CN111635636A - Preparation method of anti-aging high-thermal-conductivity gasket - Google Patents

Preparation method of anti-aging high-thermal-conductivity gasket Download PDF

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CN111635636A
CN111635636A CN202010609510.4A CN202010609510A CN111635636A CN 111635636 A CN111635636 A CN 111635636A CN 202010609510 A CN202010609510 A CN 202010609510A CN 111635636 A CN111635636 A CN 111635636A
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mixture
composite powder
aging
powder
silicone oil
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崔巍
迟克禹
张耀伦
祝渊
孙琪
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Foshan Southern China Institute For New Materials
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Abstract

The invention provides a preparation method of an anti-aging high-thermal-conductivity gasket, which has a synergistic effect after spherical alumina powder with different particle sizes and micron-sized silicon nitride powder are adopted to form composite powder, so that the adhesion degree and the thermal conductivity of the prepared thermal-conductivity gasket are improved; before the composite powder is mixed with the base bodies of vinyl silicone oil and hydrogen-containing silicone oil for reaction, the surface of spherical alumina is improved in a pretreatment mode to enable the spherical alumina to be combined with the silicone oil more easily, after the reaction, aftertreatment is set, the reaction degree of a system can be further increased, and the heat-conducting gasket with higher bonding degree is obtained.

Description

Preparation method of anti-aging high-thermal-conductivity gasket
Technical Field
The invention relates to the field of preparation of high polymer materials, in particular to a preparation method of an anti-aging high-thermal-conductivity gasket.
Background
With the development of high integration and miniature size of electronic components and electronic modules, the heat productivity is higher and higher, the problems of slow operation and more dead halt caused by temperature rise are more and more caused, and the optimization of heat dissipation design becomes more and more important. In the design of a heat dissipation system, heat generated by a chip and a module is conducted away through a heat pipe, a heat dissipation sheet and a metal shell and released to the external environment, and a thermal interface material is applied to joints of the chip, the heat pipe, the heat dissipation sheet, the shell and the like to fill up small gaps, optimize a heat dissipation channel and help to reduce the working temperature of the chip and the module. The thermal interface material comprises a heat conduction gasket, heat conduction paste, a heat conduction phase change material, a heat conduction insulation sheet and the like, wherein the heat conduction gasket is generally applied to the aspects of high heat conductivity coefficient, compressibility and resilience and convenience in mounting and pasting. However, in the heat conducting gasket in the prior art, generally, a composite material obtained by mixing and curing silicone oil and a large amount of spherical alumina is used, a large amount of spherical alumina must be added in order to obtain higher heat conducting performance, however, the surface of the spherical alumina is hydrophilic, the addition amount of the spherical alumina in the silicone oil is limited, the phenomenon of pulverization of the heat conducting gasket exists in the preparation process, even the heat conducting performance is reduced, the hardness of the prepared gasket is high, and the quality of the product is poor.
For example, the heat conductive materials disclosed in patent nos. CN101151326A, CN101942122A and CN102051049A have low overall heat conductivity, high filler content and easy pulverization.
In combination, in the field of preparation of heat conduction materials, the heat conduction material still has the phenomena of poor heat conduction performance and easy pulverization in the preparation process.
Disclosure of Invention
The invention provides a preparation method of an anti-aging high-thermal-conductivity gasket, and aims to solve the problems that a thermal-conductivity gasket prepared in the prior art is poor in thermal conductivity and easy to pulverize during preparation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an anti-aging high-thermal-conductivity gasket comprises the following steps:
s1, weighing the composite powder, adding the composite powder into analytically pure absolute ethyl alcohol, uniformly dispersing the powder at a stirring speed of 1000-5000r/min, performing suction filtration for 3-5 times under the ultrasonic assistance to obtain the composite powder for later use;
s2, heating the composite powder in the step S1 at 80-100 ℃ to obtain dry composite powder;
s3, cooling the composite powder dried in the step S2 to room temperature, adding a coupling agent accounting for 1-3% of the weight of the composite powder, and mixing for 1-10min at a stirring speed of 100-3000r/min by using a high-speed stirrer to obtain a mixture A;
s4, pretreating the mixture A;
s5, adding vinyl silicone oil accounting for 4-5% of the weight of the composite powder and hydrogen-containing silicone oil accounting for 4-5% of the weight of the composite powder into the mixture A after the post-treatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-treating the mixture B;
s7, adding an inhibitor and a catalyst into the mixture B after the post-treatment, and uniformly mixing under the condition that the stirring speed is 1000-5000r/min to obtain a mixture C;
s8, pressing the mixture C into a sheet, and heating the sheet at 80-120 ℃ for 60-80min for molding to obtain the aging-resistant high-thermal-conductivity gasket;
wherein the composite powder consists of alumina powder with different grain sizes and micron-sized silicon nitride powder.
Optionally, the composite powder comprises, by mass percent, 40-70% of 90-120 micron spherical alumina powder, 15-30% of 40-70 micron spherical alumina powder, and 10-25% of 2-5 micron spherical alumina powder.
Optionally, the composite powder further comprises 5% of 2-3 μm silicon nitride by mass percentage.
Optionally, the addition amount of the absolute ethyl alcohol in the S1 is 1.5-2 times of the weight of the composite powder.
Optionally, the frequency of the ultrasonic assistance in S1 is 40-60KHz, and the time of the ultrasonic assistance is 1-2 h.
Optionally, the coupling agent is one or two of acetoxypropyl trimethoxysilane and n-octyl trimethoxysilane.
Optionally, the vinyl silicone oil has a vinyl content of 0.5 to 0.6 wt%, and the hydrogen-containing silicone oil has a hydrogen content of 0.3 to 0.4%.
Optionally, the addition amount of the inhibitor is 0.01-0.5% of the mixture B, and the addition amount of the catalyst is 0.01-1% of the mixture B according to the mass percentage.
Optionally, the inhibitor is ethynyl cyclohexanol and the catalyst is a platinum catalyst.
Compared with the prior art, the invention has the beneficial technical effects that:
1. according to the invention, after the spherical alumina powder with different particle sizes and the micron-sized silicon nitride powder are adopted to form the composite powder, the synergistic effect is achieved, and the adhesion degree and the heat conduction performance of the prepared heat conduction gasket are improved.
2. According to the invention, the filling rate of the spherical alumina is increased by adopting a mode of improving the interface of the spherical alumina and the silicone oil by using the coupling agent, the surface of the spherical alumina is improved in a pretreatment mode before the composite powder is mixed and reacted with the matrix of the vinyl silicone oil and the hydrogen-containing silicone oil, so that the spherical alumina and the silicone oil are combined more easily, and after the reaction, the post-treatment is arranged, so that the reaction degree of the system can be further increased, and the heat-conducting gasket with higher bonding degree can be obtained.
3. The invention fully disperses the composite powder in the absolute ethyl alcohol through the ultrasonic auxiliary effect, and obtains the composite powder through multiple times of suction filtration, thereby having positive influence on the loose degree of the prepared heat conducting structure.
4. The gasket prepared by the invention not only has high heat-conducting property, but also has remarkable temperature resistance and aging resistance, and can be kept stable, not aged and not pulverized under the condition of resisting temperature of 150 ℃ for 500 hours on the premise of ensuring proper hardness, so that the gasket has wider application field.
Drawings
The invention will be further understood from the following description in conjunction with the accompanying drawings.
Fig. 1 is a schematic flow chart illustrating a process for manufacturing an aging-resistant high thermal conductivity gasket according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. 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 not indicated by the manufacturer, and are all conventional products available commercially.
The invention relates to a preparation method of an anti-aging high-thermal-conductivity gasket, which is described in the following embodiment according to the figure 1:
example 1:
as shown in fig. 1, the invention provides a method for preparing an aging-resistant high thermal conductivity gasket, comprising the following steps:
s1, weighing the composite powder, adding the composite powder into analytically pure absolute ethyl alcohol, uniformly dispersing the powder at a stirring speed of 1000-5000r/min, performing suction filtration for 3-5 times under the ultrasonic assistance to obtain the composite powder for later use; in the embodiment, the addition amount of the absolute ethyl alcohol is 1.5-2 times of the weight of the composite powder; the frequency of the ultrasonic auxiliary action is 40-60KHz, and the time of the ultrasonic auxiliary action is 1-2 h;
s2, heating the composite powder in the step S1 at 80-100 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder obtained in the step S2 to room temperature, adding a coupling agent accounting for 1-3% of the weight of the composite powder, and mixing for 1-10min at a stirring speed of 100-3000r/min by using a high-speed stirrer to obtain a mixture A; in the embodiment, the coupling agent is one or two of acetoxypropyl trimethoxy silane and n-octyl trimethoxy silane;
s4, pretreating the mixture A; in this embodiment, the pretreatment is: heating the mixture A at 80-150 ℃ for 1-4 h;
s5, adding vinyl silicone oil accounting for 4-5% of the weight of the composite powder and hydrogen-containing silicone oil accounting for 4-5% of the weight of the composite powder into the mixture A subjected to pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B, wherein the vinyl silicone oil has a vinyl content of 0.5-0.6 wt% and the hydrogen content of the hydrogen-containing silicone oil is 0.3-0.4%;
s6, post-treating the mixture B; in this embodiment, the post-processing is: placing the mixture B at the temperature of 100 ℃ for 12-48 h;
s7, adding an inhibitor and a catalyst into the mixture B after the post-treatment, and uniformly mixing at the stirring speed of 1000-5000r/min to obtain a mixture C; in the embodiment, the adding amount of the inhibitor is 0.01-0.5% of the mixture B, the adding amount of the catalyst is 0.01-1% of the mixture B, the inhibitor is ethynyl cyclohexanol, and the catalyst is platinum catalyst;
s8, pressing the mixture C into a sheet, and heating the sheet at 80-120 ℃ for 60-80min for molding to obtain the aging-resistant high-thermal-conductivity gasket;
the composite powder consists of alumina powder and micron-sized silicon nitride powder with different particle sizes, and comprises, by mass, 40-70% of 90-120 micron spherical alumina powder, 15-30% of 40-70 micron spherical alumina powder, 10-25% of 2-5 micron spherical alumina powder and 5% of 2-3 micron silicon nitride.
Example 2:
s1, adding 150g of analytically pure absolute ethyl alcohol into 35g of 90-micron spherical alumina, 30g of 40-micron spherical alumina, 30g of 5-micron spherical alumina and 5g of 2-micron silicon nitride, stirring, uniformly mixing, placing in an ultrasonic cleaner, performing ultrasonic treatment for 1h by using 40KHz, performing suction filtration by using a Buchner funnel, and repeating for 3 times;
s2, heating the composite powder after the S1 in an oven at 80 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder to room temperature, adding 1g of coupling agent into a high-speed stirrer, and uniformly mixing for 2min at the rotation speed of 1000r/min to obtain a mixture A;
s4, preprocessing: placing the mixture A in an oven for heating treatment at 80 ℃ for 2 h;
s5, adding 4g of vinyl silicone oil and 4g of hydrogen-containing silicone oil into the mixture A after the pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-processing: placing the mixture B in an oven to be heated for 24 hours at 100 ℃;
s7, adding 0.01g of ethynyl cyclohexanol inhibitor and 0.01g of platinum catalyst into the mixture B after the post-treatment, and uniformly mixing by using a high-speed stirrer to obtain a mixture C;
s8, placing the mixture C between release films, pressing the mixture C into a sheet with the required thickness by using a press, finally heating the sheet in an oven at 80 ℃ for 60min until the sheet is formed, taking out the sheet and cooling the sheet to room temperature to obtain the high-thermal-conductivity gasket.
Example 3:
the present embodiment should be understood to include all the features of the foregoing embodiments and further optimize the same, and therefore, the present embodiment provides an aging-resistant high thermal conductivity gasket and a method for preparing the same, including the following steps:
s1, adding 200g of analytically pure absolute ethyl alcohol into 50g of 90-micron spherical alumina, 25g of 40-micron spherical alumina, 20g of 5-micron spherical alumina and 5g of 2-micron silicon nitride, stirring, uniformly mixing, placing in an ultrasonic cleaner, performing ultrasonic treatment for 1.5h by using 60KHz, performing suction filtration by using a Buchner funnel, and repeating for 3 times;
s2, heating the composite powder after the S1 in an oven at 90 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder to room temperature, adding 1g of coupling agent into a high-speed stirrer, and uniformly mixing for 3min at the rotation speed of 1500r/min to obtain a mixture A;
s4, preprocessing: placing the mixture A in an oven for heating treatment at 80 ℃ for 2 h;
s5, adding 4g of vinyl silicone oil and 4g of hydrogen-containing silicone oil into the mixture A after the pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-processing: placing the mixture B in an oven to be heated for 24 hours at 100 ℃;
s7, adding 0.01g of ethynyl cyclohexanol inhibitor and 0.01g of platinum catalyst into the mixture B after the post-treatment, and uniformly mixing by using a high-speed stirrer to obtain a mixture C;
s8, placing the mixture C between release films, pressing the mixture C into a sheet with the required thickness by using a press, finally heating the sheet in an oven at 90 ℃ for 60min until the sheet is formed, taking out the sheet and cooling the sheet to room temperature to obtain the high-thermal-conductivity gasket.
Example 4:
the present embodiment should be understood to include all the features of any of the foregoing embodiments and further optimize the features, so that the present embodiment provides an aging-resistant high thermal conductivity gasket and a method for preparing the same, including the following steps:
s1, adding 150g of analytically pure absolute ethyl alcohol into 40g of 90-micron spherical alumina, 30g of 40-micron spherical alumina, 25g of 5-micron spherical alumina and 5g of 3-micron silicon nitride, stirring, uniformly mixing, placing in an ultrasonic cleaner, performing ultrasonic treatment for 2 hours by using 40KHz, performing suction filtration by using a Buchner funnel, and repeating for 5 times;
s2, heating the composite powder after the S1 in an oven at 100 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder to room temperature, adding 1g of coupling agent into a high-speed stirrer, and uniformly mixing for 4min at a rotation speed of 2000r/min to obtain a mixture A;
s4, preprocessing: placing the mixture A in an oven for heating treatment at 100 ℃ for 3 h;
s5, adding 5g of vinyl silicone oil and 5g of hydrogen-containing silicone oil into the mixture A subjected to pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-processing: placing the mixture B in an oven to be heated for 24 hours at 100 ℃;
s7, adding 0.04g of ethynyl cyclohexanol inhibitor and 0.03g of platinum catalyst into the mixture B after the post-treatment, and uniformly mixing by using a high-speed stirrer to obtain a mixture C;
s8, placing the mixture C between release films, pressing the mixture C into a sheet with the required thickness by using a press, finally heating the sheet in an oven at 100 ℃ for 70min until the sheet is formed, taking out the sheet and cooling the sheet to room temperature to obtain the high-thermal-conductivity gasket.
Example 5:
the present embodiment should be understood to include all the features of any of the foregoing embodiments and further optimize the features, so that the present embodiment provides an aging-resistant high thermal conductivity gasket and a method for preparing the same, including the following steps:
s1, adding 200g of analytically pure absolute ethyl alcohol into 40g of 90-micron spherical alumina, 30g of 40-micron spherical alumina and 25g of 5-micron spherical alumina and 5g of 2-micron silicon nitride, stirring, uniformly mixing, placing in an ultrasonic cleaner, performing ultrasonic treatment for 1.5h by using 40KHz, performing suction filtration by using a Buchner funnel, and repeating for 3 times;
s2, heating the composite powder after the S1 in an oven at 100 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder to room temperature, adding 1g of coupling agent into a high-speed stirrer, and uniformly mixing for 10min at a rotation speed of 2000r/min to obtain a mixture A;
s4, preprocessing: placing the mixture A in an oven for heating treatment at 100 ℃ for 3 h;
s5, adding 5g of vinyl silicone oil and 5g of hydrogen-containing silicone oil into the mixture A subjected to pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-processing: heating the mixture B in an oven at 100 ℃ for 36 h;
s7, adding 0.05g of ethynyl cyclohexanol inhibitor and 0.06g of platinum catalyst into the mixture B after the post-treatment, and uniformly mixing by using a high-speed stirrer to obtain a mixture C;
s8, placing the mixture C between release films, pressing the mixture C into a sheet with the required thickness by using a press, finally heating the sheet in an oven at 100 ℃ for 80min until the sheet is formed, taking out the sheet and cooling the sheet to room temperature to obtain the high-thermal-conductivity gasket.
Example 6:
the present embodiment should be understood to include all the features of any of the foregoing embodiments and further optimize the features, so that the present embodiment provides an aging-resistant high thermal conductivity gasket and a method for preparing the same, including the following steps:
s1, adding 200g of analytically pure absolute ethyl alcohol into 65g of 120-micron spherical alumina, 15g of 45-micron spherical alumina and 15g of 2-micron spherical alumina and 5g of 2-micron silicon nitride, stirring, uniformly mixing, placing in an ultrasonic cleaner, performing ultrasonic treatment for 1h by using 40KHz, performing suction filtration by using a Buchner funnel, and repeating for 5 times;
s2, heating the composite powder after the S1 in an oven at 90 ℃ to obtain dry composite powder;
s3, cooling the dried composite powder to room temperature, adding 3g of coupling agent into a high-speed stirrer, and uniformly mixing for 10min at a rotating speed of 3000r/min to obtain a mixture A;
s4, preprocessing: placing the mixture A in an oven for heating treatment at 80 ℃ for 2 h;
s5, adding 5g of vinyl silicone oil and 5g of hydrogen-containing silicone oil into the mixture A subjected to pretreatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-processing: putting the mixture B in an oven to be dried for 4h at 100 ℃;
s7, adding 0.04g of ethynyl cyclohexanol inhibitor and 0.04g of platinum catalyst into the mixture B after the post-treatment, and uniformly mixing by using a high-speed stirrer to obtain a mixture C;
s8, placing the mixture C between release films, pressing the mixture C into a sheet with the required thickness by using a press, finally heating the sheet in an oven at 120 ℃ for 80min until the sheet is formed, taking out the sheet and cooling the sheet to room temperature to obtain the high-thermal-conductivity gasket.
Comparative example 1:
the only difference from example 6 is that there are no pretreatment and post-treatment steps, the other steps being unchanged.
Comparative example 2:
the only difference from example 6 is that there is a pretreatment step, but no post-treatment step, the other steps being unchanged.
Comparative example 3:
the only difference from example 6 is that no coupling agent was added.
Comparative example 4:
the difference from example 6 is only that only two kinds of spherical alumina are added to the composite powder, which are respectively: 65g of 120 micron spherical alumina, 15g of 45 micron spherical alumina.
Comparative example 5:
the only difference from example 6 is that no silicon nitride was added to the composite powder.
Comparative example 6:
the difference from the embodiment 6 is that only one kind of spherical alumina and silicon nitride is added into the composite powder, specifically: 15g of 2 micron spherical alumina 5g of 2 micron silicon nitride.
Comparative example 7:
example 6 is different only in that the ultrasonic treatment was not performed using the ultrasonic cleaner in the step S1.
Test example I, hardness and thermal conductivity
Test samples: and the gaskets prepared in examples 2 to 6 and comparative examples 1 to 6 were subjected to relevant tests to obtain the hardness change and the degree of thermal conductivity of the prepared gaskets.
The test method comprises the following steps: the aging hardness is measured after placing each sample in an oven at 160 ℃ for continuous heating for 440 hours and then placing the sample at room temperature; the heat conductivity coefficient is detected by a heat conductivity coefficient tester.
And (3) test results: the results are shown in Table 1.
Table 1: hardness and thermal conductivity
Figure BDA0002560454800000101
Figure BDA0002560454800000111
As can be seen from comparison between comparative example 1 and comparative example 2, in comparative example 2 after pretreatment of heating the mixed alumina powder and the coupling agent, the high temperature resistance is improved compared with comparative example 1 without pretreatment, and the gasket after the pretreatment step can improve the temperature resistance and aging resistance; as can be seen from comparison of comparative example 2 and the example, the hardness change of the gasket subjected to the pretreatment and the post-treatment is smaller than that of the gasket subjected to the pretreatment only, which indicates that the temperature resistance and the aging resistance of the gasket subjected to the post-treatment step are improved; compared with the comparative example 3 and the embodiment, the preparation process does not use a coupling agent, so that the temperature resistance and the aging resistance of the gasket are good, but an effective heat conduction structure passage is not formed in the gasket, so that the heat conductivity is not high, and the heat conduction capability of the gasket is improved after the coupling agent is used; as can be seen from comparison between the comparative example 4 and the example, the thermal conductivity of the sample using only two kinds of alumina is lower than that of the sample using alumina with different particle sizes, because the thermal conduction structure formed by the sample using only two kinds of alumina is loose and not compact enough, which indicates that the thermal conduction performance of the sample can be improved by using alumina with different particle sizes; as can be seen from comparison between comparative example 5 and the example, the gasket using silicon nitride has higher thermal conductivity and smaller hardness change compared with the gasket without silicon nitride, which indicates that the addition of silicon nitride can improve the thermal conductivity and temperature resistance of the gasket. Compared with the embodiment, the comparative example 6 shows that the components in the composite powder have synergistic effect, so that the hardness of the gasket is comprehensively improved, the heat conductivity is improved, the pretreatment and the post-treatment are combined, the coupling agent is used, and the aluminum oxide with different particle sizes and the silicon nitride with the micron size of 2-3 are added, so that the heat conductivity, the temperature resistance and the aging resistance of the silica gel heat-conducting gasket are improved.
Test example two: degree of looseness
Test samples: the high thermal conductive gasket prepared in example 6, the composite powder after the step of example S1, the gasket prepared in comparative example 7 and the composite powder after the step of S1.
The test mode is as follows: after the step of S1 is completed, respectively scanning the tissue structures by using a microscope; after the preparation is completed, performing organizational structure scanning on the surface of the high thermal conductivity gasket prepared in example 6 (namely, a product is obtained after the preparation is completed), performing organizational structure scanning on the surface of the gasket prepared in comparative example 7 (namely, a product is obtained after the preparation is completed), analyzing by a technician, and performing record registration;
and (3) test results: the test results are shown in Table 2.
Table 2: degree of looseness
Figure BDA0002560454800000121
As can be seen from table 2, comparative example 7, which did not undergo the ultrasonic assistance, obtained composite powder having an arrangement uniformity which was generally inferior to that of example 6 in step S1, resulted in the production of a gasket having a surface texture microscopically rougher than that of example 6, and also having no compactness and a high uniformity as in example 6.
In combination, the high-thermal-conductivity gasket can keep stable, aging-free and powderless under the condition of resisting temperature of 150 ℃ for 500 hours on the premise of ensuring the use hardness; in addition, the heat conducting property is particularly excellent.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (9)

1. The preparation method of the aging-resistant high-thermal-conductivity gasket is characterized by comprising the following steps of:
s1, weighing the composite powder, adding the composite powder into analytically pure absolute ethyl alcohol, uniformly dispersing the powder at a stirring speed of 1000-5000r/min, performing suction filtration for 3-5 times under the ultrasonic assistance to obtain the composite powder for later use;
s2, heating the composite powder in the step S1 at 80-100 ℃ to obtain dry composite powder;
s3, cooling the composite powder dried in the step S2 to room temperature, adding a coupling agent accounting for 1-3% of the weight of the composite powder, and mixing for 1-10min at a stirring speed of 100-3000r/min by using a high-speed stirrer to obtain a mixture A;
s4, pretreating the mixture A;
s5, adding vinyl silicone oil accounting for 4-5% of the weight of the composite powder and hydrogen-containing silicone oil accounting for 4-5% of the weight of the composite powder into the mixture A after the post-treatment, and uniformly mixing by using a vacuum kneader to obtain a mixture B;
s6, post-treating the mixture B;
s7, adding an inhibitor and a catalyst into the mixture B after the post-treatment, and uniformly mixing under the condition that the stirring speed is 1000-5000r/min to obtain a mixture C;
s8, pressing the mixture C into a sheet, and heating the sheet at 80-120 ℃ for 60-80min for molding to obtain the aging-resistant high-thermal-conductivity gasket;
wherein the composite powder consists of alumina powder with different grain sizes and micron-sized silicon nitride powder.
2. The method of claim 1, wherein the composite powder comprises, by mass, 40-70% of 90-120 micron spherical alumina powder, 15-30% of 40-70 micron spherical alumina powder, and 10-25% of 2-5 micron spherical alumina powder.
3. The method for preparing an aging-resistant high thermal conductivity gasket according to claim 1, wherein the composite powder further comprises 5% by mass of 2-3 μm silicon nitride.
4. The method for preparing an aging-resistant high thermal conductivity gasket according to claim 1, wherein the amount of the absolute ethyl alcohol added in S1 is 1.5-2 times of the weight of the composite powder.
5. The method for preparing an aging-resistant high thermal conductivity gasket as claimed in claim 1, wherein the frequency of the ultrasonic assistance in S1 is 40-60KHz, and the time of the ultrasonic assistance is 1-2 h.
6. The method for preparing an aging-resistant high thermal conductivity gasket as claimed in claim 1, wherein the coupling agent is one or two of acetoxypropyl trimethoxysilane and n-octyl trimethoxysilane.
7. The method for preparing an aging-resistant high thermal conductivity gasket according to claim 1, wherein the vinyl silicone oil has a vinyl content of 0.5 to 0.6 wt%, and the hydrogen-containing silicone oil has a hydrogen content of 0.3 to 0.4 wt%.
8. The method for preparing an aging-resistant high thermal conductivity gasket according to claim 1, wherein the addition amount of the inhibitor is 0.01-0.5% of the mixture B, and the addition amount of the catalyst is 0.01-1% of the mixture B in terms of mass percentage.
9. The method for preparing an aging-resistant high thermal conductivity gasket according to claim 8, wherein the inhibitor is ethynylcyclohexanol, and the catalyst is platinum catalyst.
CN202010609510.4A 2020-06-29 2020-06-29 Preparation method of anti-aging high-thermal-conductivity gasket Pending CN111635636A (en)

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CN108129838A (en) * 2017-12-21 2018-06-08 广东乐图新材料有限公司 Heat-conducting pad and preparation method thereof, electronic device
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CN112080059A (en) * 2020-09-26 2020-12-15 追信数字科技有限公司 High-heat-conductivity low-temperature-resistant economical plastic heat exchange tube and manufacturing method thereof
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