CN115895269A - Heat-conducting gel and preparation method and application thereof - Google Patents
Heat-conducting gel and preparation method and application thereof Download PDFInfo
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- CN115895269A CN115895269A CN202211347346.XA CN202211347346A CN115895269A CN 115895269 A CN115895269 A CN 115895269A CN 202211347346 A CN202211347346 A CN 202211347346A CN 115895269 A CN115895269 A CN 115895269A
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Abstract
The invention discloses a heat-conducting gel and a preparation method and application thereof, wherein the preparation raw materials comprise a heat-conducting filler, a silicone oil matrix and a polyvinyl alcohol aqueous solution; the heat conducting filler comprises modified diamond and modified metal oxide; the surface of the modified diamond is modified with amino groups; the surface of the modified metal oxide is modified with epoxy groups. The heat-conducting gel provided by the invention has the advantages that the contact thermal resistance is reduced, and the heat-conducting performance of the heat-conducting gel is obviously improved.
Description
Technical Field
The invention relates to the technical field of new materials and application thereof, in particular to a heat-conducting gel and a preparation method and application thereof.
Background
With the development of high power consumption, miniaturization and integration of electronic devices, the energy density of the electronic devices is greatly increased, which brings about a severe heat dissipation problem. The failed thermal management can cause equipment blockage, circuit damage and serious potential safety hazard burying. Thermal interface materials are the best choice to help solve the heat dissipation problem. The heat-conducting gel is a heat-conducting interface material prepared from materials such as silicone oil, heat-conducting filler and the like. The heat dissipation device can be fully attached to the surface of a component, so that various gaps are filled, the thermal contact resistance between the component and a radiator is reduced, a heat dissipation channel is formed, and the heat dissipation device can play roles in insulation, shock absorption, sealing and the like.
Thermal gel is a thermal interface material with ultra-high conformability, is softer and has better surface affinity and can be compressed to very low thickness compared to thermal gaskets. The heat-conducting gel generally exists in a colloid form at normal temperature, has excellent plasticity, can adapt to various irregular, shape-changeable and rugged heat-radiating interfaces, and has more flexible and changeable application scenes. The heat-conducting gel on the market at present is mainly prepared by doping a heat-conducting filler in a silicone oil system. In order to obtain higher thermal conductivity, more thermal conductive filler is generally added into the resin system, and the filling ratio of the thermal conductive filler is increased to obtain better thermal conductivity. However, the compatibility of the inorganic heat-conducting fillers and the silicone oil is poor, so that the filling rate of the inorganic heat-conducting fillers is low, and the heat-conducting gel prepared by the inorganic heat-conducting fillers has low heat-conducting coefficient due to the existence of a large amount of silicone oil.
Therefore, it is urgent to develop a thermally conductive gel having high thermal conductivity.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides the heat-conducting gel which can improve the heat-conducting property of the heat-conducting gel.
According to the heat-conducting gel provided by the embodiment of the first aspect of the invention, the preparation raw materials comprise a heat-conducting filler, a silicone oil matrix and polyvinyl alcohol;
the heat conducting filler comprises modified diamond and modified metal oxide;
the surface of the modified diamond is modified with amino groups;
the surface of the modified metal oxide is modified with epoxy groups.
The heat-conducting gel provided by the embodiment of the invention has at least the following beneficial effects:
the surface of the diamond is modified with amino groups; the surface of the metal oxide is modified with epoxy groups, and the composite filler is formed by utilizing the chemical bond action of amino and epoxy groups. The composite heat-conducting filler is easy to form a heat-conducting channel when dispersed in a system, and phonon scattering can be effectively reduced when the composite heat-conducting filler assembled by chemical bonds is filled into a matrix, so that the heat-conducting property of the composite material is effectively improved. On the other hand, the invention utilizes the oxygen-containing functional groups on the surface of the metal oxide to react with the amino groups modified on the surface of the diamond, and realizes the directional distribution of the modified metal oxide and the modified diamond through the interaction of hydrogen bonds, thereby reducing the thermal resistance of the system and improving the thermal conductivity when the thermal conductive gel is formed subsequently.
According to some embodiments of the present invention, raw materials for preparing the thermal conductive gel include, by weight, 30 to 50 parts of the modified diamond, 20 to 25 parts of the modified metal oxide, 20 to 40 parts of the silicone oil matrix, and 10 to 20 parts of the polyvinyl alcohol aqueous solution.
According to some embodiments of the invention, the silicone oil matrix comprises at least one of a vinyl-containing silicone oil and a hydrogen-containing silicone oil.
According to some embodiments of the present invention, the raw material for preparing the modified diamond includes an aminosilane coupling agent, an alcohol aqueous solution, and diamond.
According to some embodiments of the present invention, in the method for preparing the modified diamond, the aminosilane coupling agent includes at least one of KH-550 and KH-792.
According to some embodiments of the invention, the diamond has a particle size in the range of 4 μm to 10 μm.
According to some embodiments of the invention, the method of making the modified diamond comprises: an aqueous alcohol solution of an aminosilane coupling agent is mixed with diamond.
According to some embodiments of the invention, the method of preparing the aqueous alcohol solution of an aminosilane coupling agent comprises mixing an aminosilane coupling agent with water.
According to some embodiments of the invention, the temperature of the mixing in the preparation of the aqueous alcohol solution of the aminosilane coupling agent is in the range of 30 to 40 ℃.
According to some embodiments of the invention, the mixing time in the preparation of the aqueous alcohol solution of the aminosilane coupling agent is 30 to 60min.
According to some embodiments of the invention, in the method for preparing modified diamond, the mixing time is 2 to 8 hours.
According to some embodiments of the invention, in the method of preparing the modified diamond, the mixing temperature is 60 to 80 ℃.
According to some embodiments of the present invention, the raw materials for preparing the modified metal oxide include an epoxy silane coupling agent, an alcohol aqueous solution, and a metal oxide.
According to some embodiments of the present invention, in the method for preparing the modified metal oxide, the epoxysilane coupling agent comprises KH-560.
According to some embodiments of the invention, the method of preparing the modified metal oxide comprises: an alcohol aqueous solution of an epoxy silane coupling agent and a metal oxide are mixed.
According to some embodiments of the invention, the method of preparing the aqueous alcohol solution of the epoxy silane coupling agent comprises mixing the epoxy silane coupling agent and water.
According to some embodiments of the invention, the temperature of the mixing in the preparation of the aqueous alcohol solution of the epoxysilane coupling agent is 30 to 40 ℃.
According to some embodiments of the invention, the mixing time in the preparation of the alcohol-water solution of the epoxysilane coupling agent is 30 to 60min.
According to some embodiments of the invention, in the method for preparing the modified metal oxide, the mixing time is 20 to 80min.
According to some embodiments of the invention, in the method of preparing the modified metal oxide, the mixing temperature is 80 to 130 ℃.
According to some embodiments of the invention, the metal oxide comprises at least one of aluminum oxide, magnesium oxide, and zinc oxide.
According to some embodiments of the invention, the metal oxide has a particle size of 0.5 to 20 μm.
According to some preferred embodiments of the present invention, the metal oxide has a particle size of 0.5 to 2 μm.
According to a second aspect of the invention, a method for preparing a heat conducting gel comprises the following steps:
s1, dispersing the heat-conducting filler and then mixing the dispersed heat-conducting filler with the polyvinyl alcohol;
s2, mixing the mixture obtained after mixing in the step S1 with the silicone oil matrix after cold treatment;
the temperature of the cold treatment is-20 to-10 ℃.
The preparation method of the invention at least has the following beneficial effects:
in the cold treatment process, the polyvinyl alcohol aqueous solution is cooled and frozen, the formed ice crystals can generate specific orientation, the orientation force of the ice crystals can separate the heat-conducting filler from the polyvinyl alcohol, the heat-conducting filler is extruded on the ice crystal interface to complete the oriented arrangement, and after the continuous reaction is carried out to obtain the heat-conducting gel, the oriented heat-conducting gel has ultrahigh heat-conducting performance in the axial arrangement direction. When the oriented heat-conducting gel is applied to electronic products, high heat-conducting performance can be realized by using less heat-conducting filler, and the filler in oriented arrangement is more favorable for the thermal weight balance of the whole composite material, so that the heat dissipation balance of the whole material is improved.
According to some embodiments of the present invention, in the preparation method of the thermal conductive gel, in the step S1, the mixing temperature is 60 to 75 ℃.
According to some embodiments of the present invention, in the preparation method of the thermal conductive gel, in step S1, the mixing time is 30 to 80min.
According to some embodiments of the present invention, in the preparation method of the heat conductive gel, in step S1, the mixing includes stirring and mixing.
According to some embodiments of the present invention, in the preparation method of the heat conducting gel, in step S1, the rotation speed of the stirring and mixing is 200 to 500r/min.
According to some embodiments of the invention, in the method for preparing the heat conductive gel, the temperature of the cold treatment is-20 to-10 ℃.
According to some embodiments of the present invention, in the preparation method of the thermal conductive gel, the cooling time is 10 to 14 hours.
According to some embodiments of the present invention, in the preparation method of the thermal conductive gel, in step S2, the mixing time is 1 to 5 hours.
According to some embodiments of the present invention, in the method for preparing the thermally conductive gel, in step S2, the mixing includes stirring and mixing.
According to some embodiments of the present invention, in the preparation method of the heat conducting gel, in step S2, the rotation speed of the stirring and mixing is 200 to 500r/min.
The application of the heat-conducting gel in the electronic equipment heat dissipation field is disclosed.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The following is illustrative of the invention by reference to the examples, which are intended to be illustrative only and are not to be construed as limiting the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1
The embodiment discloses a heat-conducting gel and a preparation method thereof, and the preparation method specifically comprises the following steps:
the preparation method of the modified diamond in the embodiment comprises the following steps:
a1: according to the parts by weight, 0.5 part of silane coupling agent (KH-550), 0.5 part of anhydrous ethanol and 0.1 part of distilled water are uniformly mixed and hydrolyzed in a constant-temperature water bath at 30 ℃ for 30min to obtain silane coupling agent hydrolysate; and adding 100 parts of diamond into a high-speed mixer, heating to 74 ℃, adding the silane coupling agent hydrolysate, continuously stirring for 4 hours, washing for 3 times by using acetone after the reaction is finished, and drying after vacuum filtration to obtain the modified diamond.
The preparation method of the modified metal oxide in this embodiment is as follows:
b1: according to the parts by weight, 0.5 part of silane coupling agent (KH-560), 0.5 part of absolute ethyl alcohol and 0.1 part of distilled water are uniformly mixed and hydrolyzed in a constant-temperature water bath at 30 ℃ for 30min to obtain silane coupling agent hydrolysate; adding 100 parts by mass of alumina powder into a high-speed mixer, heating to 110 ℃, adding the silane coupling agent hydrolysate, and continuously stirring for 30min to obtain the modified alumina with the surface modified by the epoxy group.
The preparation method of the heat-conducting gel of the embodiment specifically comprises the following steps:
c1, reacting 40 parts of modified diamond, 20 parts of modified alumina and 20 parts of polyvinyl alcohol aqueous solution at 75 ℃ for 30min at 200r/min to obtain mixed slurry;
and C2, cooling the mixed slurry obtained in the step C1 at the temperature of minus 25 ℃ for 12 hours, unfreezing the mixed slurry, and putting 40 parts of vinyl-containing silicone oil into a planetary mixer, wherein the mixing speed is 200r/min, and the mixing time is 1 hour. And after stirring, taking out the mixture to obtain the heat-conducting gel.
Example 2
This example discloses a method for preparing a thermally conductive gel, and differs from example 1 in that the amount of modified diamond is 45 parts, and the other conditions are the same.
Example 3
This example discloses a method for preparing a thermally conductive gel, and differs from example 1 in that the amount of modified diamond is 50 parts, and the other conditions are the same.
Example 4
This example discloses a method for preparing a thermally conductive gel, and differs from example 1 in that the amount of modified diamond is 30g, and the other conditions are the same.
Comparative example 1
This comparative example discloses a method for preparing a thermally conductive gel, and is different from example 1 in that unmodified diamond is added, and the other conditions are the same.
Comparative example 2
This comparative example discloses a method for preparing a thermally conductive gel, and is different from example 1 in that an unmodified metal oxide is added, and the other conditions are the same.
Comparative example 3
The comparative example discloses a method for preparing a thermal conductive gel, and is different from example 1 in that an aqueous polyvinyl alcohol solution is not added, and the other conditions are the same.
Comparative example 4
This comparative example discloses a method for preparing a thermally conductive gel, and differs from example 1 in that no cold treatment is performed, and the other conditions are the same.
Test example 1
The thermally conductive gels prepared in the above examples and comparative examples were subjected to a performance test,
and (3) testing the heat conduction performance: a standard test method for measuring heat conduction in the vertical direction by a steady state method is characterized in that a test instrument is an LW-9389TIM resistance and conductivity measuring instrument, and the method comprises the following specific steps: the relationship between thermal resistance RTotal and thickness BLT of three thermal interface composite materials with different thicknesses is respectively tested at the temperature of 80 ℃ and the pressure of 10psi, the obtained data are subjected to linear fitting, as shown in formula (1), the slope is the thermal conductivity coefficient kappa TIM of the thermal interface material, and the intercept with the y axis is the contact thermal resistance RContact:
R Total ＝R Contact +BLT/κ TIM (1)；
the test results are shown in table 1.
TABLE 1 Heat conductive gel Performance test
The difference between comparative example 1 and example 1 is that: the added diamond is not modified, under the condition, the composite heat-conducting filler cannot form an effective heat-conducting channel in a system, and meanwhile, the modified metal oxide and the modified diamond cannot be interacted through hydrogen bonds, so that the directional distribution of the modified metal oxide and the modified diamond cannot be realized, and the heat-conducting property is reduced.
The difference between comparative example 2 and example 1 is that: the added metal oxide is not modified, the composite heat-conducting filler can not form an effective heat-conducting channel in a system under the condition, and the modified metal oxide and the modified diamond can not be interacted through hydrogen bonds, so that the directional distribution of the modified metal oxide and the modified diamond can not be realized, and the heat-conducting property is reduced.
The difference between comparative example 3 and example 1 is that: without adding the polyvinyl alcohol aqueous solution, an effective heat conduction path cannot be formed under the condition, so that the heat conduction performance is reduced.
The difference between comparative example 4 and example 1 is that: the heat conducting performance is reduced because an effective heat conducting path cannot be formed under the condition that the polyvinyl alcohol aqueous solution is not subjected to cold treatment.
The surface of the diamond is modified with amino groups; the surface of the metal oxide is modified with epoxy groups, and the composite filler is formed by utilizing the chemical bond action of amino and epoxy groups. The composite heat-conducting filler can more easily form a heat-conducting channel when dispersed in a system, so that the heat-conducting property of the composite material is effectively improved. On the other hand, the invention utilizes the oxygen-containing functional group on the surface of the metal oxide to react with the amino group modified on the surface of the diamond, and realizes the directional distribution of the modified metal oxide and the modified diamond through the interaction of hydrogen bonds, thereby reducing the thermal resistance of the system and improving the thermal conductivity when the thermal conductive gel is formed subsequently.
Claims (10)
1. A thermally conductive gel, comprising: the preparation raw materials comprise heat-conducting filler, a silicone oil matrix and a polyvinyl alcohol aqueous solution;
the heat conducting filler comprises modified diamond and modified metal oxide;
the surface of the modified diamond is modified with amino groups;
the surface of the modified metal oxide is modified with epoxy groups.
2. The heat-conducting gel according to claim 1, wherein the heat-conducting gel is prepared from 30-50 parts by weight of the modified diamond, 20-25 parts by weight of the modified metal oxide, 20-40 parts by weight of the silicone oil matrix and 10-20 parts by weight of the polyvinyl alcohol aqueous solution.
3. The thermally conductive gel of claim 1, wherein the silicone oil matrix comprises at least one of vinyl silicone oil and hydrogen-containing silicone oil.
4. The thermally conductive gel of claim 1, wherein the modified diamond is prepared by a method comprising: an aqueous alcohol solution of an aminosilane coupling agent is mixed with diamond.
5. The thermally conductive gel of claim 1, wherein the modified metal oxide is prepared by a method comprising: an alcohol aqueous solution of an epoxy silane coupling agent and a metal oxide are mixed.
6. The thermally conductive gel of claim 5, wherein the metal oxide comprises at least one of aluminum oxide, magnesium oxide, and zinc oxide.
7. The thermally conductive gel of claim 5 or 6, wherein the metal oxide has a particle size of 0.5-20 μm.
8. A method for preparing a thermally conductive gel as claimed in any one of claims 1 to 7, comprising the steps of:
s1, mixing the heat-conducting filler and the polyvinyl alcohol aqueous solution;
s2, mixing the mixture obtained after mixing in the step S1 with the silicone oil matrix after cold treatment;
the temperature of the cold treatment is-20 to-10 ℃.
9. The method according to claim 8, wherein the temperature of the mixing in step S1 is 60 to 75 ℃.
10. Use of a thermally conductive gel as claimed in any one of claims 1 to 7 in the field of heat dissipation in electronic devices.
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