CN111349423A - Phase-change heat-conducting paste with low thermal resistance, low volatilization rate and low precipitation - Google Patents
Phase-change heat-conducting paste with low thermal resistance, low volatilization rate and low precipitation Download PDFInfo
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Abstract
The invention discloses a composition and a preparation method of a phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation. Low precipitation refers to low precipitation of the phase change wax and carrier oil. The phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation consists of carrier oil, hydroxyl-terminated liquid rubber, a blocked isocyanate curing agent, a coupling agent, modified phase-change wax powder, an antioxidant and heat-conducting powder. The preparation process of the phase change heat conducting paste with low thermal resistance, low volatilization rate and low precipitation comprises the following steps: mixing and stirring carrier oil, an antioxidant, a coupling agent, hydroxyl-terminated liquid rubber and heat conducting powder, vacuumizing at high temperature to remove small molecular compounds, cooling to room temperature, adding a closed isocyanate curing agent and modified phase-change wax powder, vacuumizing, mixing uniformly, and grinding by a grinding machine.
Description
Technical Field
The invention relates to an organic phase change interface heat dissipation material for a heating electronic device module, in particular to a phase change heat conduction paste material with low thermal resistance, low volatilization and low precipitation.
Technical Field
Communication, intelligent TV, automotive electronics and new forms of energy power battery, electronic product such as solar cell is along with the lightweight, and intelligent development, electronic component and module volume reduce, and the integrated level is high, and heat dissipation space and passageway reduce, and in addition, operating frequency is high, operating time is long at every turn, and the heat of local accumulation can not in time be derived. The heat-conducting silicone grease is used for reducing the interface thermal resistance between the heating element and the heat dissipation device and improving the heat-conducting efficiency. Polydimethylsiloxane and polymethylphenylsiloxane compounds in silicone grease have low surface tension and are easy to migrate, electronic elements are polluted, the silicon-oxygen compounds generated by oxidative decomposition corrode welding spots to influence electric contact conductivity, and meanwhile, cyclic siloxane compounds generated by decomposition are easy to condense on the surface of an optical component to increase haze, so that pollution is caused. The phase-change wax in the phase-change thermal conductive paste is crystallized at a temperature lower than the melting temperature, the phase-change wax is less in migration at room temperature and in regions other than a heat source (lower than the phase-change temperature), the migration of carrier oil is limited, the pollution is reduced, and meanwhile, the enthalpy of the phase-change thermal conductive paste is high in the phase-change process, and more heat can be absorbed. Patent CN105315968A discloses a silicon-free phase-change thermal paste with high thermal conductivity, low thermal resistance and high heat transfer efficiency, which is prepared by kneading and grinding matrix oil, thermal conductive powder, phase-change wax and coupling agent. The base oil is composed of polymers with different molecular weights, contains a small amount of micromolecule compounds which are easy to volatilize, and the micromolecule compounds with low melting points in the phase-change wax are easy to volatilize after the phase-change heat-conducting paste is melted, and meanwhile, the phase-change wax and the carrier oil are accelerated to be separated out and transferred to other places, so that the contact of an electric contact of an electronic module and the pollution to an optical product are influenced, and the use is influenced. In addition, the phase-change wax with low melting point and high toughness is not easy to knead, grind and disperse, is easy to agglomerate, is not fine enough, is easy to lack materials when being coated thinner, and is not beneficial to coating because wax absorbs partial base oil to form wax slurry to cause large coating viscosity after melting, dispersing and recrystallizing the phase-change heat-conducting paste. Aiming at the defects, the invention aims to increase the compatibility among phase-change wax, carrier oil and liquid rubber, increase the affinity between organic components and heat-conducting powder, reduce the volatilization rate and the precipitation rate (carrier oil compounds and phase-change wax compounds) of the phase-change heat-conducting paste after melting and reduce pollution by a high-temperature vacuum small molecule removal process. In addition, the modified phase-change wax fine powder is prepared in the preparation process, so that the fineness of the phase-change heat-conducting paste is improved, and the coating is facilitated.
Disclosure of Invention
The invention aims to overcome the technical defects of high volatilization rate and high precipitation of carrier oil and phase-change wax after high-temperature melting in the working process of the phase-change heat-conducting paste, and provides the phase-change heat-conducting paste with low thermal resistance, low volatilization and low precipitation. Low precipitation refers to low precipitation migration of the carrier oil and the phase change wax. Hydroxyl-terminated liquid rubber and a blocked isocyanate curing agent which are well compatible with phase-change wax are introduced into the phase-change heat-conducting paste, and the main chain of the liquid rubber is a hydrocarbon chain which is similar to the molecular structures of the phase-change wax and carrier oil and is physically compatible. Before the phase-change heat-conducting paste is coated and screen-printed, the hydroxyl-terminated liquid rubber is in a low-viscosity liquid state, so that the coating and screen-printing operations are convenient, an electronic product generates heat after the operation, the blocked isocyanate curing agent is gradually unblocked to release the isocyanate curing agent with high activity to react with hydroxyl, the hydroxyl-terminated liquid rubber reacts with the blocked isocyanate curing agent to form macromolecular rubber and microgel, the migration is reduced, in addition, the alcohol wax added into the modified phase-change wax can also react with the blocked isocyanate curing agent, and the alcohol wax is long-carbon-chain wax and is better compatible with the phase-change wax. The modified phase-change wax is prepared by blending and modifying phase-change wax, alcohol wax and ethylene-vinyl acetate copolymer EVA, and removing low-melting-point small-molecular wax compounds through a high-temperature melting process, wherein the EVA is compatible with the phase-change wax. In order to reduce the precipitation of the carrier oil and the paraffin, the heat conductive powder contains ultrafine powder with a particle size of D50=0.1-2um (D50 means a particle size of less than 50% of the powder in the cumulative distribution of the powder), the surface area of the powder is large, and the adsorption rate of the organic oil and the paraffin is high. In addition, in order to increase the dispersion of the heat-conducting powder and the compatibility of the organic component, a coupling agent with a non-polar long carbon chain is introduced, one end of the long carbon chain is compatible with the organic component, the other end of the long carbon chain acts with hydroxyl on the surface of the heat-conducting powder, and the coupling agent is anchored on the surface of the heat-conducting powder. In the preparation process of the phase change heat conducting paste with low thermal resistance, low volatilization rate and low precipitation, the micromolecular compounds in the carrier oil and the auxiliary agent are removed by high-temperature vacuum pumping, so that the volatilization rate and the oil wax precipitation rate are reduced. In addition, aiming at the defect that the traditional phase-change heat-conducting paste is not fine enough, the phase-change wax, the alcohol wax and the EVA are melted and blended, cooled and crushed to collect fine powder with the particle size smaller than 20um for use, and the EVA helps to improve the strength and toughness of the phase-change wax, is not easy to deform during crushing and is easy to pulverize.
The composition and preparation method of a phase-change thermal conductive paste with low thermal resistance, low volatility and low precipitation are further described as follows.
A phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation consists of,
carrier oil: 100 parts of (A);
1-10 parts of hydroxyl-terminated liquid rubber;
0.1-1 part of blocked isocyanate curing agent;
0.1-5 parts of coupling agent;
5-15 parts of modified phase-change wax powder;
1-5 parts of an antioxidant;
450 portions of heat conducting powder and 2000 portions of heat conducting powder.
Based on the composition, the carrier oil in the phase change thermal conductive paste with low thermal resistance, low volatility and low precipitation is one or a mixture of more of poly-alpha olefin, polyol ester compound (such as dipentaerythritol ester and the like) and long-chain alkyl benzene base oil, and the viscosity of the carrier oil is less than 1000 cs.
The hydroxyl-terminated liquid rubber comprises one or a mixture of more of hydroxyl-terminated polybutadiene liquid rubber, hydroxyl-terminated butylbenzene liquid rubber and hydroxyl-terminated polyisoprene liquid rubber, wherein the viscosity of the hydroxyl-terminated liquid rubber is less than 20,000 cs. For example, the viscosity of HTPB type hydroxyl-terminated polybutadiene liquid rubber of Zibozilong chemical company Limited is less than 10,000 cs.
The deblocking curing temperature of the blocked isocyanate curing agent is higher than 80 ℃, and dipentaerythritol ester without hydroxyl or with low hydroxyl content is added into a commercial blocked isocyanate curing agent. For example, the DIPE-pentaerythritol ester DIPE-20 was added to a commercially available vestatat B1358/100, PT1202G, and then the low molecular weight solvent originally present therein was removed in vacuo at 60-80 ℃. The blocked curing agent does not react with the alcohol wax containing hydroxyl and the hydroxyl-terminated liquid rubber at room temperature, and the isocyanate curing agent which is unblocked to release activity at the temperature of more than 80 ℃ performs a crosslinking reaction with the hydroxyl of the alcohol wax and the hydroxyl-terminated liquid rubber to form a polyurethane structure, so that a partial crosslinking and microgel structure is formed, and the high-temperature migration of oil and phase-change wax is reduced.
The modified phase-change wax powder in the phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation is prepared by melting and mixing phase-change wax, alcohol wax and ethylene/vinyl acetate copolymer EVA, cooling, high-speed crushing and sieving. The phase-change wax is one or more of paraffin, palm wax and microcrystalline wax, and has a melting point of 5-100 deg.C and an optimum melting point of 35-90 deg.C. Wherein, the ethylene/vinyl acetate copolymer EVA has 10-40% of vinyl acetate content and 50-100 ℃ of melting point. The alcohol wax is one or more of n-tridecanol, n-tetradecanol, n-hexadecanol, n-octadecanol, cetyl alcohol and the like, has a melting point of 30-60 ℃, is compatible with long-chain alkyl and phase-change wax in a molecular structure and EVA, can react with a blocked isocyanate curing agent, enhances the acting force between paraffin and a macromolecular liquid rubber polyurethane compound like a coupling agent, and reduces the precipitation of the molten liquid paraffin. The melting mixing mass ratio of the phase-change wax, the EVA and the alcohol wax is 100:0.1:0.1-100:5: 3; the melting processing temperature is 100-150 ℃, and simultaneously the vacuum pumping is carried out to-0.1 MPa, so as to remove the low-melting-point small molecular wax compound. The modified phase-change wax is melted, mixed evenly and cooled to 0-30 ℃. The particle size of the modified phase-change wax powder after being crushed and screened by a screen with 800 meshes is less than 20 um.
A phase-change thermal conductive paste with low thermal resistance, low volatility and low precipitation is prepared from one or more of titanate coupling agent, aluminate coupling agent and zircoaluminate coupling agent, such as titanium isopropoxide tristearate, isopropoxide distearate acyloxy aluminate, neoalkoxy tri (dodecylbenzene acyloxy) zirconate.
The heat conducting powder comprises one or a mixture of a plurality of powders of zinc oxide, aluminum nitride, aluminum oxide, magnesium oxide, boron nitride, graphite, graphene, carbon nano tubes, metal aluminum powder, copper powder, silver-coated aluminum powder, silver-coated copper powder, nickel-coated aluminum powder and the like. A phase-change thermal conductive paste with low thermal resistance, low volatility and low precipitation comprises more than 2 kinds of high thermal conductive powder, at least one kind of high thermal conductive powder has a particle size D50=0.1-2um, and the other kind has an average particle size D50= 8-20 um.
A phase-change thermal conductive paste with low thermal resistance, low volatility and low precipitation is prepared from hindered phenol and phosphite ester as antioxidant (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) N-octadecyl propionate, phosphite ester, N, N-bis (2, 4-diaminodiphenyl ether) imine and N, N-bis (2, 4-diiminodiphenyl ether) imine).
The detailed preparation process of the phase change heat conducting paste with low thermal resistance, low volatility and low precipitation is as follows,
(1) heating phase-change wax, EVA and alcohol wax in a stirring reaction kettle according to a certain mass ratio to 100-150 ℃, keeping the temperature for 0.5-1 h, stirring the phase-change wax, the EVA and the alcohol wax to a uniform and transparent solution, vacuumizing to-0.1 MPa to remove low-melting-point small-molecular wax compounds, then casting into a certain mould suitable for crushing and processing wax blocks, and cooling to 0-30 ℃. Putting the wax blocks into a high-speed pulverizer for pulverization, connecting a material pulverizing groove of the pulverizer with chilled water, and collecting the modified phase-change wax powder with the particle size of less than 20um through a screen with the mesh number of more than 800 meshes.
(2) Putting base oil, a coupling agent, an antioxidant and hydroxyl-terminated liquid rubber into a double-planet stirrer, uniformly mixing, adding heat conducting powder in batches according to a proportion, mixing and stirring, heating to 130 ℃, vacuumizing to-0.1 MPa to remove small molecular compounds, and cooling to room temperature to obtain heat conducting paste slurry.
(3) Adding the modified phase-change wax powder and the closed isocyanate curing agent in the step (1) into the heat-conducting paste slurry in the step (2), vacuumizing, stirring and mixing uniformly in a double-planet mixer, and then grinding by a three-roll grinder to obtain the fine phase-change heat-conducting paste with low thermal resistance, low volatilization rate and low precipitation.
Detailed Description
The present invention is described in further detail below with reference to examples.
In the case of example 1, the following examples,
100 parts of phase-change wax (melting point 52 ℃), 1 part of EVA (melting point 47 ℃, vinyl acetate content 40%) and 2 parts of n-hexadecanol are heated to 120 ℃ in a stirring reaction kettle, stirred at constant temperature for 40 minutes, the phase-change wax, the EVA and the alcohol wax are stirred into uniform and transparent solution, the solution is vacuumized to-0.1 MPa, the low-melting-point small-molecule wax compound is removed, then the solution is cast into a certain mould suitable for crushing and processing wax blocks, and the mould is cooled to 0-30 ℃. And putting the wax block into a high-speed grinder for grinding, connecting a material grinding groove of the grinder with chilled water, and collecting the modified phase-change wax powder smaller than 20um through a 800-mesh screen after grinding.
100 parts of alpha-olefin with the kinematic viscosity of 400-500cs, 1 part of coupling agent titanium isopropoxide tristearate, 1 part of antioxidant β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate and 10 parts of hydroxyl-terminated polybutadiene liquid rubber (with the viscosity of 800-1200 cs) are put into a double-planet stirrer to be uniformly mixed, 250 parts of zinc oxide powder with the particle size of D50=0.2um and 300 parts of aluminum oxide powder with the particle size of D50=6um are sequentially added to be mixed and stirred, the mixture is heated to 130 ℃, vacuumized to-0.1 MPa to remove small molecular compounds, then cooled to room temperature to obtain heat-conducting paste slurry, 10 parts of modified phase-change wax powder and 0.5 part of blocked isocyanate curing agent are added into the heat-conducting paste slurry, the mixture is vacuumized, stirred and uniformly mixed in the double-planet mixer, and then ground by a three-roll grinder to obtain the fine phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation.
In the case of example 2, the following examples,
heating 100 parts of phase-change wax (melting point 46 ℃), 2 parts of EVA (melting point 47 ℃, vinyl acetate content 40%) and 1 part of n-octadecanol in a stirring reaction kettle to 120 ℃, stirring at constant temperature for 30 minutes, stirring the phase-change wax, the EVA and the alcohol wax into a uniform and transparent solution, vacuumizing to-0.1 MPa, removing low-melting-point small-molecular-weight wax compounds, casting into a certain mould suitable for crushing and processing wax blocks, and cooling to 0-30 ℃. And putting the wax block into a high-speed grinder for grinding, connecting a material grinding groove of the grinder with chilled water, and collecting the modified phase-change wax powder smaller than 20um through a 800-mesh screen after grinding.
Putting dipentaerythritol ester DIPE-30100 parts, coupling agent isopropoxy distearate acyloxy aluminate ester 1.5 parts, antioxidant phosphite ester 0.5 parts and hydroxyl terminated styrene-butadiene liquid rubber 6 parts into a double-planet stirrer, uniformly mixing, adding 300 parts of alumina powder with the particle size D50=0.2um and 400 parts of alumina powder with the particle size D50=10um in sequence, mixing and stirring, heating to 130 ℃, vacuumizing to-0.1 MPa to remove small molecular compounds, and cooling to room temperature to obtain the heat-conducting paste slurry. Adding 12 parts of modified phase-change wax powder and 0.3 part of closed isocyanate curing agent into the heat-conducting paste slurry, vacuumizing, stirring and mixing uniformly in a double-planetary mixer, and grinding by a three-roll grinder to obtain the fine phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation.
In the case of example 3, the following example was carried out,
heating 100 parts of microcrystalline wax (melting point 78 ℃), 3 parts of EVA (melting point 78 ℃, vinyl acetate content 25%) and 1 part of n-octadecanol in a stirring reaction kettle to 145 ℃, stirring at constant temperature for 60 minutes, stirring the microcrystalline wax, the EVA and the alcohol wax into uniform and transparent solution, vacuumizing to-0.1 MPa, removing low-melting-point small-molecular-weight wax compounds, casting into a certain mould suitable for crushing and processing wax blocks, and cooling to 0-30 ℃. And putting the wax blocks into a high-speed grinder for grinding, connecting a material grinding groove of the grinder with chilled water, and collecting the modified phase-change wax powder with the particle size of less than 20um through a 800-mesh screen after grinding.
100 parts of poly-alpha-olefin with the kinematic viscosity of 400-500cs, 2 parts of coupling agent isopropoxy distearate acyloxy aluminate, 1 part of antioxidant phosphite ester and 12 parts of hydroxyl-terminated polybutadiene liquid rubber are put into a double-planet stirrer to be uniformly mixed, 300 parts of aluminum powder with the particle size of D50=1um and 600 parts of aluminum powder with the particle size of D50=10um are sequentially added to be mixed and stirred, the mixture is heated to 130 ℃, vacuumized to-0.1 MPa to remove small molecular compounds, and then cooled to room temperature to obtain heat-conducting paste slurry. Adding 13 parts of the modified phase-change wax powder and 0.8 part of a closed isocyanate curing agent into the heat-conducting paste slurry, vacuumizing, stirring and mixing uniformly in a double-planetary mixer, and grinding by a three-roll grinder to obtain the fine phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation.
The thermal conductivity and thermal resistance of the phase change thermal paste were tested according to ASTM D5470, and the melting phase transition temperature was tested according to ASTM D3418 using a differential scanning calorimeter. And (4) testing the volatilization rate, namely measuring the percentage of the weight lost by the phase change thermal paste sample after being baked for 2 hours at 150 ℃ to the original weight. And (3) performing a phase change heat conduction paste precipitation test, namely coating phase change heat conduction paste with the diameter of 10mm and the thickness of 1mm on ground glass, placing the ground glass in a cold and hot impact test box for cold and hot impact test, respectively keeping the ground glass at 25 ℃ and 100 ℃ for 30 minutes, then performing temperature exchange within 5 minutes, and testing the maximum diameter of the low molecular oil diffusion in the phase change heat conduction paste after 100 cycles.
Phase change thermal conductive paste was prepared by the following conventional process as a comparison
100 parts of poly-alpha-olefin with kinematic viscosity of 400-500cs, 2 parts of coupling agent isopropoxy distearate acyloxy aluminate, 1 part of antioxidant phosphite ester and 13 parts of phase change wax (phase change melting point of 78 ℃) are put into a kneader and uniformly mixed, 268 parts of aluminum powder with the particle size of D50=1um and 536 parts of aluminum powder with the particle size of D50=10um are added in sequence, vacuum-pumped, mixed and stirred for 1 hour, and then the mixture is ground by a three-roll grinder to obtain the phase change heat conduction material.
The following table shows the performance comparison of the phase-change heat-conducting paste with low thermal resistance, low volatilization and low oil evolution rate and the traditional heat-conducting paste
The data in the table show that the thermal conductivity coefficient is increased and the thermal resistance is reduced along with the increase of the content of the heat conducting powder, and under the same content of the heat conducting powder, the volatilization rate and the oil evolution diameter of the phase-change heat conducting paste in the comparative example of the traditional process are larger than those of the phase-change heat conducting paste in the invention (examples one to three), so that the advancement of low volatilization rate and low precipitation of the phase-change heat conducting paste (examples one to three) is reflected. In addition, the blade coating particle size of the phase change thermal conductive paste in the traditional process is larger, so that the phase change thermal conductive paste is more exquisite.
Claims (9)
1. The phase change thermal conductive paste with low thermal resistance, low volatility and low precipitation is characterized in that: the phase-change heat-conducting paste with low thermal resistance, low volatility and low precipitation consists of carrier oil, hydroxyl-terminated liquid rubber, blocked isocyanate curing agent, coupling agent, modified phase-change wax powder, antioxidant and heat-conducting powder, and comprises the following components,
carrier oil: 100 parts of (A);
1-10 parts of hydroxyl-terminated liquid rubber;
0.1-1 part of blocked isocyanate curing agent;
0.1-5 parts of coupling agent;
5-15 parts of modified phase-change wax powder;
1-5 parts of an antioxidant;
heat conducting powder of 450 portions and 2000 portions;
the modified phase-change wax powder is prepared by melting and blending phase-change wax, alcohol wax and ethylene/vinyl acetate EVA copolymer, vacuumizing to remove low-melting-point micromolecule compounds, cooling, crushing and sieving, wherein the particle size of the obtained phase-change wax powder is less than 20 um; the preparation process of the phase change heat conducting paste with low thermal resistance, low volatilization rate and low precipitation comprises the following steps: mixing and stirring carrier oil, an antioxidant, a coupling agent, hydroxyl-terminated liquid rubber and heat conducting powder, vacuumizing at high temperature to remove small molecular compounds, cooling to room temperature, adding a closed isocyanate curing agent and modified phase-change wax powder, vacuumizing, mixing uniformly, and grinding by a grinding machine.
2. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the carrier oil is one or a mixture of more of poly alpha olefin, polyol ester compound and long-chain alkyl benzene base oil, and the viscosity of the carrier oil is less than 1000 cs.
3. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the carrier oil is one or a mixture of more of hydroxyl-terminated polybutadiene liquid rubber, hydroxyl-terminated butylbenzene liquid rubber and hydroxyl-terminated polyisoprene liquid rubber, and the viscosity of the hydroxyl-terminated liquid rubber is less than 20,000 cs.
4. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the deblocking curing temperature of the blocked isocyanate curing agent is higher than 80 ℃, dipentaerythritol ester without hydroxyl or with low hydroxyl content is added into the commercial blocked isocyanate curing agent, and then the commercial blocked isocyanate curing agent is vacuumized to-0.1 MPa at the temperature of 60-80 ℃ to remove the original low molecular solvent in the commercial blocked isocyanate curing agent.
5. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the modified phase-change wax powder is prepared by melting and mixing phase-change wax, alcohol wax and ethylene/vinyl acetate copolymer EVA, vacuumizing to remove low-melting-point micromolecule compounds, cooling, crushing and sieving; the phase-change wax is one or a mixture of paraffin, palm wax and microcrystalline wax, the melting point range is 5-100 ℃, and the optimal melting point range is 35-90 ℃; wherein, the ethylene/vinyl acetate copolymer EVA has 10-40% of vinyl acetate chain segment content and 50-100 ℃ of melting point; the alcohol wax is one or more of n-tridecanol, n-tetradecanol, n-hexadecanol, n-octadecanol, cetyl alcohol, etc., and has melting point of 30-60 deg.C; the melting mixing mass ratio of the phase-change wax, the EVA and the alcohol wax is 100:0.1:0.1-100:5: 3; the melting processing temperature is 100-150 ℃, and simultaneously the vacuum pumping is carried out to-0.1 MPa, so as to remove the low-melting-point micromolecule compound; the modified phase-change wax is melted, mixed evenly and cooled to 0-30 ℃; the particle size of the modified phase-change wax powder after being crushed and screened by a screen with 800 meshes is less than 20 um.
6. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the coupling agent is one or more of titanate coupling agent, aluminate coupling agent and zirconium aluminate coupling agent, such as titanium isopropoxide tristearate, isopropoxy distearate acyloxy aluminate and neoalkoxy tri (dodecyl benzene acyloxy) zirconate.
7. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the heat conducting powder comprises zinc oxide, aluminum nitride, aluminum oxide, magnesium oxide, boron nitride, graphite, graphene, carbon nano tubes and one or a mixture of a plurality of powders of metal aluminum powder, copper powder, silver-coated aluminum powder, silver-coated copper powder, nickel-coated aluminum powder and the like; a phase-change thermal conductive paste with low thermal resistance, low volatility and low precipitation comprises more than 2 kinds of high thermal conductive powder, wherein at least one kind of high thermal conductive powder has an average particle size D50=0.1-2um, and the other kind of high thermal conductive powder has an average particle size D50= 8-20 um.
8. The phase change thermal paste with low thermal resistance, low volatility and low precipitation according to claim 1, wherein the antioxidant comprises hindered phenol type antioxidants, phosphite type antioxidants such as β - (3, 5-di-tert-butyl-4-hydroxyphenyl) N-octadecyl propionate, phosphite esters, N, N-bis (2, 4-diaminodiphenyl ether) imine and N, N-bis (2, 4-diiminodiphenyl ether) imine.
9. The phase-change thermal paste according to claim 1, which has low thermal resistance, low volatility and low precipitation, is characterized in that: the preparation process is as follows,
(1) heating phase-change wax, EVA and alcohol wax in a stirring reaction kettle according to a certain mass ratio to 100-150 ℃, keeping the temperature for 0.5-1 h, stirring the phase-change wax, the EVA and the alcohol wax to a uniform and transparent solution, vacuumizing to-0.1 MPa to remove low-melting-point small-molecular wax compounds, then casting into a certain mould suitable for crushing and processing wax blocks, and cooling to 0-30 ℃; putting the wax block into a high-speed grinder for grinding, connecting a material grinding groove of the grinder with chilled water, passing through a screen with the mesh number higher than 800 meshes, and collecting modified phase-change wax powder with the particle size smaller than 20 um;
(2) putting carrier oil, coupling agent, antioxidant and hydroxyl-terminated liquid rubber into a double-planet stirrer, uniformly mixing, adding heat-conducting powder in batches according to a proportion, mixing and stirring, heating to 130 ℃, vacuumizing to-0.1 MPa to remove small molecular compounds, and cooling to room temperature to obtain heat-conducting paste slurry;
(3) adding the modified phase-change wax powder and the closed isocyanate curing agent in the step (1) into the heat-conducting paste slurry in the step (2), vacuumizing, stirring and mixing uniformly in a double-planet mixer, and then grinding by a three-roll grinder to obtain the fine phase-change heat-conducting paste with low thermal resistance, low volatilization rate and low precipitation.
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