature is 25 degrees Celsius.
本申请中，所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。In this application, the model of the liquid silica gel is Waker-9212 A/B, which was purchased from Wacker, Germany.
金属粉体Metal powder
所述金属粉体晶体内部存在着大量自由电子，通过自由电子的定向迁移传递电能和热能。例如，铝的热导率为190k/W·(m·K) -1，锌的热导率为121k/W·(m·K) -1，铜的热导率为398k/W·(m·K) -1，银的热导率为471k/W·(m·K) -1。 There are a large number of free electrons inside the metal powder crystals, and electric energy and heat energy are transferred through the directional migration of free electrons. For example, the thermal conductivity of aluminum is 190k/W·(m·K) -1 , the thermal conductivity of zinc is 121k/W·(m·K) -1 , and the thermal conductivity of copper is 398k/W·(m ·K) -1 , the thermal conductivity of silver is 471k/W·(m·K) -1 .
作为一种实施方式，所述金属粉体包括铜粉、铝粉、银粉、铁粉、锌粉、镍粉、锡粉中的至少一种。As an embodiment, the metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
作为一种实施方式，所述金属粉体为铝粉。As an embodiment, the metal powder is aluminum powder.
作为一种优选的实施方式，所述金属粉体为球形结构粉体。As a preferred embodiment, the metal powder is a spherical structure powder.
金属粒子的形状及粒径大小影响其在聚合物中的分布和粒子间堆积方式，从而影响在聚合物内部构筑导热道通的能力，影响其导热及其他性能。The shape and size of the metal particles affect their distribution in the polymer and the way they are stacked between the particles, thereby affecting the ability to build a heat conduction channel inside the polymer, and affecting its thermal conductivity and other properties.
作为一种优选的实施方式，所述金属粉体的平均粒径为1-70微米；优选地，所述金属粉体的平均粒径为5-40微米；As a preferred embodiment, the average particle size of the metal powder is 1-70 microns; preferably, the average particle size of the metal powder is 5-40 microns;
作为一种优选的实施方式，所述金属粉体由平均粒径为1-10微米的金属粉体和平均粒径为30-50微米的金属粉体组成；As a preferred embodiment, the metal powder is composed of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns;
优选地，所述1-10微米金属粉体和30-50微米金属粉体的重量比为(0.8-1.2)：1。Preferably, the weight ratio of the 1-10 micron metal powder to the 30-50 micron metal powder is (0.8-1.2):1.
进一步优选地，所述5微米金属粉体和40微米金属粉体的重量比为(0.8-1.2)： 1。Further preferably, the weight ratio of the 5 micron metal powder to the 40 micron metal powder is (0.8-1.2):1.
更进一步优选地，所述5微米金属粉体和40微米金属粉体的重量比为1：1。More preferably, the weight ratio of the 5 micron metal powder to the 40 micron metal powder is 1:1.
本申请中所述金属粉体在液体硅胶内形成导热网络结构，借助自由电子及声子振动提高硅胶的导热性能。The metal powder described in the present application forms a thermally conductive network structure in the liquid silica gel, and improves the thermal conductivity of the silica gel with the help of free electron and phonon vibration.
金属氧化物Metal oxide
本申请中所述金属氧化物导热性能低于金属粉体，但是具有良好的电绝缘性、耐磨性好、硬度高。The thermal conductivity of the metal oxide described in this application is lower than that of metal powder, but it has good electrical insulation, good wear resistance, and high hardness.
作为一种实施方式，所述金属氧化物的分子式为M xO y，其中M选自Zn、Cu、Al、Ag、Ni、Fe、Mg中的一种，x为1-2，y为1-3。 As an embodiment, the molecular formula of the metal oxide is M x O y , where M is selected from one of Zn, Cu, Al, Ag, Ni, Fe, and Mg, x is 1-2, and y is 1. -3.
作为一种优选的实施方式，所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1。 As a preferred embodiment, the molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1.
作为一种优选的实施方式，所述金属氧化物为球形结构粉体。As a preferred embodiment, the metal oxide is a powder with a spherical structure.
优选地，所述金属氧化物的平均粒径为400-800nm。Preferably, the average particle size of the metal oxide is 400-800 nm.
更优选地，所述金属氧化物的平均粒径为600nm。More preferably, the average particle size of the metal oxide is 600 nm.
碳材料Carbon material
本申请中，所述碳材料选自碳纤维、碳纳米管、碳纳米线、石墨烯、氧化石墨烯中的至少一种。In this application, the carbon material is selected from at least one of carbon fibers, carbon nanotubes, carbon nanowires, graphene, and graphene oxide.
作为一种优选的实施方式，所述碳材料为碳纤维。As a preferred embodiment, the carbon material is carbon fiber.
作为一种优选的实施方式，所述碳纤维的平均长度为50～200微米。As a preferred embodiment, the average length of the carbon fiber is 50-200 microns.
优选地，所述碳纤维的平均长度为150微米。Preferably, the average length of the carbon fiber is 150 microns.
本申请中所述碳纤维具有超高的导热性和力学强度，热导率可达到700W/(m·K)，碳纤维内部主要以六角形C原子的层晶格为结构基元，共价键是C原子间相互连接(键长＝0.1421mn)的主要形式；而各层结构的稳定主要依靠范德华力来维持，层面间距在0.3360-0.3440nm范围内。所述碳纤维特殊的微晶石墨结构使其在热传导过程中发挥巨大的散热优势。The carbon fiber described in this application has ultra-high thermal conductivity and mechanical strength, and the thermal conductivity can reach 700W/(m·K). The interior of the carbon fiber is mainly based on the layer lattice of hexagonal C atoms as the structural element, and the covalent bond is The main form of interconnection between C atoms (bond length = 0.1421mn); and the stability of each layer structure is mainly maintained by van der Waals force, and the inter-layer spacing is in the range of 0.3360-0.3440nm. The special microcrystalline graphite structure of the carbon fiber makes it play a huge heat dissipation advantage in the heat conduction process.
含烯基硅氧烷Alkenyl-containing siloxane
本申请中，所述金属粉体、金属氧化物、碳材料等具有较高的导热系数，但是由于缺乏活性基团，表面能较低，与液体硅胶的相容性较差，会影响导热材料的导热性、硬度等性能。本申请通过加入含烯基硅氧烷对金属粉体、金属氧化物、 碳材料进行表面处理，增加了彼此之间的相容性，提高了界面粘合力。In this application, the metal powder, metal oxide, carbon material, etc. have high thermal conductivity, but due to the lack of active groups, the surface energy is low, and the compatibility with liquid silica gel is poor, which will affect the thermal conductivity of the material. Its thermal conductivity, hardness and other properties. In this application, the surface treatment of metal powders, metal oxides, and carbon materials is performed by adding alkenyl-containing siloxane to increase the compatibility between each other and improve the interfacial adhesion.
作为一种优选的实施方式，所述含烯基硅氧烷选自1-乙烯基-1,1,3,3,3-五甲基二硅氧烷、1,3,5-三乙烯基-1,1,3,5,5-五甲基三硅氧烷、乙烯基三(二甲基硅氧烷基)硅烷、1,3-二乙烯基四乙氧基二硅氧烷、甲基丙烯酰氧基五甲基二硅氧烷、乙烯基三(三甲基硅氧烷基)硅烷、乙烯基三甲氧基硅烷中的至少一种。As a preferred embodiment, the alkenyl-containing siloxane is selected from 1-vinyl-1,1,3,3,3-pentamethyldisiloxane, 1,3,5-trivinyl -1,1,3,5,5-pentamethyltrisiloxane, vinyltris(dimethylsiloxane)silane, 1,3-divinyltetraethoxydisiloxane, methyl At least one of acryloyloxypentamethyldisiloxane, vinyltris(trimethylsiloxy)silane, and vinyltrimethoxysilane.
作为一种优选的实施方式，所述含烯基硅氧烷为乙烯基三甲氧基硅烷。As a preferred embodiment, the alkenyl-containing siloxane is vinyltrimethoxysilane.
本申请中，所述含烯基硅氧烷的型号为KH171。In this application, the model number of the alkenyl-containing siloxane is KH171.
陶瓷材料Ceramic material
作为一种优选的实施方式，按重量份计，所述导热界面材料还包括陶瓷材料11-20份。As a preferred embodiment, based on parts by weight, the thermally conductive interface material further includes 11-20 parts of ceramic materials.
作为一种优选的实施方式，按重量份计，所述导热界面材料还包括陶瓷材料15.31份。As a preferred embodiment, in terms of parts by weight, the thermally conductive interface material further includes 15.31 parts of ceramic materials.
本申请中所述陶瓷材料具有原子晶体形式和致密的结构，以声子导热为主，热导率很高。The ceramic material described in this application has an atomic crystal form and a dense structure, mainly conducts heat conduction by phonons, and has a high thermal conductivity.
作为一种实施方式，所述陶瓷材料选自碳化硅、氮化铝、氮化硅、硅酸铝、氧化锆中一种或多种。As an embodiment, the ceramic material is selected from one or more of silicon carbide, aluminum nitride, silicon nitride, aluminum silicate, and zirconium oxide.
作为一种优选的实施方式，所述陶瓷材料为氮化铝。As a preferred embodiment, the ceramic material is aluminum nitride.
所述氮化铝为共价键化合物，为六方纤锌矿结构，呈白色或灰白色，Al原子与相邻的N原子形成歧变的(AIN 4)四面体。AIN的理论密度为3.269，莫氏硬度7-8，在2200-22500摄氏度分解，在2000℃以内的高温非氧化气氛中稳定性很好，抗热震性也好。此外，所述氮化铝具有不受铝和其他熔融金属以及砷化稼侵蚀的特性，氮化铝还具有优良的电绝缘性和介电性质。 The aluminum nitride is a covalent bond compound with a hexagonal wurtzite structure, white or off-white, and Al atoms and adjacent N atoms form a dismutated (AIN 4 ) tetrahedron. AIN has a theoretical density of 3.269, a Mohs hardness of 7-8, and decomposes at 2200-22500 degrees Celsius. It has good stability and thermal shock resistance in a high-temperature non-oxidizing atmosphere within 2000 degrees Celsius. In addition, the aluminum nitride has the characteristics of not being corroded by aluminum and other molten metals and gallium arsenide, and aluminum nitride also has excellent electrical insulation and dielectric properties.
作为一种优选的实施方式，所述氮化铝为球形结构粉体。As a preferred embodiment, the aluminum nitride is a powder with a spherical structure.
作为一种优选的实施方式，所述氮化铝的平均粒径为0.5-5微米；As a preferred embodiment, the average particle size of the aluminum nitride is 0.5-5 microns;
作为一种优选的实施方式，所述氮化铝由平均粒径为0.5-2微米的氮化铝和平均粒径为4-6微米的氮化铝组成；As a preferred embodiment, the aluminum nitride is composed of aluminum nitride with an average particle size of 0.5-2 microns and aluminum nitride with an average particle size of 4-6 microns;
优选地，所述0.5-2微米氮化铝和4-6微米氮化铝的重量比为(0.9-1.3)：1。Preferably, the weight ratio of the 0.5-2 micron aluminum nitride to the 4-6 micron aluminum nitride is (0.9-1.3):1.
进一步优选地，所述1微米氮化铝和5微米氮化铝的重量比为(0.9-1.3)：1。Further preferably, the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is (0.9-1.3):1.
更进一步优选地，所述1微米氮化铝和5微米氮化铝的重量比为1.1：1。More preferably, the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
本申请通过在液体硅胶中加入27-35份金属粉体、7-13份金属氧化物、20-30份碳材料以及通过分步混合、定向取向等工艺，得到碳材料定向取向的导热材料。但是由于金属粉体、金属氧化物、陶瓷材料的种类以及尺寸，重量份等多因素都会对材料的导热性能造成很大影响，本申请人通过潜心研究发现当金属粉体、金属氧化物、陶瓷材料的重量份比为：(2-4)：1：(1-2)时，且所述金属粉体由平均粒径为1-10微米的金属粉体和平均粒径为30-50微米的金属粉体组成；所述氮化铝由平均粒径为0.5-2微米的氮化铝和平均粒径为4-6微米的氮化铝组成时，材料的性能达到最优化。可能是因为：金属粉体、金属氧化物或陶瓷材料的粒径较小时，比表面积较大；金属粉体、金属氧化物或陶瓷材料的粒径较大时，热传导性能较好，不同粒径的填料分布在硅胶中时，受限于填料的粒径、动能的影响，不同粒径、不同导热系数的填料相互接触，形成导热链，导热材料体系中相当于形成多个“并联电路”，热流从多个“并联电路”中通过，从而提高导热性能。另外，由于乙烯基三甲氧基硅烷的存在，改善了液体硅橡胶的溶液性质、填料表面能不相容、混料粘度较大的问题，得到的界面材料硬度范围为30～50ShoreOO，具有很好的加工性能，十分适用于各种电子产品领域的散热。In this application, by adding 27-35 parts of metal powder, 7-13 parts of metal oxide, 20-30 parts of carbon material to liquid silica gel, and through processes such as stepwise mixing and orientation orientation, a thermally conductive material with carbon material orientation orientation is obtained. However, due to the types and sizes of metal powders, metal oxides, and ceramic materials, multiple factors such as parts by weight will have a great impact on the thermal conductivity of the materials. The applicant has found through painstaking research that when metal powders, metal oxides, ceramics When the weight ratio of the material is: (2-4):1:(1-2), and the metal powder is composed of metal powder with an average particle size of 1-10 microns and an average particle size of 30-50 microns When the aluminum nitride is composed of aluminum nitride with an average particle size of 0.5-2 microns and aluminum nitride with an average particle size of 4-6 microns, the performance of the material is optimized. It may be because: when the particle size of the metal powder, metal oxide or ceramic material is small, the specific surface area is larger; when the particle size of the metal powder, metal oxide or ceramic material is large, the thermal conductivity is better, and the particle size is different When the filler is distributed in the silica gel, it is limited by the particle size and kinetic energy of the filler. Fillers with different particle sizes and different thermal conductivity contact each other to form a thermal conductive chain. The thermal conductive material system is equivalent to forming multiple "parallel circuits". Heat flow passes through multiple "parallel circuits" to improve thermal conductivity. In addition, due to the existence of vinyl trimethoxy silane, the solution properties of liquid silicone rubber, the incompatibility of filler surface energy, and the large viscosity of the mixture are improved. The hardness of the interface material obtained is in the range of 30-50 ShoreOO, which has a good performance. The processing performance is very suitable for heat dissipation in various electronic product fields.
所述导热界面材料的制备方法，包括以下步骤：The preparation method of the thermally conductive interface material includes the following steps:
(1)搅拌混合(1) Stir and mix
S1：在液体硅胶中添加含烯基硅氧烷、行星搅拌1-10min；S1: Add alkenyl-containing siloxane to liquid silica gel and stir for 1-10min with planets;
S2：向步骤S1得到的混合物中添加金属粉体、金属氧化物、陶瓷材料，行星抽真空搅拌5-20min；S2: Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, and the planetary vacuum is stirred for 5-20 minutes;
S3：向步骤S2得到的混合物中添加一半重量份的碳材料，行星抽真空搅拌1-30min；S3: Add half of the carbon material to the mixture obtained in step S2, and stir the planetary vacuum for 1-30 min;
S4：向步骤S3得到的混合物中添加剩余的碳材料，行星抽真空搅拌1-30min；S4: Add the remaining carbon material to the mixture obtained in step S3, and stir the planetary vacuum for 1-30 min;
(2)取向工艺：(2) Orientation process:
将步骤(1)得到的混合材料放进液压注射挤出机中，通过针嘴吐出，在长方体容器中条状排列整齐，堆积到1/2-1/4高度后，在振动密实机将材料振实，共2-4次。Put the mixed material obtained in step (1) into the hydraulic injection extruder, spit it out through the needle nozzle, and arrange it neatly in a rectangular parallelepiped container. After it is stacked to a height of 1/2-1/4, the material is mixed in a vibrating compactor Vibrate, a total of 2-4 times.
(3)真空压实：(3) Vacuum compaction:
将步骤(2)中长方体容器放真空干燥箱中抽真空至≤-0.098MPa，1-5分钟 后放真空，在振动密实机将材料振实，反复进行至少一次；压重物后再一起放真空干燥箱中抽真空至≤-0.098MPa，1-5分钟后放真空，反复进行至少一次；Put the rectangular parallelepiped container in step (2) in a vacuum drying oven to evacuate to ≤-0.098MPa, 1-5 minutes later, release the vacuum, tap the material in a vibrating compactor, repeat at least once; then place the weights together Vacuum in the vacuum drying box to ≤-0.098MPa, release the vacuum after 1-5 minutes, repeat at least once;
(4)高温固化：(4) High temperature curing:
将重物压在步骤(3)得到的容器上，放100-150℃烤箱30-90min。Press the weight on the container obtained in step (3), and put it in an oven at 100-150°C for 30-90 minutes.
(5)切片：(5) Slice:
冷却至室温将半成品取出，切成规定厚度片材，即得。Cool down to room temperature, take out the semi-finished product, and cut it into sheets of the specified thickness to obtain.
其中，步骤(3)和步骤(4)中所述重物施加给容器的力为100-500kgf。Wherein, the force applied by the weight to the container in step (3) and step (4) is 100-500 kgf.
优选地，步骤(3)和步骤(4)中所述重物施加给容器的力为300kgf。Preferably, the force applied by the weight to the container in step (3) and step (4) is 300 kgf.
作为一种优选的实施方式，所述导热界面材料的制备方法，包括以下步骤：As a preferred embodiment, the preparation method of the thermally conductive interface material includes the following steps:
(1)搅拌混合(1) Stir and mix
S1：在液体硅胶中添加含烯基硅氧烷、行星搅拌1-10min；S1: Add alkenyl-containing siloxane to liquid silica gel and stir for 1-10min with planets;
S2：向步骤S1得到的混合物中添加金属粉体、金属氧化物、陶瓷材料，行星抽真空搅拌5-20min，然后将桨和锅壁上物料铲下继续抽真空搅拌1-10min，再将桨和锅壁上物料铲下继续抽真空搅拌1-10min；S2: Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, vacuum and stir for 5-20 minutes on the planet, then shovel the paddle and the material on the pot wall and continue to vacuum and stir for 1-10 minutes, and then add the paddle Shovel the material on the pot wall and continue to vacuum and stir for 1-10min;
S3：向步骤S2得到的混合物中添加一半重量份的碳材料，行星抽真空搅拌1-10min，然后将桨和锅壁上物料铲下继续抽真空搅拌1-10min，再将桨和锅壁上物料铲下继续抽真空搅拌1-10min；S3: Add half of the carbon material to the mixture obtained in step S2, vacuum the planetary for 1-10min, then shovel the material on the paddle and the pot wall and continue to vacuum and stir for 1-10min, and then put the paddle and the pot wall on Continue to vacuum and stir for 1-10min under the shovel;
S4：向步骤S3得到的混合物中添加剩余的碳材料，行星抽真空搅拌1-10min，然后将桨和锅壁上物料铲下继续抽真空搅拌1-10min，再将桨和锅壁上物料铲下继续抽真空搅拌1-10min，再将桨和锅壁上物料铲下继续抽真空搅拌1-10min；S4: Add the remaining carbon material to the mixture obtained in step S3, vacuum and stir for 1-10min on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 1-10min, and then shovel the material on the paddle and pot wall Continue to vacuum and stir for 1-10min, then shovel the paddle and the material on the pot wall and continue to vacuum and stir for 1-10min
(2)取向工艺：(2) Orientation process:
将步骤(1)得到的混合材料放进液压注射挤出机中，通过针嘴吐出，针嘴口径为2.5mm，在长方体容器中条状排列整齐，堆积到1/2-1/4高度后，在振动密实机将材料振实，共2-4次。Put the mixed material obtained in step (1) into a hydraulic injection extruder and spit it out through a needle nozzle. The diameter of the needle nozzle is 2.5mm. They are arranged neatly in a rectangular parallelepiped container and stacked to 1/2-1/4 height. , The material is vibrated in the vibrating compaction machine for a total of 2-4 times.
(3)真空压实：(3) Vacuum compaction:
将步骤(2)中长方体容器放真空干燥箱中抽真空至≤-0.098MPa，1-5分钟后放真空，在振动密实机将材料振实；再放真空干燥箱中抽真空至≤-0.098MPa，1-5分钟后放真空，在振动密实机将材料振实；压重物后再一起放真空干燥箱中抽真空至≤-0.098MPa，1-5分钟后放真空，压重物后再一起放真空干燥箱中抽真 空至≤-0.098MPa，1-5分钟后放真空。Put the rectangular parallelepiped container in step (2) in a vacuum drying oven to evacuate to ≤-0.098MPa, 1-5 minutes later, vacuum, and vibrate the material with a vibrating compactor; then put it in a vacuum drying oven to evacuate to ≤-0.098 MPa, 1-5 minutes later, vacuum, vibrating compactor to compact the material; after pressing the heavy objects, put them in a vacuum drying oven and vacuum to ≤-0.098MPa, 1-5 minutes after the vacuum, after pressing the heavy objects Then put it in a vacuum drying oven to evacuate to ≤-0.098MPa, and then release the vacuum after 1-5 minutes.
(4)高温固化：(4) High temperature curing:
将重物压在步骤(3)得到的容器上，放100-150℃烤箱30-90min。Press the weight on the container obtained in step (3), and put it in an oven at 100-150°C for 30-90 minutes.
(5)切片：(5) Slice:
冷却至室温将半成品取出，切成规定厚度片材，即得。Cool down to room temperature, take out the semi-finished product, and cut it into sheets of the specified thickness to obtain.
优选地，(2)取向工艺中：将步骤(1)得到的混合材料放进液压注射挤出机中，通过针嘴吐出，针嘴口径为2.5mm，在长方体容器中条状排列整齐，堆积到1/3高度后，在振动密实机将材料振实，共3次。所述容器长、宽、高的尺寸分别为250mm、150mm、150mm。Preferably, (2) in the orientation process: put the mixed material obtained in step (1) into a hydraulic injection extruder, and spit it out through a needle nozzle with a diameter of 2.5mm, which is arranged neatly in a rectangular parallelepiped container and stacked After reaching 1/3 height, vibrate the material in a vibrating compactor for a total of 3 times. The dimensions of the length, width, and height of the container are 250 mm, 150 mm, and 150 mm, respectively.
具体操作为：将步骤S1得到的混合材料放进液压注射挤出机中，通过针嘴吐出，针嘴口径为2.5mm，在容器中条状排列整齐，堆积到1/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm；继续堆积到2/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm；继续堆积到3/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm。The specific operation is: put the mixed material obtained in step S1 into a hydraulic injection extruder and spit it out through a needle nozzle. The diameter of the needle nozzle is 2.5mm. The material is compacted by the compactor. The compaction time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm; after continuing to stack to 2/3 height, the material is compacted by the vibrating compactor. The compaction time is 40 minutes, and the vibration frequency It is 5Hz and the amplitude is 5mm; after continuing to pile up to the height of 3/3, the material is tapped by a vibrating compactor, the tapping time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm.
本发明的第二方面提供了所述的导热界面材料的应用，所述界面材料用于电子产品的散热。The second aspect of the present invention provides an application of the thermally conductive interface material, which is used for heat dissipation of electronic products.
所述电子产品可以列举的有手表、智能手机、电话、电视机、影碟机(VCD、SVCD、DVD)、录像机、摄录机、收音机、收录机、组合音箱、激光唱机(CD)、电脑、游戏机等。The electronic products can be listed as watches, smart phones, telephones, televisions, video disc players (VCD, SVCD, DVD), video recorders, camcorders, radios, radio cassette recorders, combined speakers, compact disc players (CD), computers, games Machine waiting.
下面通过实施例对本发明进行具体描述。有必要在此指出的是，以下实施例只用于对本发明作进一步说明，不能理解为对本发明保护范围的限制，该领域的专业技术人员根据上述本发明的内容做出的一些非本质的改进和调整，仍属于本发明的保护范围。Hereinafter, the present invention will be described in detail through examples. It is necessary to point out that the following examples are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Those skilled in the art have made some non-essential improvements based on the above-mentioned content of the present invention. And adjustments still belong to the protection scope of the present invention.
另外，如果没有其它说明，所用原料都是市售得到的。In addition, if there are no other instructions, all the raw materials used are commercially available.
实施例Example
实施例1Example 1
一种导热界面材料，按重量份计，制备原料包括：液体硅胶15.92份、金属粉体31.45份、金属氧化物10.36份、碳材料26.64份、含烯基硅氧烷0.32份、 陶瓷材料15.31份。A thermal interface material, by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。The liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
所述金属粉体由平均粒径为5微米的铝粉和平均粒径为40微米的铝粉组成；所述5微米铝粉和40微米铝粉的重量比为1：1。The metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 1:1.
所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1；所述金属氧化物的平均粒径为600nm。 The molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
所述碳材料为碳纤维，所述碳纤维的平均长度为150微米。The carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
所述含烯基硅氧烷的型号为KH171。The model number of the alkenyl-containing siloxane is KH171.
所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为1.1：1。The ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
所述导热界面材料的制备方法，包括以下步骤：The preparation method of the thermally conductive interface material includes the following steps:
(1)搅拌混合(1) Stir and mix
S1：在液体硅胶中添加含烯基硅氧烷、行星搅拌5min；S1: Add alkenyl-containing siloxane to the liquid silica gel and stir the planet for 5 minutes;
S2：向步骤S1得到的混合物中添加金属粉体、金属氧化物、陶瓷材料，行星抽真空搅拌10min，然后将桨和锅壁上物料铲下继续抽真空搅拌5min，再将桨和锅壁上物料铲下继续抽真空搅拌5min；S2: Add metal powder, metal oxides, and ceramic materials to the mixture obtained in step S1, vacuum and stir for 10 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, and then put the paddle and pot wall on Continue to vacuum and stir for 5 minutes under the shovel;
S3：向步骤S2得到的混合物中添加一半重量份的碳材料，行星抽真空搅拌5min，然后将桨和锅壁上物料铲下继续抽真空搅拌5min，再将桨和锅壁上物料铲下继续抽真空搅拌5min；S3: Add half of the carbon material to the mixture obtained in step S2, vacuum and stir for 5 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, and then shovel the material on the paddle and pot wall to continue Vacuum and stir for 5 minutes;
S4：向步骤S3得到的混合物中添加剩余的碳材料，行星抽真空搅拌5min，然后将桨和锅壁上物料铲下继续抽真空搅拌5min，再将桨和锅壁上物料铲下继续抽真空搅拌5min，再将桨和锅壁上物料铲下继续抽真空搅拌5min；S4: Add the remaining carbon material to the mixture obtained in step S3, vacuum and stir for 5 minutes on the planet, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes, then shovel the material on the paddle and pot wall to continue vacuuming Stir for 5 minutes, then shovel the material on the paddle and pot wall and continue to vacuum and stir for 5 minutes;
(2)取向工艺：(2) Orientation process:
将步骤S1得到的混合材料放进液压注射挤出机中，通过针嘴吐出，针嘴口径为2.5mm，在容器中条状排列整齐，堆积到1/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm；继续堆积到2/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm；继续堆积到3/3高度后，在振动密实机将材料振实，振实时间为40分钟，振动频率为5Hz，振幅为5mm。Put the mixed material obtained in step S1 into a hydraulic injection extruder and spit it out through a needle nozzle. The diameter of the needle nozzle is 2.5mm. The material is arranged neatly in the container and stacked to 1/3 of the height. Then the material is removed in a vibrating compactor. Tap, the tap time is 40 minutes, the vibration frequency is 5 Hz, and the amplitude is 5 mm; after continuing to pile up to 2/3 height, the material is tapped by a vibrating compactor. The tap time is 40 minutes, the vibration frequency is 5 Hz, and the amplitude It is 5mm; after continuing to pile up to a height of 3/3, the material is tapped in a vibrating compactor. The tapping time is 40 minutes, the vibration frequency is 5Hz, and the amplitude is 5mm.
所述容器长、宽、高的尺寸分别为250mm、150mm、150mm。The dimensions of the length, width, and height of the container are 250 mm, 150 mm, and 150 mm, respectively.
(3)真空压实：(3) Vacuum compaction:
将步骤(2)中长方体容器放真空干燥箱中抽真空至≤-0.098MPa，2分钟后放真空，在振动密实机将材料振实；再放真空干燥箱中抽真空至≤-0.098MPa，2分钟后放真空，在振动密实机将材料振实；压重物后再一起放真空干燥箱中抽真空至≤-0.098MPa，2分钟后放真空，压重物后再一起放真空干燥箱中抽真空至≤-0.098MPa，2分钟后放真空。Put the rectangular parallelepiped container in step (2) in a vacuum drying box to evacuate to ≤-0.098MPa, then release the vacuum after 2 minutes, and tap the material with a vibrating compactor; then put it in the vacuum drying box to evacuate to ≤-0.098MPa, After 2 minutes, put the vacuum on, and the material will be compacted in the vibrating compactor; after pressing the heavy objects, put them in a vacuum drying oven to vacuum to ≤-0.098MPa, and put the vacuum after 2 minutes, then put the heavy objects in the vacuum drying box together Evacuate the vacuum to ≤-0.098MPa, and release the vacuum after 2 minutes.
(4)高温固化：(4) High temperature curing:
将重物压在步骤(3)得到的容器上，放120℃烤箱60min。Press the weight on the container obtained in step (3), and put it in an oven at 120°C for 60 minutes.
(5)切片：(5) Slice:
冷却至室温将半成品取出，切成规定厚度片材，即得。Cool down to room temperature, take out the semi-finished product, and cut it into sheets of the specified thickness to obtain.
其中，步骤(3)和步骤(4)中所述重物施加给容器的力为300kgf。Wherein, the force applied by the weight to the container in step (3) and step (4) is 300 kgf.
实施例2Example 2
一种导热界面材料，按重量份计，制备原料包括：液体硅胶13份、金属粉体27份、金属氧化物7份、碳材料20份、含烯基硅氧烷0.1份、陶瓷材料11份。A thermal interface material, by weight, the preparation raw materials include: 13 parts of liquid silica gel, 27 parts of metal powder, 7 parts of metal oxide, 20 parts of carbon material, 0.1 part of alkenyl-containing siloxane, and 11 parts of ceramic material .
所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。The liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
所述金属粉体由平均粒径为5微米的铝粉和平均粒径为40微米的铝粉组成；所述5微米铝粉和40微米铝粉的重量比为0.8：1。The metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 0.8:1.
所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1；所述金属氧化物的平均粒径为600nm。 The molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
所述碳材料为碳纤维，所述碳纤维的平均长度为150微米。The carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
所述含烯基硅氧烷的型号为KH171。The model number of the alkenyl-containing siloxane is KH171.
所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为1.3：1。The ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.3:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例3Example 3
一种导热界面材料，按重量份计，制备原料包括：液体硅胶20份、金属粉 体35份、金属氧化物13份、碳材料30份、含烯基硅氧烷0.5份、陶瓷材料20份。A thermal interface material, based on parts by weight, the preparation raw materials include: 20 parts of liquid silica gel, 35 parts of metal powder, 13 parts of metal oxides, 30 parts of carbon materials, 0.5 parts of alkenyl-containing siloxane, and 20 parts of ceramic materials. .
所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。The liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
所述金属粉体由平均粒径为5微米的铝粉和平均粒径为40微米的铝粉组成；所述5微米铝粉和40微米铝粉的重量比为1.2：1。The metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 1.2:1.
所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1；所述金属氧化物的平均粒径为600nm。 The molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
所述碳材料为碳纤维，所述碳纤维的平均长度为150微米。The carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
所述含烯基硅氧烷的型号为KH171。The model number of the alkenyl-containing siloxane is KH171.
所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为0.9：1。The ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 0.9:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例4Example 4
一种导热界面材料，按重量份计，制备原料包括：液体硅胶15.92份、金属粉体31.45份、金属氧化物10.36份、碳材料26.64份、含烯基硅氧烷0.32份、陶瓷材料15.31份。A thermal interface material, based on parts by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。The liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
所述金属粉体由平均粒径为5微米的铝粉和平均粒径为40微米的铝粉组成；所述5微米铝粉和40微米铝粉的重量比为0.4：1。The metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 0.4:1.
所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1；所述金属氧化物的平均粒径为600nm。 The molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
所述碳材料为碳纤维，所述碳纤维的平均长度为150微米。The carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
所述含烯基硅氧烷的型号为KH171。The model number of the alkenyl-containing siloxane is KH171.
所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为1.1：1。The ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例5Example 5
一种导热界面材料，按重量份计，制备原料包括：液体硅胶15.92份、金属粉体31.45份、金属氧化物10.36份、碳材料26.64份、含烯基硅氧烷0.32份、陶瓷材料15.31份。A thermal interface material, based on parts by weight, the preparation raw materials include: 15.92 parts of liquid silica gel, 31.45 parts of metal powder, 10.36 parts of metal oxides, 26.64 parts of carbon materials, 0.32 parts of alkenyl-containing siloxane, and 15.31 parts of ceramic materials .
所述液体硅胶型号为Waker-9212 A/B，购买于德国瓦克。The liquid silica gel model is Waker-9212 A/B, purchased from Wacker, Germany.
所述金属粉体由平均粒径为5微米的铝粉和平均粒径为40微米的铝粉组成；所述5微米铝粉和40微米铝粉的重量比为3：1。The metal powder is composed of aluminum powder with an average particle size of 5 microns and aluminum powder with an average particle size of 40 microns; the weight ratio of the 5 microns aluminum powder to the 40 microns aluminum powder is 3:1.
所述金属氧化物的分子式为M xO y，其中M为Zn，x为1，y为1；所述金属氧化物的平均粒径为600nm。 The molecular formula of the metal oxide is M x O y , where M is Zn, x is 1, and y is 1; the average particle size of the metal oxide is 600 nm.
所述碳材料为碳纤维，所述碳纤维的平均长度为150微米。The carbon material is carbon fiber, and the average length of the carbon fiber is 150 microns.
所述含烯基硅氧烷的型号为KH171。The model number of the alkenyl-containing siloxane is KH171.
所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为1.1：1。The ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns, and the weight ratio of the 1 micron aluminum nitride to the 5 micron aluminum nitride is 1.1:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例6Example 6
一种导热界面材料，具体组分同实施例1，不同点在于，所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为0.5：1。A thermally conductive interface material. The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 0.5:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例7Example 7
一种导热界面材料，具体组分同实施例1，不同点在于，所述陶瓷材料由平均粒径为1微米的氮化铝和平均粒径为5微米的氮化铝组成，所述1微米氮化铝和5微米氮化铝的重量比为3：1。A thermally conductive interface material. The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 1 micron and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 3:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例8Example 8
一种导热界面材料，具体组分同实施例1，不同点在于，所述含烯基硅氧烷的型号为KH560。A thermally conductive interface material, the specific components are the same as in Example 1, except that the model number of the alkenyl-containing siloxane is KH560.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例9Example 9
一种导热界面材料，具体组分同实施例1，不同点在于，所述金属氧化物的分子式为M xO y，其中M为Al，x为2，y为3；所述金属氧化物的平均粒径为600nm。 A thermal interface material, the specific composition is the same as that of Example 1, the difference is that the molecular formula of the metal oxide is M x O y , where M is Al, x is 2, and y is 3; The average particle size is 600nm.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例10Example 10
一种导热界面材料，具体组分同实施例1，不同点在于，所述金属粉体由平均粒径为10微米的铝粉和平均粒径为40微米的铝粉组成；所述10微米铝粉和40微米铝粉的重量比为1：1。A thermal interface material, the specific composition is the same as that of Example 1, the difference is that the metal powder is composed of aluminum powder with an average particle size of 10 microns and aluminum powder with an average particle size of 40 microns; The weight ratio of powder to 40 micron aluminum powder is 1:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
实施例11Example 11
一种导热界面材料，具体组分同实施例1，不同点在于，所述陶瓷材料由平均粒径为3微米的氮化铝和平均粒径为5微米的氮化铝组成，所述3微米氮化铝和5微米氮化铝的重量比为1.1：1。A thermally conductive interface material. The specific composition is the same as that of Example 1. The difference is that the ceramic material is composed of aluminum nitride with an average particle size of 3 microns and aluminum nitride with an average particle size of 5 microns. The weight ratio of aluminum nitride to 5 micron aluminum nitride is 1.1:1.
所述导热界面材料的制备方法，具体步骤同实施例1。The specific steps of the preparation method of the thermally conductive interface material are the same as in Example 1.
性能测试Performance Testing
导热系数：测试方法参考标准ASTMD5470，测试导热材料沿纤维取向方向的导热系数，单位：W/(m·K)Thermal conductivity: The test method refers to the standard ASTM D5470 to test the thermal conductivity of the thermally conductive material along the fiber orientation direction, unit: W/(m·K)
硬度：用Shore OO硬度仪测试，将导热界面材料放入硬度测试仪的针入装置下，待设备3秒后出现“嘀”的声音后数据稳定，记录数据(为五个不同位置的平均值)，单位：Shore OO。具体见表1。Hardness: Test with a Shore OO hardness tester, put the thermal interface material under the needle insertion device of the hardness tester, wait for the device to make a beep 3 seconds later, and the data is stable, and record the data (the average value of five different positions) ), Unit: Shore OO. See Table 1 for details.
表1Table 1
实施例Example 导热系数Thermal Conductivity 硬度hardness
实施例1Example 1 5050 4949
实施例2Example 2 4646 4747
实施例3Example 3 4848 4949
实施例4Example 4 3131 4848
实施例5Example 5 2525 3838
实施例6Example 6 3434 4848
实施例7Example 7 2828 3535
实施例8Example 8 3636 3131
实施例9Example 9 3333 4949
实施例10Example 10 3535 3434
实施例11Example 11 3737 3232
以上所述，仅是本发明的较佳实施例而已，并非是对发明作其他形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或更改为等同变化的等效实施例，但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改，等同变化与改型，仍属于本发明技术方案的保护范围。The above are only the preferred embodiments of the present invention, and are not intended to limit the invention in other forms. Any person familiar with the profession may use the technical content disclosed above to change or modify the equivalent implementation of equivalent changes. Examples, but any simple modification, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (10)

  1. 一种高性能导热界面材料，其特征在于，按重量份计，制备原料包括：液体硅胶13-20份、金属粉体27-35份、金属氧化物7-13份、碳材料20-30份、含烯基硅氧烷0.1-0.5份；A high-performance thermal interface material, characterized in that, in parts by weight, the preparation raw materials include: 13-20 parts of liquid silica gel, 27-35 parts of metal powder, 7-13 parts of metal oxides, and 20-30 parts of carbon materials. , 0.1-0.5 parts of alkenyl-containing siloxane;
    所述金属粉体包括铜粉、铝粉、银粉、铁粉、锌粉、镍粉、锡粉中的至少一种。The metal powder includes at least one of copper powder, aluminum powder, silver powder, iron powder, zinc powder, nickel powder, and tin powder.
  2. 如权利要求1所述的导热界面材料，其特征在于，所述金属粉体由平均粒径为1-10微米的金属粉体和平均粒径为30-50微米的金属粉体组成。The thermally conductive interface material of claim 1, wherein the metal powder is composed of metal powder with an average particle size of 1-10 microns and metal powder with an average particle size of 30-50 microns.
  3. 如权利要求2所述的导热界面材料，其特征在于，所述1-10微米金属粉体和30-50微米金属粉体的重量比为(0.8-1.2)：1。The thermally conductive interface material according to claim 2, wherein the weight ratio of the 1-10 micron metal powder to the 30-50 micron metal powder is (0.8-1.2):1.
  4. 如权利要求1所述的导热界面材料，其特征在于，所述金属氧化物的分子式为M xO y，其中M选自Zn、Cu、Al、Ag、Ni、Fe、Mg中的一种，x为1-2，y为1-3。 The thermally conductive interface material of claim 1, wherein the molecular formula of the metal oxide is M x O y , wherein M is selected from one of Zn, Cu, Al, Ag, Ni, Fe, and Mg, x is 1-2 and y is 1-3.
  5. 如权利要求1或4所述的导热界面材料，其特征在于，所述金属氧化物的平均粒径为400-800nm。The thermally conductive interface material of claim 1 or 4, wherein the average particle size of the metal oxide is 400-800 nm.
  6. 如权利要求1所述的导热界面材料，其特征在于，所述碳材料选自碳纤维、碳纳米管、碳纳米线、石墨烯、氧化石墨烯中的至少一种。The thermally conductive interface material of claim 1, wherein the carbon material is selected from at least one of carbon fibers, carbon nanotubes, carbon nanowires, graphene, and graphene oxide.
  7. 如权利要求6所述的导热界面材料，其特征在于，所述碳纤维的平均长度为50～200微米。7. The thermally conductive interface material of claim 6, wherein the average length of the carbon fiber is 50-200 microns.
  8. 如权利要求7所述的导热界面材料，其特征在于，所述碳纤维的平均长度为150微米。8. The thermally conductive interface material of claim 7, wherein the average length of the carbon fiber is 150 microns.
  9. 如权利要求1所述的导热界面材料，其特征在于，按重量份计，所述导热界面材料还包括陶瓷材料11-20份。3. The thermally conductive interface material of claim 1, wherein the thermally conductive interface material further comprises 11-20 parts by weight of ceramic material.
  10. 一种如权利要求1-9任一项所述的导热界面材料的应用，其特征在于，所述界面材料用于电子产品的散热。An application of the thermally conductive interface material according to any one of claims 1-9, wherein the interface material is used for heat dissipation of electronic products.
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