CN116160737A - Anisotropic heat conduction multi-layer polymer composite material and preparation method thereof - Google Patents
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Abstract
The invention provides an anisotropic heat conduction multilayer polymer composite material and a preparation method thereof, wherein the composite material is obtained by laminating or winding a plurality of heat conduction filler/polymer composite films, the heat conduction filler/polymer composite films are formed by arranging heat conduction fillers on the surfaces of polymer films in an oriented and continuous way, so that an oriented heat conduction network parallel to the surfaces of the polymer films is formed on the surfaces of the polymer films, the heat conduction filler is one or more of boron nitride, graphite, graphene, carbon nano tubes and carbon fibers, and the polymer films are one or more of polypropylene, polyethylene, polystyrene, polycarbonate, acrylonitrile-styrene-butadiene copolymer, polyamide, polyethylene terephthalate, polyphenyl ether, polyphenylene sulfide, rigid polyvinyl chloride, polymethyl methacrylate, polyoxymethylene, polysulfone, polyimide, polytetrafluoroethylene, polytrifluoroethylene, polyperfluoroethylene, polybutylene terephthalate, chlorinated polyether, styrene-butadiene rubber, nitrile rubber, silicone rubber, butadiene rubber, polyisoprene, ethylene propylene rubber and chloroprene rubber.
Description
Technical Field
The invention relates to the field of preparation of heat conducting materials, in particular to an anisotropic heat conducting multilayer polymer composite material and a preparation method thereof.
Background
In electronic devices, a significant portion of the power loss is converted to heat, so that any microelectronic component with a certain resistance is an internal heat source component dissipating heat for the microelectronic device in operation, which directly causes an increase in the temperature and thermal stress of the electronic device, and poses a serious threat to the operational reliability of the microelectronic device. With the rapid development of miniaturized, integrated, lightweight, and digitized industrial electronic devices, thermal failure has become one of the most dominant failure modes in electronic packaging. It is counted that the reliability drops by 50% every time the device operating temperature increases by 10 ℃. Similar problems of wide and urgent need of heat dissipation and cooling exist for electronic equipment, power electronic equipment, photoelectric devices, micro/nano electromechanical systems, solid lighting, solar cells and the like in the aerospace and military fields. Traditional heat conducting materials such as metals, metal oxides, nitride ceramics and other nonmetallic materials cannot meet the requirements of the development of modern electronic technology because of the performance limitations of the materials. There is an urgent need to develop new high thermal conductivity polymer composite materials to accommodate the industry development requirements. By adopting a physical or chemical method, the inorganic filler with functional characteristics is added into the polymer, so that the advantages of portability, easy processing, corrosion resistance and the like of the polymer can be effectively combined with the functionality of the inorganic matters. Therefore, inorganic particles (metals, carbons, ceramics and the like) with good thermal conductivity are widely used as thermal conductive fillers in the preparation of thermal conductive composite materials, and the requirements of the fields of motor electric, electronic packaging, aerospace, military and the like on the thermal conductive materials are met.
CN114633531a discloses a preparation method of an anisotropic heat-conducting electromagnetic shielding nylon composite film, which prepares a multifunctional nylon composite film through layering design and assembly strategies, a continuous graphene heat-conducting network at the top is used as an anisotropic heat-conducting layer and an electromagnetic shielding layer after hot-press molding, a nickel-plated nylon film in the middle is used as an electromagnetic shielding reinforcing layer, and carbon fiber cloth at the bottom is used as a mechanical property improving layer. CN114350107a discloses a rapid-forming anisotropic heat-conducting composite material and a preparation method thereof,
the anisotropic heat conduction composite material is prepared from the following raw materials in parts by mass: 50-90 parts of graphite filler; 2-20 parts of carbon fiber filler; 2-20 parts of a high molecular polymer matrix; 1-3 parts of an interface modifier; 1-3 parts of organic solvent. CN113461989a discloses an anisotropic heat-conducting composite material and a preparation method thereof, wherein the raw materials comprise, by mass, 60-80 parts of high molecular polymer matrix, 6-8 parts of chopped fibers and 2-4 parts of dispersing agent. CN114369363a discloses a method and a mould for preparing a heat conducting gasket and the obtained heat conducting gasket, wherein the heat conducting gasket comprises a heat conducting filler layer; the heat-conducting filler layer comprises granular heat-conducting filler; adjacent heat conducting fillers are in direct contact to form a continuous three-dimensional heat conducting network containing internal gaps; the internal gaps of the three-dimensional heat conduction network are filled with high molecular polymers. CN106009445a discloses a heat conductive polymer nanocomposite and a preparation method thereof, after a hexagonal boron nitride isopropyl alcohol solution is treated by adopting a room temperature plasma technology, a nanoscale boron nitride nanodisk is obtained, and then the isopropyl alcohol solution of the treated layered boron nitride nanodisk is stirred with a polyvinyl alcohol solution; the composite material obtained after solvent evaporation is the heat conducting polymer nano composite material with anisotropic heat conductivity coefficient. The above all disclose the preparation of a series of thermally conductive polymers, and these prior art techniques mainly utilize external shearing forces in the process of extruding or casting polymer melt, suction filtering thermally conductive filler slurry, etc. or utilize external fields such as magnetic fields to orient the filler. Although the thermal conductivity shows some anisotropy, the fillers after alignment are still separated by the polymer, and the thermal conductivity of the composite is still not satisfactory. In order to further improve the thermal conductivity of the composite material, the prior art increases the thermal conductivity of the polymer by adding more amount of the thermal conductive material into the polymer matrix, however, the presence of a large amount of the thermal conductive additive greatly worsens the mechanical properties of the polymer, especially seriously reduces the plasticity and toughness of the polymer, so that the performance requirements of the polymer applied in the field of thermal diffusion cannot be met. In addition, some prior art increases filler dispersion and thus filler loading by interfacial agent modification, but interfacial agent modification increases interfacial scattering and reduces the thermal conductivity of the composite.
The conductive performance of the polymer matrix composite is not only related to the properties of the filler, including material structure, thermal conductivity, electrical conductivity, optical properties, size, appearance, geometry and the like, but also has close relation to the dispersion state of the filler in the polymer matrix and the structural order. CN105733065a discloses an anisotropic heat conducting polymer composite material and a preparation method thereof, and a method for preparing the heat conducting polymer composite material by using a melt blending method in combination with magnetic field induced heat conducting particle orientation arrangement. CN106832877a discloses a method for preparing a vertically oriented boron nitride/high polymer insulating heat conductive material, wherein a coating method is used to fill vertically oriented boron nitride in a polymer matrix to form a heat conductive polymer composite material. However, the high heat conduction ceramic powder which is directionally arranged by using a magnetic field in the polymer matrix composite material matrix is difficult to form a heat conduction network again, and the severe interfacial thermal resistance still exists between the filler and the resin, and when the filling amount is high, the mechanical property of the material is poor, so that the requirement of commercial application is difficult to meet; the scheme of using silane coupling agent or dopamine to modify boron nitride for coating the surface of a polymer film can introduce defects on the surface of the material, which is unfavorable for phonon transmission, thereby reducing the intrinsic heat conduction property of the material.
Therefore, development of an anisotropic heat conduction material with both heat conduction performance and mechanical performance is a problem to be solved.
Disclosure of Invention
The invention provides an anisotropic heat-conducting multilayer polymer composite material, which is obtained by laminating or winding a plurality of heat-conducting filler/polymer composite films, wherein the heat-conducting filler/polymer composite films are formed by arranging heat-conducting fillers on the surface of a polymer film in an oriented and continuous manner, so that an oriented heat-conducting network parallel to the surface of the polymer film is formed on the surface of the polymer film. The anisotropic heat conduction multilayer polymer composite material has the heat conduction coefficient higher than the coefficient of method Xiang Daore and has anisotropic heat conduction property.
The technical scheme of the invention is as follows:
the invention provides an anisotropic heat conduction multilayer polymer composite material, which is obtained by laminating or winding a plurality of heat conduction filler/polymer composite films, wherein the heat conduction filler/polymer composite films are formed by arranging heat conduction fillers on the surfaces of polymer films in an oriented and continuous way, so that an oriented heat conduction network parallel to the surfaces of the polymer films is formed on the surfaces of the polymer films, the heat conduction filler is one or more of boron nitride, graphite, graphene, carbon nano tubes and carbon fibers, and the polymer films are one or more of polypropylene, polyethylene, polystyrene, polycarbonate, acrylonitrile-styrene-butadiene copolymer, polyamide, polyethylene terephthalate, polyphenyl ether, polyphenylene sulfide, rigid polyvinyl chloride, polymethyl methacrylate, polyoxymethylene, polysulfone, polyimide, polytetrafluoroethylene, polytrifluoroethylene, poly perfluoroethylene propylene, polybutylene terephthalate, chlorinated polyether, styrene butadiene rubber, nitrile rubber, silicone rubber, butadiene rubber, polyisoprene rubber, ethylene propylene rubber and chloroprene rubber.
Further, in the heat conducting filler/polymer composite film, the volume percentage of the heat conducting filler is 0.01-90%.
Further, in the heat conductive filler/polymer composite film, the particle diameter of the heat conductive filler is 0.01-100 μm.
Further, in the heat conductive filler/polymer composite film, the thickness of the polymer film is 1 μm to 1cm.
Further, the number of layers of the heat conducting filler/polymer composite film is 2-1000.
Further, the composite material has a thermal conductivity enhancement ratio (TCE) of 0.39Wm at a volume fraction of 0.5% of the thermally conductive filler -1 K -1 /％。
In the invention, as the heat conducting filler forms a heat conducting network parallel to the surface of the polymer film on the surface of the polymer film, the propagation speed of heat in the direction of lamination (namely facing) of the composite material is better than that in the normal direction of lamination (namely normal phase), namely the heat conduction coefficient of the composite material facing is higher than that of the method Xiang Daore, and the anisotropic heat conduction property is realized.
Further, the heat conductivity coefficient of the heat conducting filler/polymer composite film is 0.1-10W/m.K, and the heat conductivity coefficient of the liquid phase is 0.1-5W/m.K.
The invention also provides a preparation method of the anisotropic heat conduction multilayer polymer composite material, which comprises the following steps:
step 1: providing a thermally conductive filler dispersion;
step 2: adding the heat conducting filler dispersion liquid into an immiscible double-layer system, wherein the heat conducting filler is oriented and dispersed at the middle interface of the immiscible double-layer system; the immiscible double-layer system comprises an immiscible upper layer system and a lower layer system, wherein the lower layer system is in a liquid phase, and the upper layer system is in a liquid phase or a gas phase;
step 3: immersing the polymer film in an underlying system of an immiscible bilayer system containing the thermally conductive filler, and moving the polymer film obliquely upwards to adhere the thermally conductive filler to the surface of the polymer film;
removing all the polymer film attached with the heat conducting filler from the immiscible double-layer system to obtain a heat conducting filler/polymer composite film;
step 4: and laminating or winding a plurality of the heat conducting filler/polymer composite films, and performing heat treatment to obtain the anisotropic heat conducting multilayer polymer composite material.
Further, in the step 1, the heat conducting filler dispersion liquid is formed by dispersing the heat conducting filler in one or more of ethanol, isopropanol, N' -dimethylformamide and N-methylpyrrolidone, wherein the mass concentration of the heat conducting filler is 0.1-10%.
Further, in step 2, the immiscible bilayer system includes any one of an n-hexane-water system, a cyclohexane-water system, an octane-water system, an air-water system, an acetone-water system, and a water-carbon tetrachloride system.
Further, in the step 2, the volume ratio of the heat conducting filler dispersion liquid to the lower layer system of the immiscible double-layer system is 0.001-1:1.
Further, in the step 3, in the process of transferring and pulling the polymer film from the immiscible bilayer system, an included angle between a direction of obliquely moving the polymer film upwards and a horizontal direction is 1-90 degrees, and the moving speed of the polymer film is 0.001-1 m/s.
Further, in the step 4, the heat treatment is to heat the laminated or wound heat conducting filler/polymer composite film for 2-24 hours at 30-150 ℃.
The invention has the following beneficial effects:
(1) Because the particles at the mutually-insoluble binary liquid phase interface are subjected to multiple actions of interfacial tension, electrostatic force among the particles and gravity, the stress balance is achieved at the liquid-liquid interface. By matching the interfacial tension with the surface energy of the particles, the surface energy is between the corresponding surface tension values of the two liquids, and the uniform distribution of the particles on the two-dimensional liquid phase interface can be effectively realized. According to the invention, by means of the dispersion effect of interfacial tension between the interfaces of the immiscible double-layer systems (gas-liquid or liquid-liquid) on the heat conducting filler, the two-dimensional heat conducting filler can be uniformly spread on the interface between the immiscible double-layer systems; when the polymer film passes through the middle interface of the immiscible double-layer system, the two-dimensional heat conducting fillers can be aligned and continuously arranged on the surface of the polymer film, and an oriented heat conducting network parallel to the surface of the polymer film is formed on the surface of the polymer film.
(2) The traditional method for mixing the heat conducting filler into the matrix takes the uniformity degree of filler mixing as a process evaluation index, the concentration of the filler in each part of the matrix is uniformly increased, and the efficiency is lower in the aspect of improving the heat conductivity enhancement ratio of the composite material. According to the technical scheme, the distribution of the heat conducting filler in the polymer film matrix is limited in a two-dimensional area through interfacial tension and lamination process, the filler concentration is high in the area, the distribution is concentrated, the heat conducting filler is fully contacted, and the heat conducting filler has a remarkable effect on improving the heat conductivity of the composite material.
(3) The thermal conductivity enhancement ratio (TCE) of the h-BN/silicone rubber composite thermal conductive material prepared by the technical proposal reaches 0.39W/m under the condition that the volume ratio of the thermal conductive filler is 0.5 percent - K/%, and a composite material (TCE 0.005-0.323 Wm) with h-BN reported as a filler (filler ratio 1.3% -99%) -1 K -1 Compared with the prior art, the technical scheme is favorable for greatly improving the heat conductivity of the composite material under the condition of low packing ratio.
Drawings
Fig. 1 is a schematic diagram of an interfacial transfer thermally conductive filler.
Fig. 2 is a schematic structural diagram of an anisotropically thermally conductive multilayer polymer composite. In fig. 2, 1 is a container, 2 is a heat conductive filler, 3 is a polymer film, 4 is an intermediate interface of an immiscible bilayer system, 5 is a polymer film, and 6 is a heat conductive filler.
Fig. 3 is a scanning electron microscope facing photograph of an anisotropically thermally conductive multilayer polymer composite.
Fig. 4 is a cross-sectional scanning electron micrograph of an anisotropically thermally conductive multilayer polymer composite.
Fig. 5 is a graph of the thermal conductivity of the h-BN thermally conductive filler polymer composite versus the volume fraction of the thermally conductive filler, wherein the abscissa of fig. 5 is the volume fraction of the thermally conductive filler in the composite, and the ordinate is the thermal conductivity of the composite, i.e., the thermal conductivity enhancement ratio TCE, per unit volume fraction.
Detailed Description
The invention is described in detail below with reference to examples:
example 1
The anisotropic heat conducting multilayer polymer composite material is obtained by laminating 200 heat conducting filler/polymer composite films, wherein the heat conducting filler/polymer composite films are formed by arranging heat conducting fillers on the surface of the polymer films in an oriented and continuous manner, so that an oriented heat conducting network parallel to the surface of the polymer films is formed on the surface of the polymer films, the heat conducting filler is boron nitride, the polymer films are made of silicon rubber, the volume percentage of the heat conducting filler is 0.5%, the particle size of the heat conducting filler is 10-18 mu m, and the thickness of the heat conducting filler is 1-5 mu m. The thickness of the polymer film was 0.2mm.
The preparation method comprises the following steps:
step 1: adding 1g of boron nitride (with the particle size of 10-18 mu m) into 100g of ethanol, and performing ultrasonic treatment for 2 hours at 100W to obtain 1wt.% of boron nitride dispersion liquid;
step 2: adding 10mL of boron nitride dispersion liquid into 1000mL of water, and after boron nitride is uniformly dispersed on the water surface, obliquely placing a silicon rubber film with the length of 50cm, the width of 30cm and the thickness of 0.2mm below the water surface, wherein the included angle between the silicon rubber film and the horizontal direction is 30 degrees; moving the silicon rubber upward in an inclined direction at a rate of 5mm/s so that boron nitride adheres to the surface of the silicon rubber film;
step 3: completely removing the silicon rubber film from the water, and drying at 60 ℃ for 60min to obtain a boron nitride/silicon rubber composite film;
step 4: cutting the boron nitride/silicon rubber composite film into strips with the width of 5mm, laminating 200 layers of the composite film by adopting a manual mode, and then placing the composite film in a 100 ℃ oven for heat treatment for 12 hours to obtain the anisotropic heat-conducting multilayer polymer composite material.
The thermal conductivity of the composite material is 0.325W/mK, and the thermal conductivity of the composite material is 0.136W/mK.
The scanning electron microscope photo of the obtained anisotropic heat conduction multi-layer polymer composite material is shown in fig. 3. As can be seen from fig. 3, the boron nitride thermally conductive filler is directionally distributed on the surface of the silicone rubber film.
A cross-sectional scanning electron micrograph of the resulting anisotropic conductive multilayer polymer composite is shown in FIG. 4. As can be seen from fig. 4, the boron nitride thermally conductive filler is capable of forming a thermally conductive network on the surface of the polymer film parallel to the surface of the polymer film.
The larger the TCE number, the greater the ability of the thermally conductive filler to increase the thermal conductivity of the polymer. Typically, the material cost of thermally conductive fillers is higher than that of polymers, so lower thermally conductive filler volume fractions and higher TCE mean a more efficient thermal conductivity enhancement solution. As shown in fig. 5, compared with the results reported in the literature, the technical scheme provided by the invention can greatly improve the thermal conductivity of the polymer composite material under the condition of filling a small amount of thermal conductive material.
Example 2
The anisotropic heat conducting multilayer polymer composite material is obtained by winding 100 heat conducting filler/polymer composite films, wherein the heat conducting filler/polymer composite films are arranged on the surface of the polymer films in an oriented and continuous way for forming an oriented heat conducting network parallel to the surface of the polymer films on the surface of the polymer films, the heat conducting filler is boron nitride, the polymer films are made of polyurethane, the volume percentage of the heat conducting filler is 0.3%, the particle size of the heat conducting filler is 10-18 mu m, and the thickness of the heat conducting filler is 1-5 mu m. The thickness of the polymer film was 0.3mm.
The preparation method comprises the following steps:
step 1: adding 1g of boron nitride (with the particle size of 10-18 mu m) into 100g of isopropanol, and performing ultrasonic treatment at 100W for 2 hours to obtain 1wt.% of boron nitride dispersion;
step 2: adding 5mL of boron nitride dispersion liquid into 1000mL of water, and after boron nitride is uniformly dispersed on the water surface, obliquely placing a polyurethane film with the length of 30cm, the width of 20cm and the thickness of 0.3mm below the water surface, wherein the included angle between the polyurethane film and the horizontal direction is 40 degrees; moving the polyurethane upward in an oblique direction at a rate of 3mm/s to adhere boron nitride to the polyurethane film surface;
step 3: completely removing the polyurethane film from the water, and drying at 60 ℃ for 60min to obtain a boron nitride/polyurethane composite film;
step 4: mechanically winding a boron nitride/polyurethane composite film for 100 layers, and then placing the boron nitride/polyurethane composite film in an oven at 80 ℃ for heat treatment for 12 hours to obtain an anisotropic heat-conducting multilayer polymer composite material;
the test shows that the thermal conductivity of the composite material is 0.278W/m.K, and the thermal conductivity of the composite material is 0.06W/m.K.
Example 3
The anisotropic heat conducting multilayer polymer composite material is obtained by winding 100 heat conducting filler/polymer composite films, wherein the heat conducting filler/polymer composite films are arranged on the surface of the polymer films in an oriented and continuous way, so that an oriented heat conducting network parallel to the surface of the polymer films is formed on the surface of the polymer films, the heat conducting filler is graphene, the polymer films are made of silicon rubber, the volume percentage of the heat conducting filler is 0.1%, the particle size of the heat conducting filler is 0.1-0.5 mu m, and the thickness of the heat conducting filler is 0.1-0.2 mu m. The thickness of the polymer film was 0.2mm.
The preparation method comprises the following steps:
step 1: adding 0.1g of graphene (particle size of 0.1-0.5 μm) into 100g of N-methylpyrrolidone, and performing ultrasonic treatment at 100W for 2 hours to obtain 0.1wt.% of graphene dispersion;
step 2: adding 10mL of graphene dispersion liquid into an n-hexane-water system (100 mL of n-hexane and 1000mL of water), and after graphene is uniformly dispersed at an intermediate interface, obliquely placing a silicon rubber film with the length of 50cm, the width of 30cm and the thickness of 0.2mm below the water surface, wherein the included angle between the silicon rubber film and the horizontal direction is 40 degrees; moving the silicon rubber upwards at a speed of 5mm/s in an inclined direction to enable graphene to be attached to the surface of the silicon rubber film;
step 3: completely removing the silicon rubber film from the water, and drying at 60 ℃ for 60min to obtain a graphene/silicon rubber composite film;
step 4: cutting the graphene/silicon rubber composite film into strips with the width of 5mm, laminating 100 layers of the composite film by adopting a manual mode, and then placing the composite film in an oven with the temperature of 150 ℃ for heat treatment for 6 hours to obtain the anisotropic heat-conducting multilayer polymer composite material.
The test shows that the thermal conductivity of the composite material is 9.13W/mK, and the thermal conductivity of the composite material is 0.146W/mK.
Example 4
The anisotropic heat conducting multilayer polymer composite material is obtained by winding 100 heat conducting filler/polymer composite films, wherein the heat conducting filler/polymer composite films are formed by arranging the heat conducting fillers on the surface of the polymer films in an oriented and continuous way, so that an oriented heat conducting network parallel to the surface of the polymer films is formed on the surface of the polymer films, the heat conducting fillers are carbon nano tubes, the polymer films are made of polyurethane, the volume percentage of the heat conducting fillers is 0.1%, the length of the heat conducting fillers is 10-100 mu m, and the diameter of the heat conducting fillers is 0.1-0.2 mu m. The thickness of the polymer film was 0.3mm.
The preparation method comprises the following steps:
step 1: adding 0.3g of carbon nano tube (particle size is 10-100 mu m, length-diameter ratio is 50-1000) into 100g of N, N' -dimethylformamide, and performing ultrasonic treatment for 2 hours under 100W to obtain 0.3wt.% of carbon nano tube dispersion liquid;
step 2: adding the 1mL of carbon nanotube dispersion liquid into an n-hexane-water system (100 mL of n-hexane and 500mL of water), and after the carbon nanotubes are uniformly dispersed at the middle interface, obliquely placing a polyurethane film with the length of 30cm, the width of 20cm and the thickness of 0.3mm below the water surface, wherein the included angle between the polyurethane film and the horizontal direction is 45 degrees; moving polyurethane upwards in an inclined direction at a rate of 5mm/s to attach carbon nanotubes to the surface of the polyurethane film;
step 3: completely removing the polyurethane film from the water, and drying at 60 ℃ for 60min to obtain a carbon nano tube/polyurethane composite film;
step 4: mechanically winding 150 layers of carbon nano tube/polyurethane composite film, and then placing the carbon nano tube/polyurethane composite film in an oven at 80 ℃ for heat treatment for 12 hours to obtain an anisotropic heat-conducting multilayer polymer composite material;
the test shows that the thermal conductivity of the composite material is 9.73W/m.K, and the thermal conductivity of the composite material is 0.08W/m.K.
Example 5
The anisotropic heat conducting multilayer polymer composite material is obtained by winding 100 heat conducting fillers/polymer composite membranes, wherein the heat conducting fillers/polymer composite membranes are arranged on the surface of the polymer membranes in an oriented and continuous way, so that an oriented heat conducting network parallel to the surface of the polymer membranes is formed on the surface of the polymer membranes, the heat conducting fillers are boron nitride, the polymer membranes are made of TPO, the volume percentage of the heat conducting fillers is 0.1%, the particle size of the heat conducting fillers is 10-18 mu m, and the thickness of the heat conducting fillers is 1-5 mu m. The thickness of the polymer film was 0.1mm.
The preparation method comprises the following steps:
step 1: adding 1g of boron nitride (with the particle size of 10-18 mu m) into 100g of isopropanol, and performing ultrasonic treatment at 100W for 2 hours to obtain 1wt.% of boron nitride dispersion;
step 2: adding 5mL of boron nitride dispersion liquid into 1000mL of water, and after boron nitride is uniformly dispersed on the water surface, obliquely placing TPO (thermoplastic polyolefin) membranes with the length of 30cm, the width of 20cm and the thickness of 0.1mm below the water surface, wherein the included angle between the TPO membranes and the horizontal direction is 45 degrees; moving the TPO membrane upward in an inclined direction at a rate of 3mm/s to adhere boron nitride to the TPO membrane surface;
step 3: completely removing TPO membrane from water, and drying at 60deg.C for 60min to obtain boron nitride/TPO composite membrane;
step 4: and pressurizing 100 layers of the boron nitride/TPO composite membrane aligned lamination by 0.1MPa, and then placing the boron nitride/TPO composite membrane in an oven at 130 ℃ for 1h to obtain the anisotropic heat-conducting multilayer polymer composite material.
Through testing, when the filling rate of the obtained composite material is 0.5wt%, the heat conductivity of the composite material is 0.87W/m.K, and the heat conductivity of the composite material is 0.29W/m.K.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the present invention in any other way, but is intended to cover any modifications or equivalent variations according to the technical spirit of the present invention, which fall within the scope of the present invention as defined by the appended claims.
Claims (13)
1. The anisotropic heat-conducting multilayer polymer composite material is characterized in that the composite material is obtained by laminating or winding a plurality of heat-conducting filler/polymer composite films, wherein the heat-conducting filler/polymer composite films are formed by arranging heat-conducting fillers on the surfaces of polymer films in an oriented and continuous manner, so that an oriented heat-conducting network parallel to the surfaces of the polymer films is formed on the surfaces of the polymer films, the heat-conducting fillers are one or more of boron nitride, graphite, graphene, carbon nano tubes and carbon fibers, and the polymer films are one or more of polypropylene, polyethylene, polystyrene, polycarbonate, acrylonitrile-styrene-butadiene copolymer, polyamide, polyethylene terephthalate, polyphenyl ether, polyphenylene sulfide, rigid polyvinyl chloride, polymethyl methacrylate, polyoxymethylene, polysulfone, polyimide, polytetrafluoroethylene, polytrifluoroethylene, polyperfluoroethylene propylene, polybutylene terephthalate, chlorinated polyether, styrene butadiene rubber, nitrile rubber, silicone rubber, butadiene rubber, polyisoprene, ethylene propylene rubber and chloroprene rubber.
2. The anisotropic conductive multilayer polymer composite of claim 1, wherein the volume percentage of the thermally conductive filler in the thermally conductive filler/polymer composite film is 0.01 to 90%.
3. The anisotropic conductive multilayer polymer composite according to claim 2, wherein the particle size of the conductive filler is 0.01 to 100 μm in the conductive filler/polymer composite film.
4. An anisotropic, thermally conductive multilayer polymer composite as in claim 3 wherein the thickness of the polymer film in the thermally conductive filler/polymer composite film is from 1 μm to 1cm.
5. The anisotropic, thermally conductive multilayer polymer composite of claim 4, wherein the number of layers of the thermally conductive filler/polymer composite film is 2 to 1000.
6. An anisotropic, thermally conductive multilayer polymer composite as claimed in claim 1 or 2, wherein,the thermal conductivity enhancement ratio (TCE) of the composite material reaches 0.39Wm under the condition that the volume fraction of the thermal conductive filler is 0.5 percent -1 K -1 /％。
7. An anisotropic heat conductive multilayer polymer composite according to claim 1 or 2, wherein the heat conductive filler/polymer composite film has a heat conductivity of 0.1 to 10W/m-K for the facing direction and 0.1 to 5W/m-K for the normal phase.
8. A method of preparing an anisotropic, thermally conductive multilayer polymer composite as claimed in any of claims 1 to 7, said method comprising the steps of:
step 1: providing a thermally conductive filler dispersion;
step 2: adding the heat conducting filler dispersion liquid into an immiscible double-layer system, wherein the heat conducting filler is oriented and dispersed at the middle interface of the immiscible double-layer system; the immiscible double-layer system comprises an immiscible upper layer system and a lower layer system, wherein the lower layer system is in a liquid phase, and the upper layer system is in a liquid phase or a gas phase;
step 3: immersing the polymer film in an underlying system of an immiscible bilayer system containing the thermally conductive filler, and moving the polymer film obliquely upwards to adhere the thermally conductive filler to the surface of the polymer film;
removing all the polymer film attached with the heat conducting filler from the immiscible double-layer system to obtain a heat conducting filler/polymer composite film;
step 4: and laminating or winding a plurality of the heat conducting filler/polymer composite films, and performing heat treatment to obtain the anisotropic heat conducting multilayer polymer composite material.
9. The method for producing an anisotropic heat conductive multilayer polymer composite according to claim 8, wherein in step 1, the heat conductive filler dispersion is a dispersion of the heat conductive filler in one or more of ethanol, isopropanol, N' -dimethylformamide and N-methylpyrrolidone, and the mass concentration of the heat conductive filler is 0.1 to 10%.
10. The method for preparing an anisotropic conductive multilayer polymer composite according to claim 9, wherein in step 2, the immiscible bilayer system comprises any one of n-hexane-water system, cyclohexane-water system, octane-water system, air-water system, acetone-water and water-carbon tetrachloride system.
11. The method for preparing an anisotropic heat conductive multilayer polymer composite according to claim 10, wherein in step 2, the volume ratio of the heat conductive filler dispersion liquid to the lower layer system of the immiscible bilayer system is 0.001-1:1.
12. The method for preparing an anisotropic heat conductive multilayer polymer composite according to claim 11, wherein in step 3, in the process of transferring and pulling the polymer film from the immiscible bilayer system, an included angle between a direction of obliquely moving the polymer film upwards and a horizontal direction is 1-90 °, and a moving speed of the polymer film is 0.001-1 m/s.
13. The method for preparing an anisotropic heat conductive multilayer polymer composite according to claim 12, wherein in the step 4, the heat treatment is to heat the laminated or wound heat conductive filler/polymer composite film at 30 to 150 ℃ for 2 to 24 hours.
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| CN116874826B (en) * | 2023-07-25 | 2023-12-22 | 常州宏巨电子科技有限公司 | Heat-conducting silicone rubber composite material with directional arrangement of fillers and preparation method thereof |
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