CN113088037B - Heat dissipation material with high heat conductivity coefficient and high radiation coefficient and preparation method thereof - Google Patents
Heat dissipation material with high heat conductivity coefficient and high radiation coefficient and preparation method thereof Download PDFInfo
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- CN113088037B CN113088037B CN202110392654.3A CN202110392654A CN113088037B CN 113088037 B CN113088037 B CN 113088037B CN 202110392654 A CN202110392654 A CN 202110392654A CN 113088037 B CN113088037 B CN 113088037B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention belongs to the technical field of heat dissipation materials, and discloses a heat dissipation material with high heat conductivity and high emissivity and a preparation method thereof, wherein the heat dissipation material is prepared from the following components: graphite, carbon nano tubes, resin, fiber reinforced filler, a curing agent and a diluent; the graphite is oxidized graphite or expanded graphite. The heat dissipation material has the characteristics of corrosion resistance, high heat conductivity coefficient and high heat radiation coefficient, and can be processed into various heat dissipation parts by adopting mould pressing or injection molding.
Description
Technical Field
The invention belongs to the technical field of heat dissipation materials, and particularly relates to a heat dissipation material with high heat conductivity coefficient and high radiation coefficient and a preparation method thereof.
Background
With the continuous development of industrial production and scientific technology, people have higher and higher requirements on the comprehensive performance of heat conducting materials, and the traditional metal materials cannot meet the use requirements of some special occasions. Due to the increase of power and performance of the present electronic equipment, the heat generation amount is inevitably increased, and if the heat cannot be efficiently dissipated, the heat will be rapidly accumulated and increased, so that the device cannot normally work, and the level of heat dissipation performance becomes an important factor influencing the service life of the electronic equipment.
Based on this, it is required to develop a heat dissipating material excellent in combination of high reliability and high heat dissipation property in place of the conventional metal material. Although the traditional heat-conducting plastic has the characteristics of light weight, chemical corrosion resistance, easiness in processing and forming, excellent electrical insulation performance, excellent mechanical and fatigue resistance performance and the like, the heat-radiating effect is insufficient, the heat of a heat source cannot be timely dissipated, and finally the heat source is damaged due to overhigh temperature.
Therefore, the development of high-thermal-conductivity and high-heat-dissipation polymer materials is the key point for ensuring better development of the electrical appliance industry, has received more and more attention from people, and is gradually a hot spot for international and domestic research and development.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a heat dissipation material with high heat conductivity coefficient and high emissivity coefficient and a preparation method thereof, the heat dissipation material has the characteristics of corrosion resistance, high heat conductivity coefficient and high thermal emissivity coefficient, and can be processed into various heat dissipation parts by adopting mould pressing or injection molding.
The invention provides a heat dissipation material which is prepared from the following components in parts by weight: graphite, carbon nano tubes, resin, fiber reinforced filler, a curing agent and a diluent; the graphite is graphite oxide or expanded graphite.
The invention takes the graphite oxide and the expanded graphite as raw materials instead of the graphene, because the graphene powder has a stacking effect and can not be fully dispersed in a resin system in the using process, the performance of products is reduced, and the graphite oxide and the expanded graphite can be peeled in a liquid solvent system to obtain the graphene, so the defects are avoided, and the dispersing effect is effectively improved. According to the invention, the resin is modified together by the carbon nano tube and the stripped graphene, so that the heat conduction advantages of the graphene with a lamellar structure and the carbon nano tube with a large length-diameter ratio are fully utilized, the heat of a heating source can be quickly led out, and the heat can be efficiently diffused to other media in a radiation mode, so that the heat radiation effect incomparable with other heat conduction materials is achieved, the temperature of the heat source can reach a constant temperature state for a long time, and the performance stability of the heat source is protected most effectively; meanwhile, the graphene and the carbon nano tube can be more fully fused with resin by combined use, and the dispersion effect of the graphene and carbon nano tube is incomparable with the effect of fusing pure graphene powder or the carbon nano tube with resin.
Preferably, the heat dissipation material is prepared from the following components in parts by weight: 1-20 parts of graphite, 1-5 parts of carbon nano tubes, 50-90 parts of resin, 20-40 parts of fiber reinforced filler, 2-10 parts of curing agent and 200-450 parts of diluent.
Preferably, the resin is selected from at least one of epoxy resin, phenolic resin or unsaturated polyester resin.
Preferably, the fibrous reinforcing filler is selected from at least one of glass fibers, carbon fibers, metal fibers, ceramic fibers or aramid fibers.
Preferably, the curing agent is selected from at least one of ethylenediamine, triethylamine, triethanolamine, diethylenetriamine, maleic anhydride, phthalic anhydride, amino resin, urea resin, furfural resin, or polyamide.
Preferably, the diluent is selected from at least one of dibutyl phthalate, dioctyl phthalate, styrene, diallyl phthalate, ethyl acetate, toluene, xylene, propenyl glycidyl ether, butyl glycidyl ether or phenyl glycidyl ether.
The invention also provides a preparation method of the heat dissipation material, which comprises the following steps:
(1) Adding graphite and carbon nanotubes into a diluent, stirring, and vacuumizing to obtain a carbon material mixed solution;
(2) Grinding and concentrating the carbon material mixed solution to obtain concentrated slurry;
(3) Mixing resin, a curing agent and the concentrated slurry to obtain a premixed solution A;
(4) And mixing the fiber reinforced filler with the premix A to prepare the heat dissipation material.
According to the invention, air in pores in the carbon material is pumped out by adopting a vacuumizing method, so that the diluent can fully infiltrate graphite and carbon nanotubes, and meanwhile, the stirring and grinding process adopted by the invention is beneficial to stripping of graphite, and the preparation efficiency of nano-scale graphene is improved. According to the invention, the nano-carbon material is prepared in the resin diluent, and then the nano-carbon material slurry with high concentration (accounting for 50-75%) is prepared by concentration, so that the heat conduction advantages of the graphene with a lamellar structure and the carbon nano-tube with a large length-diameter ratio are fully utilized, the heat of a heating source can be rapidly led out, and the heat can be efficiently diffused to other media in a radiation mode, thereby achieving a heat dissipation effect incomparable with other heat conduction materials; meanwhile, the graphene and the carbon nano tube can be more fully fused with resin by combined use, and the dispersion effect of the graphene/carbon nano tube composite material is incomparable to that of the graphene powder or the carbon nano tube and the resin.
Preferably, the rotation speed of the stirring in the step (1) is 800-2500r/min, and the stirring time is 10-20min.
Preferably, the vacuum degree after the vacuum pumping in the step (1) is-10 KPa to-50 KPa.
Preferably, the step (2) is carried out by a sand mill, the grinding speed is 40-85r/min, the grinding linear speed is 8-15m/s, and the grinding time is 2.5-3h.
Preferably, the rotation speed of the mixing in the step (3) is 800-2500r/min, and the mixing time is 15-55min.
Preferably, a screw mixer is adopted for mixing in the step (4), the mixing speed is 10-60r/min, and the mixing time is 20-100min.
The invention also discloses application of the heat dissipation material in industrial heat dissipation, illumination heat dissipation and electronic device heat dissipation.
Compared with the prior art, the invention has the following beneficial effects:
(1) The heat dissipation material has the characteristics of high heat conduction coefficient and high heat radiation coefficient, can enable the temperature of a heat source to reach a constant temperature state for a long time, and protects the performance stability of the heat source;
(2) According to the invention, air in pores in the carbon material is pumped out by adopting a vacuumizing method, so that the diluent can fully infiltrate graphite and carbon nano tubes, and the product performance is improved;
(3) Aiming at the defects that the conventional graphene powder has a stacking effect and cannot be fully dispersed in a resin system in the using process, so that the performance of the product is reduced, the graphene oxide/expanded graphite composite material takes graphite oxide or expanded graphite as a starting raw material, and the graphene is stripped in the preparation process and dispersed in a heat dissipation material by adopting stirring and grinding processes, so that the defects of the conventional process are avoided;
(4) According to the invention, the graphene and the carbon nano tube are combined for use, so that the graphene and the carbon nano tube can be more fully fused with resin, and the dispersion effect of the graphene and carbon nano tube is incomparable with that of the graphene powder or the carbon nano tube fused with resin.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are only preferred embodiments of the present invention, and the claimed protection scope is not limited thereto, and any modification, substitution, combination made without departing from the spirit and principle of the present invention are included in the protection scope of the present invention.
The starting materials, reagents or apparatuses used in the following examples are, unless otherwise specified, either commercially available from conventional sources or can be obtained by known methods.
Example 1
The embodiment provides a heat dissipation material which is prepared from the following components in parts by weight: 10 parts of graphite oxide, 2 parts of carbon nano tubes, 52 parts of epoxy resin, 35 parts of glass fibers, 2 parts of ethylenediamine and 228 parts of styrene.
The preparation method of the heat dissipation material comprises the following steps:
(1) Adding graphite oxide and carbon nanotubes into styrene, stirring sufficiently by using a high-speed stirrer (the rotating speed is 2000r/min, the stirring time is 15 min), then pumping the vacuum degree of the mixed liquid to-35 KPa by using a vacuum tank, pumping out air in pores in the carbon material, and infiltrating the carbon material sufficiently with the styrene to obtain a carbon material mixed liquid;
(2) Circularly grinding the carbon material mixed solution prepared in the step (1) for 240min at a high speed by a sand mill, wherein the grinding medium is 1mm of zirconium oxide particles, the grinding speed is 65r/min, and the grinding linear speed is 12m/s; concentrating the obtained dispersion liquid by an ultrahigh-speed centrifugal concentration device, and increasing the concentration of the nano carbon material in the styrene to obtain concentrated slurry with the carbon material content of 55%;
(3) Pouring the resin, the curing agent and the concentrated slurry prepared in the step (2) into a mixing tank, and stirring at a high speed of 2000r/min for 30min in a high-speed stirrer to obtain a premixed solution A;
(4) And (3) fully mixing the premixed solution A and glass fiber (with the length of 12 mm) for 20min by using a spiral mixer (with the rotating speed of 30 r/min), taking out, and packaging in blocks to obtain the heat dissipation material.
Example 2
The embodiment provides a heat dissipation material which is prepared from the following components in parts by weight: 15 parts of graphite oxide, 3 parts of carbon nano tubes, 48 parts of epoxy resin, 33 parts of glass fiber, 2 parts of ethylenediamine and 360 parts of styrene.
The preparation method of the heat dissipation material comprises the following steps:
(1) Adding graphite oxide and carbon nanotubes into styrene, stirring sufficiently by using a high-speed stirrer (the rotating speed is 2500r/min, the stirring time is 10 min), then pumping the vacuum degree of the mixed liquid to-45 KPa by using a vacuum tank, pumping out air in pores in the carbon material, and sufficiently infiltrating the carbon material with the styrene to obtain a carbon material mixed liquid;
(2) Circularly grinding the carbon material mixed solution prepared in the step (1) for 300min at a high speed by a sand mill, wherein the grinding medium is 1mm of zirconium oxide particles, the grinding speed is 75r/min, and the grinding linear speed is 10m/s; concentrating the obtained dispersion liquid by an ultrahigh-speed centrifugal concentration device, and increasing the concentration of the nano carbon material in the styrene to obtain concentrated slurry with the carbon material content of 55%;
(3) Pouring the resin, the curing agent and the concentrated slurry prepared in the step (2) into a mixing tank, and stirring at a high speed for 45min in a high-speed stirrer (the rotating speed is 1000 r/min) to fully mix to obtain a premixed solution A;
(4) And (3) fully mixing the premixed solution A and glass fiber (with the length of 12 mm) for 30min by using a spiral mixer (with the rotating speed of 40 r/min), taking out, and packaging in blocks to obtain the heat dissipation material.
Comparative example 1
This comparative example provides a heat dissipating material having a composition completely identical to that of example 2 except that: the heat dissipating material of this comparative example was prepared without a vacuum evacuation step.
Product effectiveness testing
The thermal conductivity and emissivity of the heat dissipating materials prepared in examples 1 and 2 were measured and compared with those of aluminum, and the results are shown in table 1.
TABLE 1 Heat Release Table (example 1, example 2, aluminum)
As can be seen from table 1, in example 2, the weight part of the carbon material was increased from 12 parts to 18 parts, which is 50% higher than that in example 1; and the heat conductivity coefficient is improved from 6.3W/mK to 13.5W/mK, which is increased by more than 1 time. The heat conductivity coefficient of the product can be rapidly improved along with the increase of the carbon material part, which provides a direction for developing high-heat-conductivity plastics, but the heat conductivity coefficient of the product is greatly different from that of metal aluminum.
Compared with the embodiment 1, the embodiment 2 has the advantages that the increase of the weight parts of the carbon material does not obviously enhance the emissivity of the heat dissipation material, and the emissivity of the heat dissipation material prepared in the embodiment 1-2 can reach 6-7 times that of metal aluminum, namely, the heat dissipation material can meet the requirement of heat conductivity, and a heat radiator made of the heat dissipation material can use a smaller heat dissipation surface to dissipate the heat of a heat source into the air, so that the heat radiator replaces a heavy large aluminum heat radiator.
The thermal conductivity and emissivity of the heat dissipating materials prepared in example 2 and comparative example 1 were measured, and the results are shown in table 2.
TABLE 2 Heat Release Table (example 2, comparative example 2)
As can be seen from table 2, compared to comparative example 1, example 2 further includes a vacuum-pumping step, and the thermal conductivity of the prepared product is significantly better than that of comparative example 1, the main reason is that air in the pores in the carbon material can be pumped out after vacuum-pumping, styrene can more fully infiltrate the carbon material, so that graphene can be more easily ground and peeled under the same conditions, and more importantly, after styrene is filled in the pores of the carbon material, the graphene cannot be overlapped and changed into graphite blocks due to high-speed collision and extrusion of zirconia particles in the process of peeling the graphene by a sand mill, so that the peeling effect of the graphene is better, and the high thermal conductivity of the graphene is better exerted.
The heat dissipation material prepared by the invention has the performances of excellent heat conduction efficiency, lighter weight and the like, and can reduce the weight by about 50% compared with a common aluminum product under the same volume.
As is known, the thermal conductivity of an aluminum heat sink is certainly higher than that of a resin heat sink, and the thermal conductivity of the existing resin heat sink at home and abroad does not exceed that of an aluminum heat sink anyway, because the heat sink is improved by a heat conductive filler, and the thermal conductivity of the heat conductive filler is hardly higher than that of a metal material such as aluminum.
However, any heat sink, in addition to being able to quickly conduct heat from a heat generating source to the surface of the heat sink, eventually dissipates heat to the air by convection and radiation. The heat conductivity is high, only the problem of fast heat transfer is solved, and the heat dissipation is mainly determined by the heat dissipation area, the shape, the natural convection and the heat radiation capability, which are almost independent of the heat conductivity of the material. Therefore, the resin heat dissipation material with high radiation capability can be used for preparing a good heat sink as long as the resin heat dissipation material has certain heat conduction capability. Generally, if the distance from the heat source to the surface of the thermally conductive plastic heat sink is less than 5mm, the heat dissipation is dominated by convection as long as the thermal conductivity is greater than 5W/m · K, at which time the conductive heat dissipation has no effect. Therefore, the heat dissipation material prepared by the invention can completely meet the heat dissipation requirement of a heat source, and the heat dissipation effect is even better than that of aluminum materials.
Claims (9)
1. The heat dissipation material is characterized by being prepared from the following components in parts by weight: graphite, carbon nano tubes, resin, fiber reinforced filler, a curing agent and a diluent; the graphite is graphite oxide or expanded graphite;
the preparation method of the heat dissipation material comprises the following steps:
(1) Adding graphite and carbon nanotubes into a diluent, stirring, and vacuumizing to obtain a carbon material mixed solution;
(2) Grinding and concentrating the carbon material mixed solution to obtain concentrated slurry;
(3) Mixing resin, a curing agent and the concentrated slurry to obtain a premixed solution A;
(4) And mixing the fiber reinforced filler with the premix A to prepare the heat dissipation material.
2. The heat dissipating material of claim 1, wherein the heat dissipating material is prepared from the following components in parts by weight: 1-20 parts of graphite, 1-5 parts of carbon nano tubes, 50-90 parts of resin, 20-40 parts of fiber reinforced filler, 2-10 parts of curing agent and 200-450 parts of diluent.
3. The heat dissipating material of claim 1, wherein the fiber-reinforced filler is selected from at least one of glass fibers, carbon fibers, metal fibers, ceramic fibers, or aramid fibers.
4. The heat dissipating material of claim 1, wherein the curing agent is selected from at least one of ethylenediamine, triethylamine, triethanolamine, diethylenetriamine, maleic anhydride, phthalic anhydride, amino resin, urea resin, furfural resin, or polyamide.
5. The heat dissipating material of claim 1, wherein the diluent is selected from at least one of dibutyl phthalate, dioctyl phthalate, styrene, diallyl phthalate, ethyl acetate, toluene, xylene, propenyl glycidyl ether, butyl glycidyl ether, or phenyl glycidyl ether.
6. The heat dissipating material of claim 1, wherein the stirring in step (1) is performed at a rotation speed of 800 to 2500r/min for a period of 10 to 20min.
7. The heat dissipating material of claim 1, wherein the degree of vacuum after the evacuation in step (1) is from-10 to-50 KPa.
8. The heat dissipating material of claim 1, wherein the step (2) is performed by using a sand mill at a rotation speed of 40-85r/min, a linear speed of 8-15m/s, and a grinding time of 2.5-3h.
9. Use of the heat dissipating material of any one of claims 1 to 8 for industrial heat dissipation, lighting heat dissipation, and electronic device heat dissipation.
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