CN111909522B - Heat-conducting insulating material and preparation method thereof - Google Patents
Heat-conducting insulating material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heat-conducting insulating material and a preparation method thereof, wherein the heat-conducting insulating material comprises a silica gel matrix and a filler, and the filler accounts for 80-99% of the heat-conducting insulating material by mass; wherein, the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%. Through the mode, the heat-conducting insulating material has higher heat conductivity coefficient, so that the prepared product has higher heat-conducting property and excellent insulating property.
Description
Technical Field
The application relates to the technical field of heat conduction materials, in particular to a heat conduction insulating material and a preparation method thereof.
Background
Statistics show that the reliability of the electronic components is reduced by 10% when the temperature of the electronic components is increased by 2 ℃, and the service life of the electronic components is doubled when the temperature is reduced by 8 ℃.
Therefore, the role of thermal interface materials in the field of information technology is becoming more and more important. How to further improve the thermal conductivity of the thermal interface material and reduce the thermal resistance is still a very important issue for the electronic packaging and heat dissipation engineering.
Disclosure of Invention
The application mainly provides a heat-conducting insulating material and a preparation method thereof, and the heat-conducting insulating material has higher heat conductivity coefficient, so that the prepared product has higher heat-conducting property and excellent insulating property.
In order to solve the technical problem, the application adopts a technical scheme that: the heat-conducting insulating material is provided, the raw materials of the heat-conducting insulating material comprise a silica gel matrix and a filler, and the mass percentage of the filler in the heat-conducting insulating material is 80-99%; wherein, the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%.
In order to solve the above technical problem, another technical solution adopted by the present application is: the preparation method of the heat-conducting insulating material comprises the following steps: obtaining a filler, and carrying out first treatment on the filler to obtain a first mixture; obtaining a silica gel matrix, and mixing the first mixture with the silica gel matrix to obtain a second mixture; carrying out second treatment on the second mixture to obtain a heat-conducting insulating material; wherein, in the heat-conducting insulating material, the mass percentage of the filler is 80-99%, the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%.
The beneficial effect of this application is: different from the situation of the prior art, the heat-conducting insulating material comprises a silica gel matrix and a filler, wherein the filler accounts for 80-99% of the heat-conducting insulating material by mass; and the aluminum nitride particles and the aluminum oxide particles with higher heat conductivity are compounded in the filler, and the aluminum nitride particles and the aluminum oxide particles with a certain particle size range are selected, so that the particle sizes of the aluminum nitride particles and the aluminum oxide particles reach a certain proportion, and an efficient heat-conducting network is constructed, namely the particle size of the aluminum nitride particles is 50-100 mu m, the particle size of the aluminum oxide particles is 1-30 mu m, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, the heat-conducting insulating material has higher heat conductivity coefficient, and the prepared product has higher heat-conducting property and excellent insulating property.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts. Wherein:
FIG. 1 is a schematic flow chart illustrating an embodiment of a method for making a thermally conductive insulating material according to the present invention;
fig. 2 is a schematic flow chart of another embodiment of the method for preparing the thermally conductive insulating material of the present application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
In the related technology, the material of the heat-conducting insulating silica gel gasket is generally prepared by compounding alumina particles and silica gel, the heat conductivity coefficient is only about 75W/(m.K) at most, and the aluminum nitride particles have high heat conductivity and high insulativity, the theoretical value of single crystal of the aluminum nitride particles is 320W/(m.K), and the actual value can still reach 100W/(m.K) -280W/(m.K), which is 5-10 times of that of the alumina particles; in order to increase the heat conductivity, the existing research also tries to adopt aluminum nitride particles as fillers to improve the heat conductivity coefficient of the heat conducting gasket, but the high heat conducting requirement cannot be met.
Based on the above, the present application provides a heat conducting and insulating material, the raw materials of which include a silica gel matrix and a filler, and the mass percentage content of the filler in the heat conducting and insulating material can be 80% to 99%, for example, 80%, 82%, 84%, 85%, 87%, 88%, 90%, 92%, 94%, 98%, 99%.
Wherein, the filler can comprise aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles can be 50-100 μm, the particle size of the aluminum oxide particles can be 1-30 μm, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage content of the aluminum nitride particles can be 30-60%.
The particle size of the aluminum nitride particles may be, for example, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm. The alumina particles may have a particle size of, for example, 1 μm, 2 μm, 5 μm, 10 μm, 20 μm, or 30 μm.
The ratio of the average particle diameter of the aluminum nitride particles to the average particle diameter of the aluminum oxide particles is less than or equal to 5: 1, and may be greater than 5: 3, for example, can be 5: 1. 4.8: 1. 4.5: 1. 4: 1. 3.8: 1. 3.5: 1. 3: 1. 2:1 or 5: 3.
the mass percentage of the aluminum nitride particles in the filler may be, for example, 30%, 35%, 40%, 45%, 50%, or 60%.
The inventor of the present application finds, in long-term research and experiments, that high thermal conductivity can be obtained by adopting a way of compounding aluminum nitride particles and aluminum nitride particles, and the filler of the present embodiment not only utilizes the aluminum nitride particles with higher thermal conductivity and compounds the aluminum nitride particles with aluminum oxide particles, but also unexpectedly finds that when the mass and particle size of the aluminum oxide particles and the aluminum nitride particles reach a certain ratio, the thermal conductivity effect generated by the filler is far higher than that generated by singly adopting the aluminum oxide particles or the aluminum nitride particles as the filler. The heat-conducting insulating material prepared from the heat-conducting filler prepared by compounding the aluminum nitride particles and the aluminum oxide particles in different mass ratios and particle sizes can form an efficient heat-conducting network, so that the overall heat-conducting coefficient of the heat-conducting insulating material is improved, and can reach more than 8W/(m.K) and even exceed 9W/(m.K).
The heat-conducting insulating material comprises a silica gel matrix and a filler, wherein the filler accounts for 80-99% of the heat-conducting insulating material by mass; and the aluminum nitride particles and the aluminum oxide particles with higher heat conductivity are compounded in the filler, and the aluminum nitride particles and the aluminum oxide particles with a certain particle size range are selected, so that the particle sizes of the aluminum nitride particles and the aluminum oxide particles reach a certain proportion, and an efficient heat-conducting network is constructed, namely the particle size of the aluminum nitride particles is 50-100 mu m, the particle size of the aluminum oxide particles is 1-30 mu m, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, the heat-conducting insulating material has higher heat conductivity coefficient, and the prepared product has higher heat-conducting property and excellent insulating property.
Alternatively, the mass ratio of aluminum nitride particles to aluminum oxide particles may be in the range of 1: 2-1: 1, for example 1: 2. 3: 5. 4: 5. 9: 10 or 1: 1.
optionally, the aluminum nitride particles have a particle size gradient of 1-3 in a particle size range of 50-100 μm. The alumina particles may be at least one of spherical alumina particles, spheroidal alumina particles, alpha-alumina particles.
Optionally, the alumina particles have a particle size gradient of 2 to 5 in a particle size range of 1 μm to 30 μm. The aluminum nitride particles may be at least one of spherical aluminum nitride particles or particulate aluminum nitride particles.
Optionally, the aluminum nitride particles are spherical aluminum oxide particles having a particle size of at least one of 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm.
Optionally, the alumina particles are spherical aluminum nitride particles having a particle size of at least one of 1 μm, 2 μm, 5 μm, 10 μm, 20 μm, 30 μm
For example, only one kind of spherical aluminum nitride particle with a particle size of 50 μm can be selected as the filler; and selecting spherical alumina particles with three particle sizes, wherein the particle sizes of the three spherical alumina particles are respectively 20 mu m, 5 mu m and 1 mu m.
For example, only one kind of spherical aluminum nitride particles with a particle size of 100 μm can be selected as the filler; and selecting spherical alumina particles with four particle sizes, wherein the particle sizes of the three spherical alumina particles are respectively 30 mu m, 10 mu m, 2 mu m and 1 mu m.
For example, spherical aluminum nitride particles of two particle sizes, which are 80 μm and 50 μm, respectively, can be used as the filler; and selecting spherical alumina particles with three particle sizes, wherein the particle sizes of the three spherical alumina particles are respectively 10 mu m, 2 mu m and 1 mu m.
In the above example, it is also necessary to simultaneously mix the mass ratios of the alumina particles or the aluminum nitride particles with different particle diameters so that the ratio of the average particle diameter of the aluminum nitride particles to the average particle diameter of the alumina particles is less than or equal to 5: 1.
by limiting the particle size selection range of the aluminum nitride particles and the aluminum oxide particles, the overall thermal conductivity of the thermal conductive insulating material can be further improved.
Optionally, the filler may further comprise: surfactants and dispersants.
Wherein, the mass ratio of the alumina particles, the aluminum nitride particles, the surfactant and the dispersant can be 100-200: 80-160: 1-5: 5 to 10.
Specifically, the mass ratio of the alumina particles, the aluminum nitride particles, the surfactant and the dispersant may be 100: 80: 1: 5. 200: 150: 5: 10 or 150: 100: 3: 8.
understandably, in the raw materials for preparing the filler, the mass ratio of the aluminum nitride particles to the aluminum oxide particles can also be 1: 2-1: 1.
Alternatively, the surfactant may be at least one of hexamethyldisilazane, octyltrimethoxysilane, decyltrimethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethylsilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy), propyltrimethoxysilane.
Alternatively, the dispersant may be ethanol, which is used as a two-phase solvent and dispersant in the surface modification or modification of alumina particles and aluminum nitride particles.
Alternatively, the silica gel-based starting materials may include: polydimethylsiloxane, hydrogen-containing silicone oil, dimethyl silicone oil, a catalyst and an inhibitor.
Wherein, the mass ratio of the polydimethylsiloxane, the hydrogen-containing silicone oil, the dimethyl silicone oil, the catalyst and the inhibitor can be 100: 5-20: 5-20: 1-2: 0.1 to 0.2.
Specifically, the mass ratio of the polydimethylsiloxane, the hydrogen-containing silicone oil, the simethicone, the catalyst and the inhibitor can be 100: 5: 5: 1:0.1, 100: 20: 20: 2: 0.2 or 100: 15: 15: 1:0.15.
Alternatively, the polydimethylsiloxane is a vinyl terminated polydimethylsiloxane, which may have a viscosity of 50cps to 5000cps, for example 50cps, 100cps, 200cps, 500cps, 1000cps, 2000cps, 3000cps, 3500cps, 4000cps or 5000 cps.
The inventor researches and discovers that the strength and toughness of a cured crosslinking network can be improved by matching the vinyl-terminated polydimethylsiloxane with high and low viscosity. Therefore, the vinyl-terminated polydimethylsiloxane with the viscosity of 50-500 cps and the vinyl-terminated polydimethylsiloxane with the viscosity of 1000-5000 cps can be used in a compounding way, or the vinyl-terminated polydimethylsiloxane with the viscosity of 80-150 cps and the vinyl-terminated polydimethylsiloxane with the viscosity of 1500-2500 cps can be used in a compounding way, and the mass ratio of the high-viscosity vinyl-terminated polydimethylsiloxane to the low-viscosity vinyl-terminated polydimethylsiloxane is 9: 5-2.2: 1. For example, a vinyl terminated polydimethylsiloxane may be used in a combination of 150cps and 2000cps, wherein the mass ratio of the vinyl terminated polydimethylsiloxane having a viscosity of 150cps to the vinyl terminated polydimethylsiloxane having a viscosity of 2000cps is 2: 1.
Alternatively, the hydrogen-containing silicone oil may be a side chain hydrogen-containing silicone oil or an end side hydrogen-containing silicone oil, or at least two of the side chain hydrogen-containing silicone oil, the end hydrogen-containing silicone oil, and the end side hydrogen-containing silicone oil. The hydrogen content of the hydrogen-containing silicone oil can be 0.1-0.2%.
Optionally, the hydrogen-containing silicone oil can be a side chain hydrogen-containing silicone oil and a terminal hydrogen-containing silicone oil which are compounded for use. Wherein the mass ratio of the side chain hydrogen-containing silicone oil to the terminal hydrogen-containing silicone oil can be 9: 5-2.2: 1.
Alternatively, the dimethicone may have a viscosity of 50cps to 500cps, for example 50cps, 100cps, 200cps, 280cps, 350cps, 400cps, 440cps, or 500 cps.
Alternatively, the catalyst may be at least one of chloroplatinic acid isopropyl alcohol solution, platinum complex, platinum catalyst. The concentration of the catalyst may be 1000ppm to 5000ppm, for example 1000ppm, 1500ppm, 1800ppm, 2000ppm, 2200ppm, 2500ppm, 3000ppm, 3400ppm, 4000ppm, 4500ppm or 5000 ppm.
Wherein, the platinum catalyst can be Karstedt platinum catalyst, the concentration is 3000ppm, and the Karstedt platinum catalyst has high-efficiency catalytic activity and anti-poisoning property.
Alternatively, the inhibitor may be at least one of ethynl cyclohexanol, methyl butynol, phenyl butynol, vinyl ring, diallyl maleate, diallyl fumarate, silanized alkynol.
Alternatively, the inhibitor may be selected according to the inhibiting effect and curing temperature, and the inhibitor may be ethynl cyclohexanol.
Based on this, this application still provides a heat conduction insulating silica gel gasket, and this heat conduction insulating silica gel gasket's material can be the heat conduction insulating material in the above-mentioned heat conduction insulating material embodiment.
In a specific embodiment, the calendering thickness of the calender is adjusted to be 1.5mm (film thickness reduction), the heat-conducting and insulating material is subjected to cold press molding through the calender, and is cooled after being vulcanized by hot air in an oven, so that the heat-conducting and insulating silica gel gasket with a certain thickness (1.5 mm, for example) can be obtained.
Optionally, the hot air vulcanization temperature in the oven can be 80-150 ℃, and the vulcanization time can be 10-20 min.
For example, the hot air vulcanization temperature in the oven is 80 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, 100 deg.C, 120 deg.C, 130 deg.C, 140 deg.C or 150 deg.C, and the vulcanization time can be 10min, 12min, 14min, 16min, 18min or 20 min.
Based on the above, the application also provides a preparation method of the heat-conducting insulating material, which can be used for preparing the heat-conducting insulating material.
Referring to fig. 1, fig. 1 is a schematic flow chart illustrating a method for manufacturing a thermal conductive insulating material according to an embodiment of the present disclosure.
The embodiment provides a preparation method of a heat-conducting insulating material, which comprises the following steps:
s120: the filler is obtained and subjected to a first treatment to obtain a first mixture.
Wherein, in the raw materials of the heat-conducting insulating material, the mass percentage content of the filler is 80-99%, the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 μm, the particle size of the aluminum oxide particles is 1-30 μm, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%.
S140: and obtaining a silica gel matrix, and mixing the first mixture with the silica gel matrix to obtain a second mixture.
In one embodiment, the obtained silica gel matrix can be put into a kneader or a planetary mixer, and then the first mixture is added and fully and uniformly stirred in the kneader or the planetary mixer to obtain a second mixture.
S160: and carrying out second treatment on the second mixed material to obtain the heat-conducting insulating material.
In the embodiment, the heat-conducting insulating material can be obtained by obtaining the filler, performing first treatment on the filler to obtain a first mixture, then obtaining the silica gel matrix, mixing the first mixture with the silica gel matrix to obtain a second mixture, and performing second treatment on the second mixture, wherein the filler accounts for 80-99% of the raw materials of the heat-conducting insulating material in percentage by mass; and the aluminum nitride particles and the aluminum oxide particles with higher heat conductivity are compounded in the filler, and the aluminum nitride particles and the aluminum oxide particles with a certain particle size range are selected, so that the particle sizes of the aluminum nitride particles and the aluminum oxide particles reach a certain proportion, and an efficient heat-conducting network is constructed, namely the particle size of the aluminum nitride particles is 50-100 mu m, the particle size of the aluminum oxide particles is 1-30 mu m, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, the prepared heat-conducting insulating material has higher heat conductivity coefficient, and the prepared product has higher heat-conducting property and excellent insulating property.
Referring to fig. 2, fig. 2 is a schematic flow chart of another embodiment of a method for manufacturing a thermal conductive insulating material according to the present application.
Alternatively, step S120 may include:
s121: mixing aluminum nitride particles and aluminum oxide particles, adding a surfactant and a dispersing agent, uniformly mixing, and heating to 70-90 ℃ to obtain first powder.
In a specific embodiment, aluminum nitride particles and aluminum oxide particles with different particle sizes and morphologies are compounded according to a certain ratio (for example, the mass ratio of the aluminum nitride particles to the aluminum oxide particles can be 1: 2), after uniform mixing and stirring, a mixed solution of a surfactant and a dispersing agent (for example, ethanol) is added, sufficient stirring is carried out to fully wet the aluminum nitride particles and the aluminum oxide particles, and then, continuous stirring and heating to 80 ℃ are carried out to obtain first powder.
S122: and stirring the first powder for 3-5 h, and heating to 120-160 ℃ to obtain second powder.
In one embodiment, the first powder may be stirred for 4 hours, and the temperature is raised to 150 ℃ to obtain the second powder.
S123: removing low molecular substances in the second powder to obtain a first mixture.
The removing of the low molecular substance in the second powder may be vacuum removing of the low molecular substance in the first powder, and simultaneously performing drying treatment to obtain the first mixture. The low molecular weight means unreacted ethanol, water molecules, and the like.
Optionally, when removing low molecules in the first powder in vacuum, the vacuumizing time is 30-60 min, and the stirring speed is 30-50 r/min.
For example, the time period for evacuation may be 30min, 35min, 40min, 45min, 50min, 55min, or 60 min. The stirring speed can be 30r/min, 34r/min, 35r/min, 37r/min, 40r/min, 42r/min, 45r/min, 48r/min or 50 r/min.
Alternatively, step S140 may include:
s141: and (3) acquiring polydimethylsiloxane, hydrogen-containing silicone oil, an inhibitor, a catalyst and an inhibitor, and mixing the polydimethylsiloxane, the hydrogen-containing silicone oil, the inhibitor and the first mixture to obtain a second mixture.
The raw materials for preparing the silica gel matrix comprise: polydimethylsiloxane, hydrogen-containing silicone oil, dimethyl silicone oil, a catalyst and an inhibitor.
In one embodiment, 100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethynl cyclohexanol are put into a kneader or a planetary mixer together, and then the first mixture is added and fully and uniformly stirred in the kneader or the planetary mixer to obtain a second mixture.
Alternatively, step S160 may include:
s161: and adding a catalyst into the second mixture, and performing catalysis and mixing treatment to obtain the heat-conducting insulating material.
In a specific embodiment, the catalyst is added into the second mixture, and after the mixture is stirred by a kneader or a planetary mixer to achieve mixing treatment, the mixture can be further subjected to three-roll grinding and then placed into a vacuum defoaming machine for vacuum defoaming, so as to obtain the heat-conducting insulating material.
Wherein the mass ratio of the polydimethylsiloxane, the hydrogen-containing silicone oil, the dimethyl silicone oil, the catalyst and the inhibitor is 100: 5-20: 5-20: 1-2: 0.1 to 0.2.
For the specific selection and proportion of the raw materials, reference may be made to the description of the above embodiments of the thermal conductive insulating material, and the detailed description of the embodiments is omitted here.
The present application is further described below with reference to specific embodiments:
example 1:
selecting aluminum nitride particles and aluminum oxide particles in a compounding way:
and compounding the aluminum nitride particles and the aluminum oxide particles, uniformly mixing and stirring, adding a mixed solution of 24 parts of a surfactant and 72 parts of ethanol, fully stirring until the aluminum nitride particles and the aluminum oxide particles are wetted, continuously stirring, heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2400 parts of a treated first mixed material.
Putting 100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of the vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to the vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol into a kneader or a planetary stirrer, adding 2400 parts of the first mixture, and fully and uniformly stirring in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the data are shown in Table 1 below:
table 1 table of thermal conductivity data for example 1
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.522 | 2.225 | 6.84 | 20.09 |
| 3.013 | 3.933 | 7.66 | 20.09 |
| 4.493 | 5.573 | 8.06 | 20.09 |
The thermal conductivity coefficient obtained by data fitting calculation is 8.87W/(m.K).
Example 2:
selecting aluminum nitride particles and aluminum oxide particles in a compounding way:
compounding the aluminum nitride particles and the aluminum oxide particles, mixing and stirring uniformly, adding a mixed solution of 26 parts of a surfactant and 78 parts of ethanol, fully stirring until the aluminum nitride particles and the aluminum oxide particles are wetted, continuously stirring, heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2600 parts of the treated first mixed material powder.
Putting 100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol into a kneader or a planetary stirrer together, adding 2600 parts of first mixture, and fully and uniformly stirring in the kneader or the planetary stirrer to obtain a second mixture
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the data are shown in Table 2 below:
table 2 table of thermal conductivity data for example 2
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.394 | 1.927 | 7.24 | 10.04 |
| 2.676 | 3.316 | 8.07 | 10.07 |
| 3.823 | 4.469 | 8.55 | 10.07 |
The coefficient of thermal conductivity was 9.54W/(m.K) by data fitting calculation.
Example 3:
selecting aluminum nitride particles and aluminum oxide particles in a compounding way:
compounding the aluminum nitride particles and the aluminum oxide particles, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the aluminum nitride particles and the aluminum oxide particles are wetted, continuously stirring, heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain 2500 parts of a treated first mixed material.
Putting 100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of the vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to the vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol into a kneader or a planetary stirrer, adding about 2500 parts of the first mixture, and fully and uniformly stirring in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the measured data are shown in Table 3 below:
table 3 table of thermal conductivity data for example 3
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.516 | 2.094 | 7.24 | 40.11 |
| 3.012 | 3.793 | 7.94 | 40.00 |
| 4.445 | 5.295 | 8.39 | 40.02 |
The coefficient of thermal conductivity was 9.15W/(m.K) by data fitting calculation.
Example 4:
selecting aluminum nitride particles and aluminum oxide particles in a compounding way:
compounding the aluminum nitride particles and the aluminum oxide particles, mixing and stirring uniformly, adding a mixed solution of 25 parts of a surfactant and 75 parts of ethanol, fully stirring until the aluminum nitride particles and the aluminum oxide particles are wetted, continuously stirring, heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2400 parts of a treated first mixed material.
Putting 100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of the vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to the vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol into a kneader or a planetary stirrer, adding 2400 parts of the first mixture, and fully and uniformly stirring in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the measured data are shown in Table 4 below:
table 4 table of thermal conductivity data for example 4
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.504 | 2.184 | 6.88 | 40.00 |
| 2.998 | 3.692 | 7.48 | 40.00 |
| 4.455 | 5.371 | 8.49 | 40.01 |
The coefficient of thermal conductivity was 9.66W/(m.K) by data fitting calculation.
Comparative example 1:
and (3) selecting the single spherical alumina particles in a compounding way:
compounding the alumina particles with different particle sizes, mixing and stirring uniformly, adding a mixed solution of 24 parts of surfactant and 72 parts of ethanol, fully stirring until the alumina particles are wetted, continuously stirring and heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2400 parts of a treated first mixed material.
100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of the vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to the vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol are put into a kneader or a planetary stirrer together, and then 2400 parts of the first mixture is added and fully and uniformly stirred in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the measured data are shown in Table 5 below:
TABLE 5 thermal conductivity data Table for comparative example 1
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.505 | 3.321 | 4.60 | 10.02 |
| 2.952 | 5.799 | 5.09 | 9.91 |
| 4.201 | 7.862 | 5.34 | 9.93 |
The coefficient of thermal conductivity is 5.89W/(m.K) through data fitting calculation.
Comparative example 2:
and (3) compounding and selecting single spherical aluminum nitride particles:
compounding the aluminum nitride particles with different particle sizes, uniformly mixing and stirring, adding a mixed solution of 24 parts of surfactant and 72 parts of ethanol, fully stirring until the aluminum nitride particles are wetted, continuously stirring, heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2400 parts of a treated first mixed material.
100 parts of vinyl-terminated polydimethylsiloxane (the mass ratio of the vinyl-terminated polydimethylsiloxane with the viscosity of 100cps to the vinyl-terminated polydimethylsiloxane with the viscosity of 2000cps is 2:1), 6 parts of hydrogen-containing silicone oil (the mass ratio of lateral hydrogen to terminal hydrogen in the hydrogen-containing silicone oil is 2:1), 10 parts of dimethyl silicone oil with the viscosity of 100cps and 0.1 part of ethyne cyclohexanol are put into a kneader or a planetary stirrer together, and then 2400 parts of the first mixture is added and fully and uniformly stirred in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the following data are shown in Table 6 below:
table 6 thermal conductivity data table for comparative example 2
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.499 | 2.014 | 6.68 | 40.00 |
| 2.962 | 3.582 | 7.58 | 40.02 |
| 4.211 | 5.221 | 8.29 | 40.01 |
The coefficient of thermal conductivity was 9.01W/(m.K) by data fitting calculation.
Comparative example 3
Selecting aluminum nitride particles and aluminum oxide particles in a compounding way:
compounding the alumina particles with different particle sizes, mixing and stirring uniformly, adding a mixed solution of 24 parts of surfactant and 72 parts of ethanol, fully stirring until the alumina particles are wetted, continuously stirring and heating to 80 ℃ to obtain first powder, keeping stirring the first powder for 4 hours, heating to 150 ℃ to obtain second powder, and removing low molecules in the second powder in vacuum to obtain about 2400 parts of a treated first mixed material.
100 parts of vinyl-terminated polydimethylsiloxane (100 cps: 2000cps ═ 2:1), 6 parts of hydrogen-containing silicone oil (side hydrogen: end hydrogen ═ 2:1), 10 parts of 100cps dimethylsilicone oil and 0.1 part of inhibitor (ethynl cyclohexanol) are put into a kneader or a planetary stirrer, about 2400 parts of the first mixture is added, and the mixture is fully and uniformly stirred in the kneader or the planetary stirrer to obtain a second mixture.
And adding a catalyst into the second mixture, uniformly stirring, and performing vacuum defoaming to obtain the heat-conducting insulating material.
Adjusting the calendering thickness of a calender to be 1.5mm (film thickness reduction), cold-pressing and molding the heat-conducting insulating material through the calender, vulcanizing the heat-conducting insulating material through hot air in an oven, and cooling to obtain the heat-conducting insulating silica gel gasket with the thickness of 1.5 mm.
The thermal conductivity of the high thermal conductivity silica gel was measured using a Taiwan Ruiki LW-9389 thermal conductivity tester in accordance with ASTM-5470, and the following data are shown in Table 7:
TABLE 7 thermal conductivity data Table for comparative example 3
| Thickness | Imp | K | Press |
| mm | (℃xcm2/W) | W/(mx℃) | (Psi) |
| 1.511 | 2.332 | 5.44 | 40.00 |
| 2.949 | 3.703 | 7.28 | 40.00 |
| 4.367 | 5.417 | 8.39 | 40.01 |
The coefficient of thermal conductivity was 9.23W/(m.K) by data fitting calculation.
The heat-conducting insulating material comprises a silica gel matrix and a filler, wherein the filler accounts for 80-99% of the heat-conducting insulating material by mass; and the aluminum nitride particles and the aluminum oxide particles with higher heat conductivity are compounded in the filler, and the aluminum nitride particles and the aluminum oxide particles with a certain particle size range are selected, so that the particle sizes of the aluminum nitride particles and the aluminum oxide particles reach a certain proportion, and an efficient heat-conducting network is constructed, namely the particle size of the aluminum nitride particles is 50-100 mu m, the particle size of the aluminum oxide particles is 1-30 mu m, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, the heat-conducting insulating material has higher heat conductivity coefficient, and the prepared product has higher heat-conducting property and excellent insulating property.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (11)
1. The heat-conducting insulating material is characterized in that raw materials of the heat-conducting insulating material comprise a silica gel matrix and a filler, and the filler accounts for 80-99% of the heat-conducting insulating material by mass;
the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 microns, the particle size of the aluminum oxide particles is 1-30 microns, 2-5 particle size gradients are formed, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%.
2. The heat-conducting insulating material as claimed in claim 1, wherein the mass ratio of the aluminum nitride particles to the aluminum oxide particles is 1: 2-1: 1;
the aluminum nitride particles have 1-3 particle size gradients in a particle size range of 50-100 μm.
3. The thermally conductive insulating material of claim 1, wherein the alumina particles are at least one of spherical alumina particles, spheroidal alumina particles, alpha-alumina particles;
the aluminum nitride particles are at least one of spherical aluminum nitride particles or granular aluminum nitride particles.
4. The thermally conductive insulating material according to claim 3,
the aluminum nitride particles are spherical aluminum oxide particles, and the particle size is at least one of 50 μm, 60 μm, 70 μm, 80 μm, 90 μm and 100 μm;
the aluminum oxide particles are spherical aluminum nitride particles, and the particle size of the aluminum oxide particles is at least one of 1 μm, 2 μm, 5 μm, 10 μm, 20 μm and 30 μm.
5. The thermally conductive insulating material of claim 1, wherein the filler further comprises: surfactants and dispersants;
the mass ratio of the aluminum oxide particles to the aluminum nitride particles to the surfactant to the dispersant is 100-200: 80-160: 1-5: 5 to 10.
6. The thermally conductive insulating material of claim 5, wherein the silica gel matrix comprises: polydimethylsiloxane, hydrogen-containing silicone oil, dimethyl silicone oil, a catalyst and an inhibitor;
wherein the mass ratio of the polydimethylsiloxane, the hydrogen-containing silicone oil, the dimethyl silicone oil, the catalyst and the inhibitor is 100: 5-20: 5-20: 1-2: 0.1 to 0.2.
7. The thermally conductive insulating material according to claim 6,
the surfactant is at least one of hexamethyldisilazane, octyltrimethoxysilane, decyltrimethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethylsilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy) and propyltrimethoxysilane;
the inhibitor is at least one of ethynl cyclohexanol, methyl butynol, phenyl butynol, vinyl ring body, diallyl maleate, diallyl fumarate and silanized alkynol;
the hydrogen-containing silicone oil is side chain hydrogen-containing silicone oil or end side hydrogen-containing silicone oil, or at least two of the side chain hydrogen-containing silicone oil, the end hydrogen-containing silicone oil and the end side hydrogen-containing silicone oil, and the hydrogen content of the hydrogen-containing silicone oil is 0.1-0.2%;
the catalyst is at least one of chloroplatinic acid isopropanol solution, platinum complex and platinum catalyst.
8. A heat-conducting insulating silica gel gasket is characterized in that the heat-conducting insulating silica gel gasket is made of the heat-conducting insulating material according to any one of claims 1 to 7.
9. The preparation method of the heat-conducting insulating material is characterized by comprising the following steps of:
obtaining a filler, and carrying out first treatment on the filler to obtain a first mixture;
obtaining a silica gel matrix, and mixing the first mixture with the silica gel matrix to obtain a second mixture;
carrying out second treatment on the second mixture to obtain the heat-conducting insulating material;
the raw materials of the heat-conducting insulating material comprise 80-99% of filler by mass, the filler comprises aluminum nitride particles and aluminum oxide particles, the particle size of the aluminum nitride particles is 50-100 μm, the particle size of the aluminum oxide particles is 1-30 μm and has 2-5 particle size gradients, and the ratio of the average particle size of the aluminum nitride particles to the average particle size of the aluminum oxide particles is less than or equal to 5: 1, in the filler, the mass percentage of the aluminum nitride particles is 30-60%.
10. The method for preparing a heat-conducting insulating material according to claim 9, wherein the obtaining the filler and performing a first treatment on the filler to obtain a first mixture material comprises:
mixing the aluminum nitride particles and the aluminum oxide particles, adding a surfactant and a dispersant, uniformly mixing, and heating to 70-90 ℃ to obtain first powder;
stirring the first powder for 3-5 hours, and heating to 120-160 ℃ to obtain second powder;
and removing low molecular substances in the second powder to obtain the first mixture.
11. The method for preparing a heat conductive insulating material according to claim 10, wherein the obtaining a silica gel matrix and mixing the first mixture with the silica gel matrix to obtain a second mixture comprises:
acquiring polydimethylsiloxane, hydrogen-containing silicone oil, simethicone, a catalyst and an inhibitor, and mixing the polydimethylsiloxane, the hydrogen-containing silicone oil, the inhibitor and the first mixture to obtain a second mixture;
the second treatment is carried out on the second mixture to obtain the heat-conducting and insulating material, and the method comprises the following steps:
adding the catalyst into the second mixture, and performing catalysis and mixing treatment to obtain the heat-conducting insulating material;
wherein the mass ratio of the polydimethylsiloxane, the hydrogen-containing silicone oil, the dimethyl silicone oil, the catalyst and the inhibitor is 100: 5-20: 5-20: 1-2: 0.1 to 0.2.
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| JPH1149958A (en) * | 1997-08-06 | 1999-02-23 | Shin Etsu Chem Co Ltd | Heat conductive silicone composition |
| CN103146198A (en) * | 2013-03-12 | 2013-06-12 | 深圳市博恩实业有限公司 | Heat conducting composite material and heat conducting composite sheet prepared by applying same |
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| CN110684354A (en) * | 2019-06-24 | 2020-01-14 | 上海航天设备制造总厂有限公司 | Insulating and heat-conducting silicone grease composite material and preparation method thereof |
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| CN103146198A (en) * | 2013-03-12 | 2013-06-12 | 深圳市博恩实业有限公司 | Heat conducting composite material and heat conducting composite sheet prepared by applying same |
| CN109312216A (en) * | 2016-06-24 | 2019-02-05 | 日本山村硝子株式会社 | High-heat-conductive composite material |
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