CN111675897A - Phase change heat conduction material and preparation method thereof - Google Patents
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Abstract
The invention relates to a phase change heat conduction material and a preparation method thereof. The phase change high heat conduction material is prepared from a polyethylene glycol composite phase change base material, heat conduction filler carbon-coated nano aluminum and an auxiliary agent; the polyethylene glycol composite phase change base material accounts for 60-70% by mass, the heat-conducting filler carbon-coated nano aluminum accounts for 20-30% by mass, and the auxiliary agent accounts for 1-10% by mass; the auxiliary agent comprises a heat stabilizer, a heat conduction reinforcing agent and an interface regulator. During preparation, the components are prepared according to the proportion by a hot melting method. The phase change high-heat-conductivity material has the characteristics of good heat conduction performance, strong adhesion with an interface material and aging resistance.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a phase change heat conduction material and a preparation method thereof.
Background
The phase change material mainly consists of a matrix, a heat-conducting filler and the phase change material, and the heat conductivity of the phase change material is mainly determined by the type, the size and the number of the base material, the heat-conducting filler particles and the interface relationship between the base material and the filler particles. When the quantity of the filler particles reaches a certain value, a heat channel can be formed, and the heat conducting property is greatly improved. The traditional phase change thermal interface material mainly comprises phase change materials directly added with high heat conduction particles, the improvement of the heat conduction performance of the traditional phase change thermal interface material mainly depends on the directly added heat conduction particles, and the fillers commonly used for improving the heat conduction performance mainly comprise carbon materials, zinc oxide, aluminum oxide, boron nitride, silicon carbide, magnesium oxide, aluminum hydroxide or mixtures thereof and the like. The heat conduction performance is poor, and meanwhile, when the material is used as a phase change material, the material is aged after being used for a period of time, and the phase change and heat conduction performance are easily lost.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a phase change heat conduction material and a preparation method thereof. The composite material prepared by taking the polyethylene glycol composite material as a phase change material and the carbon-coated nano aluminum as a heat conduction filler in cooperation with the heat stabilizer, the heat conduction reinforcing agent and the interface regulator has the characteristics of excellent heat conduction performance, strong adhesion with an interface material, aging resistance and obvious phase change process within the temperature range of 55-65 ℃.
In order to achieve the purpose, the invention adopts the technical scheme that:
on one hand, the phase change heat conduction material is characterized by being prepared from a polyethylene glycol composite phase change base material, heat conduction filler carbon-coated nano aluminum and an auxiliary agent; the polyethylene glycol composite phase change base material accounts for 60-70% by mass, the carbon-coated nano aluminum accounts for 20-30% by mass, and the auxiliary agent accounts for 1-10% by mass; the auxiliary agent comprises a heat stabilizer, a heat conduction reinforcing agent and an interface regulator.
Further, the heat stabilizer is at least one of di-n-butyltin dilaurate, dibutyltin maleate monoester or dialkyltin dodecanethiolate.
Further, the heat conduction enhancer is rare earth; the rare earth is one or more of yttrium oxide, lanthanum oxide and samarium oxide.
Further, the interface modifier is trimethoxy propyl silane.
Furthermore, the particle size of the carbon-coated nano aluminum is 50-150 nm.
Further, the auxiliary agent comprises the following components in percentage by mass (1-3%): (2-5%): (0.5% -2%).
On the other hand, the preparation method of the phase change high thermal conductive material comprises the following specific steps:
(1) weighing the polyethylene glycol composite phase change base material, the carbon-coated nano aluminum and the heat stabilizer according to the proportion, mixing, placing in a reaction kettle at the temperature of 80-100 ℃, and heating and stirring for 20-30 min;
(2) adding a heat conduction reinforcing agent and an interface regulator into the mixed solution obtained in the step (1), and heating and stirring for 10-20 min;
(3) and (3) placing the mixed solution obtained in the step (2) in a water bath at the temperature of 60-80 ℃ for ultrasonic dispersion for 10-20 min, and cooling to obtain the phase change high thermal conductivity material.
Further, the preparation method of the polyethylene glycol composite phase change base material comprises the following steps: dissolving hexamethylene diisocyanate in a DMF solution, introducing argon, slowly adding a polyethylene glycol DMF solution under the condition of a constant-temperature water bath at 70-80 ℃, stirring for reaction, and carrying out condensation reflux to obtain an NCO-polyethylene glycol prepolymer; under the conditions of introducing argon and constant-temperature water bath at 70-80 ℃, slowly dropwise adding a hydroxypropyl methyl cellulose DMF solution into the NCO-polyethylene glycol prepolymer, stirring for reaction, condensing, refluxing, drying and grinding to obtain a polyethylene glycol composite phase-change base material;
further, the ratio of hexamethylene diisocyanate, polyethylene glycol and hydroxypropylmethyl cellulose to DMF solution was 1 g: (1-3) mL.
Further, the carbon-coated nano aluminum is prepared by a carbon arc method.
The invention adopts polyethylene glycol composite phase change base material, polyethylene glycol is phase change energy storage material, and hydroxypropyl methyl cellulose is framework material. Because the polyethylene glycol is a linear high molecular long chain which is composed of (O-CH2-CH2-O) n and contains hydroxyl at two ends, the polyethylene glycol has simple structure, easy crystallization and larger phase change enthalpy, and is a good solid-liquid phase change material. And the hydroxypropyl methyl cellulose has stable performance in the phase transition temperature range of polyethylene glycol, and can provide active groups for grafting. The polyethylene glycol of the composite phase-change material is connected with the hydroxypropyl methyl cellulose through a chemical reaction, and the polyethylene glycol is bound by the hydroxypropyl methyl cellulose during phase change, so that the composite phase-change material has the characteristics of a solid-solid phase-change material on a macroscopic scale.
Has the advantages that:
(1) according to the invention, the polyethylene glycol composite material is used as a phase change material, the carbon-coated nano aluminum is used as a heat conduction filler, and the heat conduction reinforcing agent is cooperated, so that the prepared composite material has excellent heat conduction performance, the heat conductivity reaches 6.5W/(m.K), the thermal resistance is as low as 0.021 ℃ in2/W, and an obvious phase change process is shown in the temperature range of 55-65 ℃.
(2) The phase change heat conduction material prepared by the invention is convenient to operate when in use, and the cohesion of the phase change material and the bonding performance with other interfaces can be improved by optimally adding the interface regulator with proper mass fraction into the formula; by adding the heat stabilizer, the anti-aging effect of the phase change heat conduction material is improved, so that the performance of the phase change material is kept more durable.
(3) The phase-change material prepared by the invention has no agglomeration phenomenon and good uniformity, which shows that polyethylene glycol is uniformly dispersed in a three-dimensional network structure of carbon-coated nano aluminum, the carbon-coated nano aluminum plays a role of a matrix, and the dispersion form provides good mechanical strength for the whole compound. Meanwhile, the coating effect on the polyethylene glycol composite material can ensure that the molten polyethylene glycol cannot leak in the phase change process, so that the composite material can keep a solid shape.
Detailed Description
The present invention is further described in the following examples, which should not be construed as limiting the scope of the invention, but rather as providing the following examples which are set forth to illustrate and not limit the scope of the invention.
Example 1
Preparation of polyethylene glycol phase change substrates
Weighing and adding 200080 g of dried polyethylene glycol into 80mL of DMF solution, and stirring for dissolving; under the condition of introducing argon, weighing 30g of hexamethylene diisocyanate, adding into a reaction kettle, adding 60mL of DMF, and stirring for dissolving; slowly dripping a polyethylene glycol 2000DMF solution into the reaction kettle filled with the hexamethylene diisocyanate solution under the conditions of 75 ℃ constant-temperature water bath and argon, controlling the dripping speed to be 15mL/h, stirring for reaction, condensing and refluxing for 6h to obtain an NCO-polyethylene glycol prepolymer, adding 10g of hydroxypropyl methyl cellulose into 50mL of DMF, stirring and dissolving, slowly adding into the NCO-PEG prepolymer under the conditions of argon and 75 ℃ constant-temperature water bath, controlling the dripping speed to be 25mL/h, stirring for reaction, condensing and refluxing for 24h to obtain a cross-linked polymer; pouring the cross-linked polymer solution into a beaker, placing the beaker in a blast drying oven at 75 ℃, and drying the beaker to constant weight; finally grinding the sample to obtain the required polyethylene glycol phase change material;
example 2
Preparation of carbon-coated aluminum
Preparing carbon-coated nano aluminum by adopting a carbon arc method, wherein the raw materials comprise graphite powder (with the purity of 99 percent and the average particle size of about 50 microns) and aluminum powder (with the purity of 99 percent and the average particle size of about 100 microns), and a reaction electrode of the direct-current carbon arc method is prepared from the graphite powder and the aluminum powder; firstly weighing 8g of graphite powder and 15g of aluminum powder, adding 200mL of absolute ethyl alcohol, mixing the graphite powder and the aluminum powder, ultrasonically stirring for 1h, then removing the ethyl alcohol through suction filtration to obtain a solid mixture, drying the solid mixture in a forced air drying oven at the temperature of 80 ℃ for two days, and finally putting the obtained powder into a metallographic embedding machine, and heating and pressing for 24h to obtain a cylindrical sample with the diameter of 24mm and the height of 50 mm; the sample is used as an anode of a reaction electrode, a pure graphite electrode is used as a cathode, a reaction chamber is vacuumized and is filled with argon until the air pressure reaches 1Pa, the working current of a carbon arc discharge device is 120A, the working voltage is 25V, and the distance between the reaction electrode and the graphite electrode is about 3-5 mm; carbon-coated nano aluminum particles generated in the arc discharge process are deposited on the inner wall of the reaction cavity, and the carbon-coated nano aluminum particles deposited on the inner wall are collected after the discharge is finished, standing and cooling are carried out for 24 hours;
example 3
Preparation method of phase change heat conduction material
Weighing 65g of polyethylene glycol phase-change material, 25g of carbon-coated nano aluminum particles and 2g of thermal stabilizer di-n-butyltin dilaurate, mixing, placing in a 90 ℃ reaction kettle, melting the polyethylene glycol phase-change material, heating and stirring for 25min, adding 3g of thermal conductivity enhancer yttrium oxide and 1g of interface regulator trimethoxy propyl silane, heating and stirring for 25min, placing the obtained solution in a 70 ℃ water bath for ultrasonic dispersion for 10min, and finally cooling the obtained solution at room temperature to obtain the phase-change high thermal conductivity material.
Example 4
Preparation method of phase change heat conduction material
Weighing 60g of polyethylene glycol phase-change material, 30g of carbon-coated nano aluminum particles and 3g of thermal stabilizer di-n-butyltin dilaurate, mixing, placing in a reaction kettle at 80 ℃, melting the polyethylene glycol phase-change material, heating and stirring for 25min, adding 2g of thermal conductivity enhancer yttrium oxide and 2g of interface regulator trimethoxy propyl silane, heating and stirring for 25min, placing the obtained solution in a water bath at 80 ℃ for ultrasonic dispersion for 20min, and finally cooling the obtained solution at room temperature to obtain the phase-change high thermal conductivity material.
Example 5
Preparation method of phase change heat conduction material
Weighing 70g of polyethylene glycol phase-change material, 20g of carbon-coated nano aluminum particles and 1g of thermal stabilizer di-n-butyltin dilaurate, mixing, placing in a reaction kettle at 90 ℃, melting the polyethylene glycol phase-change material, heating and stirring for 25min, then adding 5g of thermal conductivity enhancer yttrium oxide and 0.5g of interface regulator trimethoxypropylsilane, heating and stirring for 25min, then placing the obtained solution in a 70 ℃ water bath for ultrasonic dispersion for 15min, and finally cooling the obtained solution at room temperature to obtain the phase-change high thermal conductivity material.
Comparative example 1
Compared with the example 3, the components do not contain a heat stabilizer, and the rest is the same;
comparative example 2
Compared with the example 3, the composition does not contain a heat conduction reinforcing agent, and the balance is the same;
comparative example 3
Compared with the example 3, the components do not contain an interface regulator, and the rest is the same;
comparative example 4
Compared with the example 3, the polyethylene glycol base material is adopted to replace the polyethylene glycol composite base material, and the rest is the same.
And (3) performance testing:
the phase change high thermal conductivity materials prepared in examples 3 to 5 and comparative examples 1 to 4 were used to determine thermal conductivity, thermal resistance, phase change temperature and peel strength. The specific data are as follows:
table 1 results of performance testing
The results in Table 1 show that the phase change materials prepared in the embodiments 3-5 of the present invention have a thermal conductivity of 6.5-6.7W/(m.K), a thermal impedance of 0.021-0.025 ℃ in2/W, a phase change temperature of 60-62 ℃, and a peel strength of 8.5-8.9N, which indicates that the phase change materials prepared in the embodiments of the present invention have excellent performance. The phase-change materials of comparative examples 1 to 4 have different properties, and compared with example 3, comparative example 2 has a larger influence on the thermal conductivity without the thermal conductivity enhancer, comparative example 3 has a larger influence on the adhesive property without the interfacial modifier, and comparative example 4 has the worst phase-change temperature and adhesive property by replacing the polyethylene glycol composite base material with the polyethylene glycol base material.
Claims (9)
1. The phase change heat conduction material is characterized by being prepared from a polyethylene glycol composite phase change base material, heat conduction filler carbon-coated nano aluminum and an auxiliary agent; the polyethylene glycol composite phase change base material accounts for 60-70% by mass, the carbon-coated nano aluminum accounts for 20-30% by mass, and the auxiliary agent accounts for 1-10% by mass; the auxiliary agent comprises a heat stabilizer, a heat conduction reinforcing agent and an interface regulator.
2. The phase change heat conductive material according to claim 1, wherein the heat stabilizer is at least one of di-n-butyltin dilaurate, dibutyltin maleate monoester, or dialkyltin dodecanethiolate.
3. A phase change heat conductive material as claimed in claim 1, wherein the heat conductivity enhancer is a rare earth; the rare earth is one or more of yttrium oxide, lanthanum oxide and samarium oxide.
4. The phase change heat conductive material according to claim 1, wherein the interface modifier is trimethoxypropylsilane.
5. The phase change thermal conductive material as claimed in claim 1, wherein the carbon-coated nano aluminum has a particle size of 50 to 150 nm.
6. The phase change thermal conductive material according to claim 1, wherein the auxiliary agent comprises (1-3%) by mass: (2-5%): (0.5% -2%).
7. The preparation method of the phase change high thermal conductive material according to claim 1, which comprises the following steps:
(1) weighing the polyethylene glycol composite phase change base material, the carbon-coated nano aluminum and the heat stabilizer according to the proportion, mixing, placing in a reaction kettle at the temperature of 80-100 ℃, and heating and stirring for 20-30 min;
(2) adding a heat conduction reinforcing agent and an interface regulator into the mixed solution obtained in the step (1), and heating and stirring for 10-20 min;
(3) and (3) placing the mixed solution obtained in the step (2) in a water bath at the temperature of 60-80 ℃ for ultrasonic dispersion for 10-20 min, and cooling to obtain the phase change high thermal conductivity material.
8. The phase change heat conduction material according to claim 1, wherein the preparation method of the polyethylene glycol composite phase change base material comprises the following steps: dissolving hexamethylene diisocyanate in a DMF solution, introducing argon, slowly adding a polyethylene glycol DMF solution under the condition of a constant-temperature water bath at 70-80 ℃, stirring for reaction, and carrying out condensation reflux to obtain an NCO-polyethylene glycol prepolymer; under the conditions of introducing argon and constant-temperature water bath at 70-80 ℃, slowly dropwise adding a hydroxypropyl methyl cellulose DMF solution into the NCO-polyethylene glycol prepolymer, stirring for reaction, condensing, refluxing, drying and grinding to obtain a polyethylene glycol composite phase-change base material; the ratio of hexamethylene diisocyanate, polyethylene glycol and hydroxypropyl methyl cellulose to DMF solution is 1 g: (1-3) mL.
9. The phase change heat conduction material as claimed in claim 1, wherein the carbon-coated nano aluminum is prepared by carbon arc method.
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| CN114316497A (en) * | 2021-12-28 | 2022-04-12 | 青岛理工大学 | Phase change trigger type thermal interface material with low contact thermal resistance and preparation method thereof |
| CN117720881A (en) * | 2023-09-16 | 2024-03-19 | 广东长特思智能电器科技有限公司 | Insulating high-thermal-conductivity aqueous phase-change gel and preparation method thereof |
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