CN111393856B - Graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste and preparation method thereof - Google Patents
Graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The invention discloses a graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste and a preparation method thereof, wherein the paste is prepared by vacuum heating, defoaming and grinding the following materials, and the material formula mainly comprises the following components: silicon substrate, graphene, spherical alumina, flaky boron nitride, graphite whisker, surfactant, viscosity regulator, dispersant, defoamer and antioxidant. The invention has the advantages that the heat-conducting fillers with different particle sizes and different shapes added in the formula can realize effective stacking among the heat-conducting particles after surface modification treatment, thereby solving the problems of high impedance and low heat-conducting property of the traditional heat-conducting paste and preparing the heat-conducting paste with high heat-conducting property and low heat resistance.
Description
Technical Field
The invention relates to a thermal interface heat conduction material, in particular to a high-heat-conduction low-heat-resistance heat conduction paste and a preparation method thereof.
Background
In recent years, electronic technology is rapidly developed, the size, power and integration of an integrated circuit are miniaturized, the assembly density of electronic components is continuously increased, the heat productivity of the electronic components in unit area is greatly increased, various heat dissipation modes are adopted for dissipating heat generated by the electronic components during operation as soon as possible, such as heat pipe heat dissipation, water cooling auxiliary heat dissipation and the like, however, because the contact interface between a heat dissipation device and the electronic components cannot reach an ideal flat surface, air can exist in a surface gap between the heat dissipation device and the electronic components, the interface heat resistance is increased, the heat transfer is seriously hindered, and the overall heat dissipation effect is influenced. Therefore, the heat conducting paste is required to be added between the electronic component and the heat dissipation device to ensure the sufficient contact of the interface, the heat generated by the electronic component is rapidly transferred to the heat dissipation device by utilizing the flowability and the high heat conducting performance of the heat conducting paste, and then the heat is dissipated by the heat dissipation device to ensure the stable operation of the electronic component.
The conventional heat conducting paste is generally a paste composed of a silicon substrate and heat conducting fillers such as metal oxides, graphite, ceramic materials and the like. The heat conduction network formed by the heat conduction fillers in a mutually staggered mode can endow the heat conduction paste with relatively high heat conductivity, the heat conduction coefficient can be remarkably improved by the high-content heat conduction fillers, however, the viscosity of the heat conduction paste is increased due to the excessive heat conduction fillers, the wettability of the heat conduction paste and the shape matching property of an interface are reduced, and finally the contact thermal impedance of the heat conduction paste in use is increased. Since the graphene is discovered in 2004, the graphene serving as a novel two-dimensional carbon nanomaterial has excellent thermal conductivity and electrical conductivity, is a known substance with the highest mechanical strength, has the advantages of stable chemical properties, good light transmittance and the like, has a profound research prospect as a novel heat conduction auxiliary agent, and is attracted by research institutions in the industry.
Disclosure of Invention
The invention mainly solves the technical problems of low heat conductivity coefficient and thermal impedance of the conventional heat conducting paste, and provides the heat conducting paste with high heat conductivity and low thermal impedance and the preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste is prepared from the following raw materials in parts by weight: 45-55 parts of silicon substrate, 10-15 parts of graphene, 3-6 parts of spherical alumina, 2-5 parts of flaky boron nitride, 6-9 parts of graphite whisker, 0.1-1 part of surfactant, 0.2-2 parts of viscosity regulator, 0.5-3 parts of dispersant, 0.1-1 part of defoaming agent and 0.5-1 part of antioxidant.
In the invention, the silicon matrix is polydimethylsiloxane, the room temperature viscosity of the silicon matrix is 12000mPa & s-18000 mPa & s, and the silicon matrix is specifically one or more of amino silicone oil, phenyl silicone oil or dimethyl silicone oil; the transverse size of a sheet layer of the graphene is 120-180 mu m, and the thickness of the sheet layer is 2.2-2.8 nm; the particle size of the spherical alumina is 40-70 mu m, and the nodularity is 95-98%; the diameter of the flaky boron nitride is 6-12 mu m, and the thickness of the flaky boron nitride is 50-150 nm; the diameter of the graphite whisker is between 0.2 and 5 mu m, and the length of the graphite whisker is between 50 mu m and 100 mu m.
In the invention, the surfactant is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent; the viscosity regulator is one or more of oxidized polyethylene wax, sodium carboxymethyl cellulose or unsaturated polycarboxylate; the dispersing agent is one or more of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone or sodium deoxycholate; the defoaming agent is one or more of a mineral oil defoaming agent, an organic silicon defoaming agent or a polymer defoaming agent; the antioxidant is one or more of 1098 type, 168 type or 1010 type.
The invention discloses a preparation method of a graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste, which comprises the following steps: mixing graphene, spherical alumina, flaky boron nitride and graphite whiskers, and then treating the mixture by using a surfactant to obtain a surface-modified heat-conducting filler; and then uniformly mixing the surface modified heat-conducting filler, the silicon matrix, the viscosity regulator, the dispersant, the defoaming agent and the antioxidant, and performing vacuum defoaming to obtain the graphene-based high-heat-conductivity low-heat-resistance heat-conducting paste.
In the invention, mixing is carried out in a three-dimensional mixing system, the preferred rotating speed is 80-150 rpm/min, and the time is 30-90 min; the surfactant treatment is carried out in ethanol, the temperature of the surfactant treatment is 75-90 ℃, and the time is 4-6 h; the vacuum degree of vacuum defoaming is 0.05-0.2 MPa, the temperature is room temperature, and the time duration is 30-90 min.
Further, after vacuum defoaming, three-roll grinding treatment is carried out, and the grinding speed is preferably 150-250 rpm/min.
The preparation method of the graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste disclosed by the invention can be carried out as follows:
1) firstly, putting a certain amount of graphene, spherical alumina, flaky boron nitride and graphite whiskers together in a three-dimensional mixing system for mixing, wherein the rotating speed is 80-150 rpm/min, and the time duration is 30-90 min;
2) placing the mixed compound powder obtained in the step 1) into a reaction container provided with a condensing device, adding a certain amount of ethanol solution and surfactant, stirring and heating at 75-90 ℃, reacting for 4-6 h, cleaning with absolute ethyl alcohol, and drying in an oven at 120-150 ℃ for 2-5 h to obtain a surface-modified compound heat-conducting filler;
3) mixing and stirring the surface-modified compound heat-conducting filler obtained in the step 2), a silicon substrate, a viscosity regulator, a dispersant, a defoaming agent and an antioxidant uniformly, and then removing bubbles in vacuum at room temperature, wherein the vacuum degree is 0.05-0.2 MPa, and the duration is 30-90 min;
4) and finally, uniformly grinding the mixture obtained in the step 3) by three rollers at a grinding speed of 150-250 rpm/min to obtain the uniformly mixed heat conducting paste.
According to the invention, the weight ratio of silicon matrix, graphene, spherical alumina, flaky boron nitride, graphite whisker, surfactant, viscosity regulator, dispersant, defoaming agent, antioxidant and silicone oil is 45-55: 10-15: 3-6: 2-5: 6-9: 0.1-1: 0.2-2: 0.5-3: 0.1-1: 0.5-1. The invention limits the heat-conducting filler, can form a conductive network, can not generate aggregation, solves the key problems of the existing conductive filler, has more interface polarization among the fillers, has small steric effect, improves the density of the network, and is beneficial to exerting effective heat conduction and reducing thermal resistance; furthermore, the invention limits the size of the filler, easily forms a heat conduction network in the matrix, reduces the thermal resistance, forms more heat conduction paths, and has large heat conductivity coefficient and small thermal resistance of the heat conduction paste product.
Compared with the prior art, the invention has the innovation points that:
(1) and a three-dimensional mixing system is used for mechanically mixing in the circumferential direction, the radial direction and the axial direction, so that different heat-conducting fillers flow, diffuse, accumulate and dope mutually, and the aim of uniformly mixing is fulfilled.
(2) After the compound heat-conducting filler is treated by the surfactant, a chemical bridging is established between the heat-conducting filler and the resin matrix, so that the dispersion uniformity of the heat-conducting filler in the resin can be improved, the interface bonding force between the heat-conducting filler and the resin is enhanced, a heat-conducting network chain is formed, the heat transfer speed is increased, and the heat-conducting performance is further greatly improved.
(3) The heat-conducting filler is compounded in different particle sizes and different shapes, so that effective stacking among heat-conducting particles is realized, more three-dimensional heat-conducting network chains can be established, and rapid heat transfer is realized.
Detailed Description
In the embodiment of the invention, the raw materials are all commercial products, for example, the silicon substrate is polydimethylsiloxane (amino silicone oil), liquid is produced in the chemical industry of New Ann, and the room temperature viscosity is 15000mPa & s; the transverse size of a sheet layer of the graphene is 120-150 mu m, the thickness of the sheet layer is 2.2-2.5 nm, the graphene is commercially-available reduced graphene oxide, and oxygen-containing groups on the surface of the graphene are few; the particle size of the spherical alumina is 50-55 mu m, and the nodularity is 97%; the diameter of the flaky boron nitride is 8-10 mu m, and the thickness of the flaky boron nitride is 95-100 nm; the diameter of the graphite whisker is between 1.5 and 2 mu m, and the length of the graphite whisker is between 85 mu m and 90 mu m; the filler is directly used after being purchased from markets. The surfactant is a silane coupling agent KH 550; the viscosity regulator is sodium carboxymethyl cellulose (AbMole); the dispersant is sodium dodecyl benzene sulfonate; the defoaming agent is organic silicon defoaming agent (Hill); the antioxidant is 1098 type antioxidant (Ciba).
The thermal impedance test is in accordance with the standard of ASTM D5470-06, and the thermal conductivity is in accordance with the standard of ISO 22007-2; as in the test method disclosed in CN 110041703A.
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention and to clearly and unequivocally define the scope of the present invention.
Example 1
The weight ratio of the silicon matrix to the graphene to the spherical alumina to the flaky boron nitride to the graphite whisker to the surfactant to the viscosity regulator to the dispersant to the defoaming agent to the antioxidant is 50: 10: 3: 2: 6: 0.105: 0.5: 0.8: 0.7.
According to the parts by weight, 10 parts of graphene, 3 parts of spherical alumina, 2 parts of flaky boron nitride and 6 parts of graphite whisker are placed in a three-dimensional mixing system together to be fedMixing materials at the rotation speed of 80rpm/min for 30min, placing the mixed compound heat-conducting powder in a reaction container provided with a condensing device, adding 50 parts of ethanol and 0.105 part of surfactant, stirring and heating at 80 ℃, reacting for 5h, then cleaning with absolute ethyl alcohol, drying in an oven at 130 ℃ for 3h to obtain the compound heat-conducting filler with modified surface, and then mixing the surface-modified compound heat-conducting filler with 50 parts of silicon substrate, 0.5 part of viscosity regulator, 0.8 part of dispersant, 0.8 part of defoaming agent and 0.7 part of antioxidant, stirring uniformly, removing bubbles at room temperature in vacuum at a vacuum degree of 0.05MPa for 30min, and finally grinding the mixture by three rollers for 20 min at a grinding speed of 200rpm/min to obtain the uniformly-mixed high-heat-conductivity low-heat-resistance heat-conducting paste with a heat conductivity coefficient of 5.5W/(m ∙ K) and a thermal impedance of 7.1 (K.mm).2）/W。
Comparative example
On the basis of example 1, spherical alumina is replaced by flaky alumina (with the diameter of 10-30 μm, Pengda new material), and the rest is unchanged, so that the obtained thermal conductive paste has the thermal conductivity of 4.3W/(m ∙ K) and the thermal impedance of 10.5 (K.mm)2）/W。
On the basis of the example 1, the thermal conductive filler graphene, spherical alumina, flaky boron nitride and graphite whisker are not added, and the rest is unchanged, so that the obtained thermal conductive silicone grease has a thermal conductivity of 0.18W/(m ∙ K).
The thermal conductive paste obtained by replacing the graphite whiskers with the flaky boron nitride (i.e., without adding the graphite whiskers) on the basis of example 1, and keeping the remainder constant, had a thermal conductivity of 5.1W/(m ∙ K) and a thermal impedance of 9.7 (K. mm)2）/W。
In example 1, spherical alumina, flaky boron nitride, and graphite whisker were all replaced with graphene (that is, only graphene was used as a heat conductive filler), and the rest was unchanged, so that the obtained heat conductive paste had a thermal conductivity of 6.9W/(m ∙ K) and a thermal impedance of 16.8 (K · mm)2）/W。
Example 2
Placing 12 parts of graphene, 5 parts of spherical alumina, 4 parts of flaky boron nitride and 7 parts of graphite whisker together in a three-dimensional mixing system for mixing according to parts by weightThe rotating speed is 120rpm/min, the time is 60min, the mixed compound heat conducting powder is placed in a reaction vessel provided with a condensing device, 50 parts of ethanol solution and 0.14 part of surfactant are added, stirring and heating at 80 ℃, reacting for 5h, then cleaning with ethanol, drying in an oven at 130 ℃ for 3h to obtain the surface-modified compound heat-conducting filler, then mixing and stirring the surface-modified compound heat-conducting filler with 50 parts of silicon substrate, 0.6 part of viscosity regulator, 0.9 part of dispersant, 0.8 part of defoamer and 0.7 part of antioxidant uniformly, removing bubbles at room temperature under vacuum of 0.05MPa for 30min after stirring uniformly, and finally grinding the mixture by three rollers for 20 min at a grinding speed of 200rpm/min to obtain the uniformly-mixed high-heat-conductivity low-heat-resistance heat-conducting paste with a heat conductivity coefficient of 6.2W/(m ∙ K) and a thermal impedance of 5.8 (K.mm).2）/W。
Example 3
Placing 15 parts of graphene, 6 parts of spherical alumina, 5 parts of flaky boron nitride and 9 parts of graphite whisker into a three-dimensional mixing system for mixing according to parts by weight, rotating at 150rpm/min for 90min, placing the mixed compound heat-conducting powder into a reaction container provided with a condensing device, adding 50 parts of ethanol and 0.175 part of surfactant, stirring and heating at 80 ℃, reacting for 5h, cleaning with absolute ethanol, drying in an oven at 130 ℃ for 3h to obtain a surface-modified compound heat-conducting filler, mixing and stirring the surface-modified compound heat-conducting filler with 50 parts of silicon substrate, 0.7 part of viscosity regulator, 1.0 part of dispersant, 0.8 part of defoamer and 0.7 part of antioxidant uniformly, removing bubbles under the vacuum condition at room temperature after stirring uniformly, keeping the vacuum degree at 0.05MPa for 30min, finally performing three-roll grinding on the mixture for 20 min at the grinding speed of 200rpm/min, the obtained uniformly mixed high-thermal-conductivity low-thermal-resistance thermal conductive paste has the thermal conductivity of 6.6W/(m ∙ K) and the thermal impedance of 6.3 (K.mm)2）/W。
The technical effects disclosed by the prior art are as follows:
the technical scheme disclosed by the invention has the advantages that the thermal impedance is obviously reduced while the good heat conductivity coefficient is obtained, and the defects such as bubbles and the like are avoided when the filling material is applied to filling.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (4)
1. A high-thermal-conductivity low-thermal-resistance thermal conductive paste based on graphene is prepared from a silicon substrate, graphene, spherical alumina, flaky boron nitride, graphite whiskers, a surfactant, a viscosity regulator, a dispersant, a defoaming agent and an antioxidant; the weight ratio of the silicon matrix to the graphene to the spherical alumina to the flaky boron nitride to the graphite whisker to the surfactant to the viscosity regulator to the dispersant to the defoaming agent to the antioxidant is 50: 10: 3: 2: 6: 0.105: 0.5: 0.8: 0.7; or the weight ratio of the silicon substrate, the graphene, the spherical alumina, the flaky boron nitride, the graphite whisker, the surfactant, the viscosity regulator, the dispersant, the defoamer and the antioxidant is 50: 12: 5: 4: 7: 0.14: 0.6: 0.9: 0.8: 0.7; or the weight ratio of the silicon substrate, the graphene, the spherical alumina, the flaky boron nitride, the graphite whisker, the surfactant, the viscosity regulator, the dispersant, the defoamer and the antioxidant is 50: 15: 6: 5: 9: 0.175: 0.7: 1.0: 0.8: 0.7; the transverse size of a sheet layer of the graphene is 120-180 mu m, and the thickness of the sheet layer is 2.2-2.8 nm; the particle size of the spherical alumina is 40-70 mu m; the diameter of the flaky boron nitride is 6-12 mu m, and the thickness of the flaky boron nitride is 50-150 nm; the diameter of the graphite whisker is between 0.2 and 5 mu m, and the length of the graphite whisker is between 50 mu m and 100 mu m; the silicon substrate is polydimethylsiloxane; the surfactant is one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent;
the preparation method of the graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste comprises the following steps: mixing graphene, spherical alumina, flaky boron nitride and graphite whiskers, and then treating the mixture by using a surfactant to obtain a surface-modified heat-conducting filler; then uniformly mixing the surface modified heat-conducting filler, the silicon matrix, the viscosity regulator, the dispersant, the defoaming agent and the antioxidant, and then carrying out vacuum defoaming to obtain the graphene-based high-heat-conductivity low-heat-resistance heat-conducting paste; mixing in a three-dimensional mixing system at the rotating speed of 80-150 rpm for 30-90 min; the surfactant treatment is carried out in ethanol, the temperature of the surfactant treatment is 75-90 ℃, and the time is 4-6 h; the vacuum degree of vacuum defoaming is 0.05-0.2 MPa, the temperature is room temperature, and the time duration is 30-90 min; and carrying out three-roll grinding treatment after vacuum defoaming, wherein the grinding speed is between 150 and 250 rpm.
2. The graphene-based high thermal conductivity low thermal resistance thermal paste of claim 1, wherein: the polydimethylsiloxane is amino silicone oil.
3. The graphene-based high thermal conductivity low thermal resistance thermal paste of claim 1, wherein: the viscosity regulator is one or more of oxidized polyethylene wax, sodium carboxymethyl cellulose or unsaturated polycarboxylate; the dispersing agent is one or more of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone or sodium deoxycholate; the defoaming agent is one or more of a mineral oil defoaming agent, an organic silicon defoaming agent or a polymer defoaming agent; the antioxidant is one or more of 1098 type, 168 type or 1010 type.
4. Use of the graphene-based high thermal conductivity low thermal resistance thermal paste of claim 1 as a heat sink material for electronic components.
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| CN103911565B (en) * | 2014-04-23 | 2016-02-24 | 北京科技大学 | A kind of high conductive graphite whisker orientation strengthens the preparation method of metal-base composites |
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