CN108251072B - Preparation method of liquid metal composite phase-change material - Google Patents

Preparation method of liquid metal composite phase-change material Download PDF

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CN108251072B
CN108251072B CN201810179572.9A CN201810179572A CN108251072B CN 108251072 B CN108251072 B CN 108251072B CN 201810179572 A CN201810179572 A CN 201810179572A CN 108251072 B CN108251072 B CN 108251072B
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liquid metal
composite phase
melting point
carbon nanotube
change material
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CN108251072A (en
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王戈
陈晓
高鸿毅
董文钧
邢立文
王军勇
陈思远
郑海燕
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University of Science and Technology Beijing USTB
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

A preparation method of a liquid metal composite phase-change material belongs to the field of shaped composite phase-change materials. The method comprises the steps of uniformly mixing water-soluble metal salt, carbon nano tubes and polyvinylidene fluoride raw materials in different proportions, placing the mixture in a mold with a specific shape for drying, and finally dissolving the metal salt in hot water to obtain the flexible carbon nano tube sponge with the specific shape. And simultaneously placing the prepared carbon nanotube sponge carrier material and liquid metal in a vacuum environment by adopting a melting impregnation method, selecting a proper temperature to melt the liquid metal core material, adsorbing and limiting the liquid metal core material in the pore channel by utilizing the pore channel of the carbon nanotube sponge carrier material in the vacuum environment, and cooling to obtain the liquid metal composite phase-change material. The invention can realize the high-efficiency heat dissipation of the CPU in different temperature ranges; controllable preparation of the pore structure is realized by changing the types and the proportions of the raw materials; the encapsulated shaped composite phase-change material can solve the problem of short circuit of an electronic element circuit caused by free flow of liquid metal, and can also meet the requirement of dynamic heat dissipation of a flexible electronic element.

Description

Preparation method of liquid metal composite phase-change material
Technical Field
The invention belongs to the field of shaped composite phase-change materials, and particularly relates to a preparation method of a liquid metal composite phase-change material.
Background
The electronic heat dissipation is related to the service life and reliability of electronic equipment, and is a bottleneck influencing the development of the current electronic industry. Along with the development of three major trends of high performance, miniaturization and integration of the electronic industry, the heat dissipation problem is more and more prominent. Especially for chips with higher thermal load sensitivity, the heat accumulation at the chip will seriously affect its stability and service life. Research shows that if the working temperature of a single electronic element is increased by 10 ℃, the reliability of the single electronic element is reduced by 50 percent; the failure problem of the CPU is mostly caused by overheating. If a large amount of heat generated by the CPU is not timely dissipated to the external environment, the CPU is halted slightly, and a chip may be burnt out seriously. With the continuous upgrade of the performance of the CPU, the heat dissipation technology of the CPU is increased from air-cooled heat dissipation, heat pipe heat dissipation to water-cooled heat dissipation, heat-conductive silicone grease heat dissipation, and other higher technologies, but still the demand of people for heat dissipation of the chip is not completely satisfied. And the heat conductivity of the liquid metal breaks through the traditional heat conductivity by several times, so that the heat dissipation efficiency is more efficient.
The liquid metal generally refers to an alloy functional material which is in a liquid state at normal temperature, such as a metal with a melting point below 30 ℃ and an alloy material thereof, and also includes a low-melting-point alloy material which is in a liquid state in a working temperature range of 40-300 ℃. The liquid metal has the characteristics of low melting point, high thermal conductivity/electric conductivity, stable property, high temperature resistance, difficult volatilization, no toxicity, environmental protection and the like, and the technical parameters of the melting point, the adhesion, the fluidity, the electric conductivity, the thermal conductivity and the like can be adjusted according to different requirements. Due to the requirements for ultra-small volume, low power consumption, low noise and even high quality experience, the liquid metal is mainly used for heat dissipation of a high-end CPU at present. Although the liquid metal can fully fill the micro-gap of the thermal interface, the heat conduction rate of the heating body and the heat dissipation interface is greatly improved, and the heat dissipation efficiency is higher, the liquid metal is in a liquid state during working, so that the problem of short circuit of an electronic circuit is easily caused, the normal operation of a CPU is directly influenced, and even the CPU can be damaged. Therefore, the Shape-controllable flexible carbon nanotube sponge is synthesized by using the water-soluble metal salt as a template and utilizing the carbon nanotube and the polyvinylidene fluoride (PVDF) to encapsulate the liquid metal to prepare the shaped composite Phase Change Materials (ss-PCMs), and the method fixes the liquid metal in the pore channel of the sponge, so that the problem of line short circuit caused by free flow of the liquid metal can be effectively solved. In addition, the carbon nanotube sponge has good flexibility, can be made into different shapes, and can meet the requirement of dynamic flexible electronic element heat dissipation, thereby having wider heat dissipation application prospect.
Disclosure of Invention
The invention aims to prepare flexible carbon nanotube sponge by taking water-soluble metal salt as a template and carbon nanotubes and polyvinylidene fluoride as raw materials, and further prepare a novel liquid metal composite phase change material by utilizing a pore passage packaged liquid metal phase change core material, thereby developing a simplified, rapid and green novel liquid metal composite phase change material, improving the heat dissipation performance of an electronic element CPU, effectively solving the problem of line short circuit caused by free flow of liquid metal by the prepared shaped composite phase change material, simultaneously realizing diversified liquid metal selection, meeting the requirements of efficient heat dissipation of CPUs in different temperature ranges and also meeting the requirement of dynamic heat dissipation of flexible electronic elements.
The technical scheme of the invention is as follows: 1) firstly, uniformly mixing water-soluble metal salt, carbon nano tube and polyvinylidene fluoride raw materials in different proportions by adopting a physical mixing method, placing the mixture in a mould in a specific shape, then placing the mould in an oven at the temperature of 200-300 ℃ for a certain time to obtain a block material in a specific shape, and finally placing the block material in hot water to completely dissolve the metal salt in the block material so as to obtain the flexible carbon nano tube sponge in a specific shape. The flexible carbon nanotube sponges with different apertures can be obtained by adjusting the proportion of the raw materials, so that different types of liquid metal core materials can be better matched; 2) the prepared carbon nano tube sponge carrier material and liquid metal are simultaneously placed in a vacuum environment by adopting a melt impregnation method, the carbon nano tube sponge carrier material and the liquid metal are melted at a proper temperature according to the type of the liquid metal core material, the liquid metal core material is adsorbed and limited in a pore channel by utilizing the pore channel of the carrier material in the vacuum environment, and then the novel liquid metal composite phase-change material is obtained by cooling.
The preparation method comprises the following specific steps:
(1) preparing a flexible carbon nanotube sponge carrier:
firstly, uniformly mixing water-soluble metal salt, carbon nano tube and polyvinylidene fluoride raw materials, then placing the mixture into a mould with a specific shape, and placing the mould into an oven with the temperature of 200-300 ℃ for 1-5 h. Finally, the product is placed in hot water at 50-90 ℃ for washing for multiple times to completely remove the water-soluble metal salt in the product, and the product is dried in vacuum at 100-150 ℃ for 12-36h to obtain the flexible carbon nanotube sponge carrier material with a specific shape. Wherein, the water-soluble metal salt: carbon nanotube: the mass ratio of the polyvinylidene fluoride is as follows: 1-10:1-100:1-10.
(2) Preparing a liquid metal composite phase-change material:
and vacuumizing the prepared flexible carbon nanotube sponge carrier material at 100 ℃ for 12-36h, and completely opening the inner pore channel. And then placing the carbon nano tube sponge carrier material subjected to vacuum treatment and liquid metal into a vacuum flask at the same time, selecting a proper temperature to melt the liquid metal core material according to the type of the liquid metal core material, adsorbing and limiting the liquid metal core material in the pore channel by utilizing the pore channel of the carrier material in a vacuum environment, and then cooling to obtain the novel liquid metal composite phase-change material. Wherein the mass ratio of the liquid metal core material to the carbon nano tube sponge carrier is 1-100: 1-100.
Further, the water-soluble metal salt includes: one or more of sodium chloride, potassium chloride, magnesium chloride, calcium chloride, ammonium chloride, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium sulfate, potassium sulfate, sodium bisulfate, potassium bisulfate, etc.
Further, the liquid metal core material includes: bi20Pb20Hg60(20℃)、Bi45Pb23Sn8Cd5In19(47℃)、Bi49Pb18Sn12In21(57℃)、Bi50Pb27Sn13Cd10(70℃)、Bi52Pb40Cd8(92℃)、Bi53Pb32Sn15(96℃)、Bi54Pb26Cd20(103℃)、Bi55.5Pb44.5(124℃)、Bi56Sn40Zn4(130℃)、Bi29Pb43Sn28(132℃)、Bi57Sn43(138℃)、Pb32Sn50Cd18(145℃)、Bi50Pb50(160 ℃) and the like, wherein the subscript numbers represent the percent ingredients and the temperature represents the melting point.
The invention has the advantages that: 1) developing a simplified, rapid and green novel liquid metal composite phase-change material; 2) the liquid metal is diversified in selection, and the high-efficiency heat dissipation of the CPU in different temperature ranges can be realized; 3) the pore structure is adjustable, the problem of short circuit of the electronic element circuit caused by free flow of liquid metal can be effectively prevented, and dynamic heat dissipation of the flexible electronic element can be met.
Drawings
Fig. 1 is a flexible representation of the carbon nanotube sponge obtained in example 1 of the present invention.
Fig. 2 is an SEM of the carbon nanotube sponge obtained in example 1 of the present invention.
Fig. 3 is a TEM of the carbon nanotube sponge obtained in example 1 of the present invention.
Fig. 4 shows Raman of the carbon nanotube sponge obtained in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained with reference to the specific embodiments.
Example 1
(1) Preparing a flexible carbon nanotube sponge carrier material:
uniformly and mechanically mixing 1g of polyvinylidene fluoride, 7g of sodium chloride and 0.2g of carbon nanotubes, adding the mixture into a cylindrical mold, putting the cylindrical mold into a drying oven at 200 ℃ for 4 hours, taking out the product, immersing the product into hot water at 90 ℃ to completely dissolve the sodium chloride inside, and finally drying the product in a vacuum drying oven at 100 ℃ for 24 hours to obtain the cylindrical flexible carbon nanotube sponge carrier material, wherein the flexibility demonstration is shown in a figure 1, the SEM is shown in a figure 2, the TEM is shown in a figure 3, and the Raman is shown in a figure 4.
(2) Preparing a liquid metal composite phase-change material:
and vacuumizing the prepared flexible carbon nanotube sponge carrier material for 24h at 100 ℃, and completely opening the inner pore channel. Then the vacuum-treated carbon nano tube sponge carrier material and liquid metal Bi are added45Pb23Sn8Cd5In19Simultaneously placing the mixture into a vacuum flask, heating the mixture to 50 ℃ to melt the mixture, and utilizing the pore channels of the carrier material to melt the liquid metal Bi in a vacuum environment45Pb23Sn8Cd5In19Adsorbing and limiting in the pore canal, and then cooling to obtain the novel liquid metal Bi45Pb23Sn8Cd5In19A composite phase change material.
Example 2
(1) Preparing a flexible carbon nanotube sponge carrier material:
and (2) mechanically and uniformly mixing 0.8g of polyvinylidene fluoride, 5g of sodium chloride and 0.3g of carbon nano tube, adding the mixture into a square mold, placing the square mold into a 220 ℃ oven for 2 hours, taking out a product, immersing the product into 80 ℃ hot water to completely dissolve the sodium chloride inside, and finally drying the product in a 120 ℃ vacuum oven for 18 hours to obtain the square flexible carbon nano tube sponge carrier material.
(2) Preparing a liquid metal composite phase-change material:
and (3) vacuumizing the prepared flexible carbon nanotube sponge carrier material for 18h at the temperature of 100 ℃, and completely opening the inner pore channel. Then the vacuum-treated carbon nano tube sponge carrier material and liquid metal Bi are added49Pb18Sn12In21Simultaneously placing the mixture into a vacuum flask, heating the mixture to 60 ℃ to melt the mixture, and utilizing the pore channels of the carrier material to melt the liquid metal Bi in a vacuum environment49Pb18Sn12In21Adsorbing and limiting in the pore canal, and then cooling to obtain the novel liquid metal Bi49Pb18Sn12In21A composite phase change material.
Embodiment 3
(1) Preparing a flexible carbon nanotube sponge carrier material:
and (2) mechanically and uniformly mixing 0.6g of polyvinylidene fluoride, 6g of sodium chloride and 0.5g of carbon nano tube, then adding the mixture into a rectangular mould, putting the mould into a 240 ℃ drying oven for 1h, taking out the product, immersing the product into 85 ℃ hot water to completely dissolve the sodium chloride in the product, and finally drying the product in a 140 ℃ vacuum drying oven for 20h to obtain the rectangular flexible carbon nano tube sponge carrier material.
(2) Preparing a liquid metal composite phase-change material:
and (3) vacuumizing the prepared flexible carbon nanotube sponge carrier material for 20h at 100 ℃, and completely opening the inner pore channel. Then the vacuum-treated carbon nano tube sponge carrier material and liquid metal Bi are added50Pb27Sn13Cd10Simultaneously placing the mixture into a vacuum flask, heating the mixture to 75 ℃ to melt the mixture, and utilizing the pore channels of the carrier material to melt the liquid metal Bi in a vacuum environment50Pb27Sn13Cd10Adsorbing and limiting in the pore canal, and then cooling to obtain the novel liquid metal Bi50Pb27Sn13Cd10A composite phase change material.
Example 4
(1) Preparing a flexible carbon nanotube sponge carrier material:
and (2) mechanically and uniformly mixing 0.5g of polyvinylidene fluoride, 10g of sodium chloride and 0.8g of carbon nano tube, then adding the mixture into a diamond-shaped mold, putting the mold into a 250 ℃ oven for 5 hours, taking out the product, immersing the product into 80 ℃ hot water to completely dissolve the sodium chloride in the product, and finally drying the product in a 120 ℃ vacuum oven for 36 hours to obtain the diamond-shaped flexible carbon nano tube sponge carrier material.
(2) Preparing a liquid metal composite phase-change material:
and vacuumizing the prepared flexible carbon nanotube sponge carrier material for 36h at 100 ℃, and completely opening the inner pore channel. Then the vacuum-treated carbon nano tube sponge carrier material and liquid metal Bi are added52Pb40Cd8Simultaneously placing the mixture into a vacuum flask, heating the mixture to 95 ℃ to melt the mixture, and utilizing the pore channels of the carrier material to melt the liquid metal Bi in a vacuum environment52Pb40Cd8Adsorbing and limiting in the pore canal, and then cooling to obtain the novel liquid metal Bi52Pb40Cd8A composite phase change material.

Claims (4)

1. A preparation method of a liquid metal composite phase-change material is characterized by comprising the following preparation steps:
1) firstly, uniformly mixing water-soluble metal salt, carbon nano tube and polyvinylidene fluoride raw materials in different proportions by adopting a physical mixing method, placing the mixture in a mould in a specific shape, then placing the mould in an oven at the temperature of 200-300 ℃ for a certain time to obtain a block material in a specific shape, and finally placing the block material in hot water to completely dissolve the metal salt in the block material so as to obtain flexible carbon nano tube sponge in a specific shape; the flexible carbon nanotube sponges with different apertures can be obtained by adjusting the proportion of the raw materials, so that different types of liquid metal core materials can be better matched;
2) and (2) simultaneously placing the prepared carbon nanotube sponge carrier material and liquid metal in a vacuum environment by adopting a melt impregnation method, selecting a proper temperature to melt the liquid metal core material according to the type of the liquid metal core material, adsorbing and limiting the liquid metal core material in the pore channel by utilizing the pore channel of the carrier material in the vacuum environment, and then cooling to obtain the liquid metal composite phase-change material.
2. The preparation method of the liquid metal composite phase-change material according to claim 1, which is characterized by comprising the following specific preparation steps:
(1) preparing a flexible carbon nanotube sponge carrier:
firstly, uniformly mixing water-soluble metal salt, a carbon nano tube and a polyvinylidene fluoride raw material, then placing the mixture in a mould with a specific shape, and placing the mould in an oven at 300 ℃ of 200-; finally, the product is placed in hot water at the temperature of 50-90 ℃ for washing for multiple times to completely remove the water-soluble metal salt in the product, and the product is dried in vacuum at the temperature of 100-150 ℃ for 12-36h to obtain the flexible carbon nanotube sponge carrier material with a specific shape; wherein, the water-soluble metal salt: carbon nanotube: the mass ratio of the polyvinylidene fluoride is as follows: 1-10:1-100: 1-10;
(2) preparing a liquid metal composite phase-change material:
vacuumizing the prepared flexible carbon nanotube sponge carrier material for 12-36h at 100 ℃, and completely opening the inner pore channel; then placing the carbon nanotube sponge carrier material subjected to vacuum treatment and liquid metal into a vacuum flask at the same time, selecting a proper temperature to melt the liquid metal core material according to the type of the liquid metal core material, adsorbing and limiting the liquid metal core material in a pore channel by utilizing the pore channel of the carrier material in a vacuum environment, and then cooling to obtain a liquid metal composite phase-change material; wherein the mass ratio of the liquid metal core material to the carbon nano tube sponge carrier is 1-100: 1-100.
3. The method for preparing a liquid metal composite phase change material according to claim 1 or 2, wherein the water-soluble metal salt comprises: one or more of sodium chloride, potassium chloride, magnesium chloride, calcium chloride, ammonium chloride, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium sulfate, potassium sulfate, sodium bisulfate and potassium bisulfate.
4. The method for preparing a liquid metal composite phase change material according to claim 1 or 2, wherein the liquid metal core material comprises: bi20Pb20Hg60Melting point of 20 ℃ and Bi45Pb23Sn8Cd5In19Melting point of 47 ℃ and Bi49Pb18Sn12In21Melting point 57 ℃ and Bi50Pb27Sn13Cd10Melting point 70 ℃ and Bi52Pb40Cd8Melting point of 92 ℃ and Bi53Pb32Sn15Melting point of 96 ℃ and Bi54Pb26Cd20Melting point of 103 ℃ and Bi55.5Pb44.5Melting point of 124 ℃ and Bi56Sn40Zn4Melting point of 130 ℃ and Bi29Pb43Sn28Melting point of 132 ℃ and Bi57Sn43Melting point of 138 ℃ and Pb32Sn50Cd18Melting point of 145 ℃ and Bi50Pb50One or more of the melting points of 160 ℃ andthe middle subscript numbers represent the percent ingredients and the temperatures represent melting points.
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