CN115651411A - High-flexibility low-exudation heat-conducting gel and preparation method thereof - Google Patents
High-flexibility low-exudation heat-conducting gel and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000001879 gelation Methods 0.000 title description 2
- 229920002545 silicone oil Polymers 0.000 claims abstract description 67
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052582 BN Inorganic materials 0.000 claims abstract description 39
- 239000000945 filler Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 33
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 30
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000003490 calendering Methods 0.000 claims abstract description 16
- 239000004970 Chain extender Substances 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 229930006000 Sucrose Natural products 0.000 claims abstract description 10
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 10
- 229960004793 sucrose Drugs 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000010008 shearing Methods 0.000 claims abstract description 8
- 238000009736 wetting Methods 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 125000000524 functional group Chemical group 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 34
- 239000001257 hydrogen Substances 0.000 claims description 34
- 150000002431 hydrogen Chemical class 0.000 claims description 23
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000347 magnesium hydroxide Substances 0.000 claims description 11
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003112 inhibitor Substances 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 6
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical group C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-UHFFFAOYSA-N 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical group 0.000 claims description 3
- 229910052755 nonmetal Inorganic materials 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 239000000499 gel Substances 0.000 abstract description 79
- 239000003921 oil Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 238000009413 insulation Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
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- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052990 silicon hydride Inorganic materials 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a high-flexibility low-exudation heat-conducting gel and a preparation method thereof, relating to the technical field of heat-conducting gels, wherein the preparation method of the heat-conducting gel comprises the following steps: s1, performing functional group modification treatment on boron nitride powder by adopting a method of modifying boron nitride by cane sugar-assisted ball milling to obtain boron nitride powder containing hydroxyl functional groups; s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, and uniformly mixing for defoaming; s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 1-6 hours; step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, calendering by a calender, and finally curing at high temperature in an oven at 120-150 ℃ to obtain the cured heat-conducting gel.
Description
Technical Field
The invention relates to the technical field of heat-conducting gel, in particular to high-flexibility low-exudation heat-conducting gel and a preparation method thereof.
Background
More heat energy is generated during the operation of the electronic device, and the continuous increase of the heat energy causes the temperature rise of the electronic equipment and the increase of the thermal stress, which seriously affects the reliability and the service life of the electronic device, so that the heat energy needs to be dissipated by using a thermal interface material. Thermal interface materials are one of the common heat dissipation methods, and are commonly used for IC packaging and electronic heat dissipation. The heat dissipation is a durable topic, the normal operation of the electronic equipment cannot be separated from the heat conduction function of various heat conduction materials, especially, the requirements on the heat conduction materials are continuously improved along with the development of high performance and light weight of intelligent equipment, and heat conduction products are also rapidly upgraded and updated.
The heat conducting gasket is a common thermal interface material at present, but the heat conducting gasket is difficult to cover an uneven place and is not tightly attached to an electronic device, so that the heat radiating efficiency is low.
The heat-conducting gel is a gel-like heat-conducting interface material which is newly developed in recent years and is prepared by stirring, mixing and packaging a high-heat-conducting filler and a high-molecular matrix, is a preformed soft material with low hardness, is prepared by mixing and mixing a plurality of heat-conducting powder bodies and heat-conducting silica gel after being completely cured, and has the following characteristics: the heat-conducting gel is packaged by a needle cylinder, and automatic production can be realized by combining an automatic dispensing technology; the heat-conducting gel is not dry for a long time, can be infinitely compressed, has long service life, good surface affinity, good flexibility, small hardness and no internal stress on equipment after being used, and can be molded into any shape; compared with a heat-conducting gasket, the heat-conducting gel can be well attached to most materials, is self-adhesive, does not need an adhesive and reduces heat resistance of heat transfer.
The existing heat-conducting gel has the problem of high silicone oil leaching rate, the prepared heat-conducting silicone gel is in a solid-liquid coexisting state after vulcanization, and the crosslinking density is low, so that the prepared heat-conducting silicone gel is easy to have the problem of oil leaching, thereby polluting electronic devices and reducing the reliability of long-time work of the electronic devices.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the high-flexibility low-exudation heat-conducting gel and the preparation method thereof, and solves the problems of low heat conductivity and high oil seepage rate of the traditional high-flexibility low-exudation heat-conducting gel.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a highly flexible, low exuding thermally conductive gel comprising, by mass: 50-70 parts of heat-conducting filler, 10-25 parts of vinyl silicone oil, 1-2 parts of alkoxy silicone oil modifier, 3-5 parts of lateral hydrogen silicone oil cross-linking agent, 0.8-2 parts of terminal hydrogen silicone oil chain extender, 0.05-0.2 part of catalyst and 0.04-0.1 part of inhibitor, wherein the heat-conducting filler is metal oxide powder and nonmetal powder with different particle sizes and comprises the following components in parts by mass: 4 parts of magnesium hydroxide powder, 4 parts of boron nitride powder and 1 part of silicon carbide powder.
Preferably, the thermally conductive gel with high flexibility and low exudation of claim 1, wherein: the particle size range of the magnesium hydroxide is 5-15 mu m, the particle size range of the boron nitride is 5-20 mu m, and the particle size of the silicon carbide powder is 0.5-5 mu m.
Preferably, the preferred proportion of the heat conducting gel is as follows: 65 parts of heat-conducting filler, 15 parts of vinyl silicone oil, 1.2 parts of alkoxy silicone oil, 3.2 parts of side hydrogen silicone oil, 1.0 part of end hydrogen silicone oil and 0.1 part of catalyst, wherein the catalyst is CAT-PL-56 type catalyst produced by shin-Yuan corporation, and the inhibitor is 2-phenyl-3-butyn-2-ol.
Preferably, the ratio of silicon hydride to vinyl in the heat-conducting gel is 1.5-3.2.
Preferably, the viscosity of the vinyl silicone oil at 25 ℃ is 200-450mpa.s, and the vinyl content is 0.28-3.0 mmol/g; the viscosity of the lateral hydrogen silicone oil at 25 ℃ is 20-100mpa.s, and the hydrogen base content is 1.0-2.5 mmol/g; the viscosity of the hydrogen-terminated silicone oil at 25 ℃ is 4-20mpa.s, and the hydrogen content is 0.2-0.33 mmol/g.
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, modifying a heat-conducting filler: performing functional group modification treatment on the boron nitride powder by adopting a method of modifying boron nitride by cane sugar-assisted ball milling to obtain boron nitride powder containing hydroxyl functional groups;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, mixing uniformly and defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 1-6 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, then calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at high temperature in a drying oven at 120-150 ℃ to obtain the cured heat-conducting gel.
Preferably, the modification of the boron nitride comprises the following steps: firstly, weighing boron nitride powder, putting the boron nitride powder into vacuum drying performance, and carrying out vacuum drying for 12 hours at 80 ℃ for later use; then weighing the dried boron nitride powder and sucrose, uniformly mixing according to the proportion of 1; and (4) removing the cane sugar after ball milling to obtain modified or post-processed boron nitride powder.
The invention principle is as follows: the heat conducting filler has excellent heat conducting performance, is used in heat conducting gel, has good matching performance with silicon oil, has a similar thermal expansion coefficient with semiconductor silicon and silicon, has good interface compatibility, can improve the electric conduction and insulation performance, increases the heat conduction of the heat conducting gel through different combinations of fillers, increases hydroxyl functional groups by modified boron nitride, improves the dispersibility and cohesiveness of the boron nitride in the gel, forms a filler framework by the boron nitride and magnesium hydroxide, fills the framework with silicon carbide powder to form a compact structure, wherein the magnesium hydroxide generates crystal water after absorbing heat, increases the heat conducting performance of the heat conducting gel, controls the adding amount of the fillers to reduce the oil permeability of the heat conducting gel by controlling the ratio of silicon hydrogen to vinyl, and obtains the heat conducting gel with good super electric insulation performance and working temperature of-15-250 ℃.
(III) advantageous effects
The invention provides a high-flexibility low-exudation heat-conducting gel and a preparation method thereof, and the gel has the following beneficial effects: according to the high-flexibility low-seepage heat-conducting gel, the heat conduction of the heat-conducting gel is increased through fillers in different combinations, the modified boron nitride increases hydroxyl functional groups, the dispersibility and the cohesiveness of the boron nitride in the gel are improved, the boron nitride and magnesium hydroxide form a filler framework, silicon carbide powder fills the framework to form a compact structure, the magnesium hydroxide generates crystal water after absorbing heat, the heat conduction performance of the heat-conducting gel is improved, the oil seepage rate of the heat-conducting gel is reduced by controlling the ratio of silicon hydrogen to vinyl and controlling the addition amount of the fillers, and the heat-conducting gel with good super-electric insulation property and working temperature of-15-250 ℃ is obtained.
Detailed Description
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.
Example 1
The invention provides the following technical scheme: a highly flexible, low exuding thermally conductive gel comprising, by mass: 50-70 parts of heat-conducting filler, 10-25 parts of vinyl silicone oil, 1-2 parts of alkoxy silicone oil modifier, 3-5 parts of lateral hydrogen silicone oil cross-linking agent, 0.8-2 parts of terminal hydrogen silicone oil chain extender, 0.05-0.2 part of catalyst and 0.04-0.1 part of inhibitor, wherein the heat-conducting filler is metal oxide powder and nonmetal powder with different particle sizes and comprises the following components in parts by mass: 4 parts of magnesium hydroxide powder, 4 parts of boron nitride powder and 1 part of silicon carbide powder.
Further, a thermally conductive gel with high flexibility and low exudation according to claim 1, wherein: the particle size range of the magnesium hydroxide is 5-15 mu m, the particle size range of the boron nitride is 5-20 mu m, and the particle size of the silicon carbide powder is 0.5-5 mu m.
Further, the preferred proportion of the heat conducting gel is as follows: 65 parts of heat-conducting filler, 15 parts of vinyl silicone oil, 1.2 parts of alkoxy silicone oil, 3.2 parts of side hydrogen silicone oil, 1.0 part of end hydrogen silicone oil and 0.1 part of catalyst, wherein the catalyst is CAT-PL-56 type catalyst produced by shin-Yuan corporation, and the inhibitor is 2-phenyl-3-butyn-2-ol.
Further, the ratio of silicon hydrogen to vinyl in the heat conducting gel is 1.5-3.2.
Further, the viscosity of the vinyl silicone oil at 25 ℃ is 200-450mpa.s, and the vinyl content is 0.28-3.0 mmol/g; the viscosity of the lateral hydrogen silicone oil at 25 ℃ is 20-100mpa.s, and the hydrogen base content is 1.0-2.5 mmol/g; the viscosity of the hydrogen-terminated silicone oil at 25 ℃ is 4-20mpa.s, and the hydrogen content is 0.2-0.33 mmol/g.
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, modifying a heat-conducting filler: performing functional group modification treatment on the boron nitride powder by adopting a method of modifying boron nitride by cane sugar-assisted ball milling to obtain boron nitride powder containing hydroxyl functional groups;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, and uniformly mixing for defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 1-6 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, then calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at high temperature in a drying oven at 120-150 ℃ to obtain the cured heat-conducting gel.
Further, the modification of the boron nitride comprises the following steps: firstly, weighing boron nitride powder, putting the boron nitride powder into vacuum drying performance, and carrying out vacuum drying for 12 hours at 80 ℃ for later use; then weighing the dried boron nitride powder and sucrose, uniformly mixing according to the proportion of 1; and (4) removing the cane sugar after ball milling to obtain modified or post-processed boron nitride powder.
Example 2
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, weighing 50 parts of heat-conducting filler, 10 parts of vinyl silicone oil, 1 part of alkoxy silicone oil modifier, 3 parts of lateral hydrogen silicone oil cross-linking agent, 0.8 part of terminal hydrogen silicone oil chain extender, 0.05 part of catalyst and 0.05 part of inhibitor;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, and uniformly mixing for defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 5 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at a high temperature in an oven at 140 ℃ to obtain the cured heat-conducting gel.
Example 3
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, weighing 60 parts of heat-conducting filler, 18 parts of vinyl silicone oil, 1.5 parts of alkoxy silicone oil modifier, 5 parts of lateral hydrogen silicone oil cross-linking agent, 1.0 part of terminal hydrogen silicone oil chain extender, 0.1 part of catalyst and 0.1 part of inhibitor;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, mixing uniformly and defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 5 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at a high temperature in an oven at 140 ℃ to obtain the cured heat-conducting gel.
Example 4
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, weighing 70 parts of heat-conducting filler, 25 parts of vinyl silicone oil, 1.5 parts of alkoxy silicone oil modifier, 4 parts of lateral hydrogen silicone oil cross-linking agent, 1.5 parts of terminal hydrogen silicone oil chain extender, 0.15 part of catalyst and 0.08 part of inhibitor;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, and uniformly mixing for defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 5 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, then calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at a high temperature in a drying oven at 140 ℃ to obtain the cured heat-conducting gel.
Example 5
In order to achieve the purpose, the invention provides the following technical scheme: a high-flexibility low-exudation heat-conducting gel, which is prepared by the following steps:
s1, weighing 70 parts of heat-conducting filler, 22 parts of vinyl silicone oil, 1.2 parts of alkoxy silicone oil modifier, 4 parts of lateral hydrogen silicone oil cross-linking agent, 1.2 parts of terminal hydrogen silicone oil chain extender, 0.15 part of catalyst and 0.08 part of inhibitor;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, mixing uniformly and defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 5 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, calendering the crosslinked gel by a calender, and finally curing the crosslinked gel at a high temperature in an oven at 140 ℃ to obtain the cured heat-conducting gel.
Examples of the experiments
The heat conductivity coefficient, the thermal resistance, the rheological property, the reliability and the oil permeability of the heat-conducting gel provided by the embodiment 2-4 are verified through experimental examples, and the heat conductivity is tested by a laser heat conductivity instrument; the rheological properties are characterized by a rheometer; the reliability is tested by a thermogravimetric analyzer; the test mode of the oil permeability is as follows: attaching oil absorption filter paper to the upper surface and the lower surface of the heat-conducting rubber mat, placing the heat-conducting rubber mat into a fixture, enabling the pressure of the fixture to be 50%, placing the heat-conducting rubber mat into a drying oven at the temperature of 100 ℃, heating the heat-conducting rubber mat for 24 hours, then adding and opening the fixture, and testing the weight gain of the filter paper to determine the oil seepage weight, wherein the following table is obtained through testing of the embodiments 2-4:
and (4) conclusion: the heat-conducting gel provided by the invention has good heat conductivity, low oil permeability and good rheological property.
In summary, the high-flexibility low-exudation heat-conducting gel and the preparation method thereof have the advantages that the heat-conducting filler has excellent heat-conducting property, is used in the heat-conducting gel, has good matching property with silicone oil, has similar thermal expansion coefficient with semiconductor silicon and silicon, has good interface compatibility, can improve the electric conduction and insulation property, increases the heat conduction of the heat-conducting gel through different combinations of fillers, increases hydroxyl functional groups through modified boron nitride, improves the dispersibility and cohesiveness of boron nitride in the gel, forms a filler framework through boron nitride and magnesium hydroxide, fills the framework through silicon carbide powder, forms a compact structure, generates crystal water after the magnesium hydroxide absorbs heat, increases the heat-conducting property of the heat-conducting gel, reduces the oil-exudation rate of the heat-conducting gel through controlling the ratio of silicon hydrogen and vinyl, controls the addition amount of the filler, obtains the heat-conducting gel with good super-electric insulation property and working temperature of-15-250 ℃, and solves the problems of low heat conduction rate and high oil exudation rate of the existing heat-conducting gel.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A highly flexible, low exudation thermally conductive gel, comprising, by mass: 50-70 parts of heat-conducting filler, 10-25 parts of vinyl silicone oil, 1-2 parts of alkoxy silicone oil modifier, 3-5 parts of lateral hydrogen silicone oil cross-linking agent, 0.8-2 parts of terminal hydrogen silicone oil chain extender, 0.05-0.2 part of catalyst and 0.04-0.1 part of inhibitor, wherein the heat-conducting filler is metal oxide powder and nonmetal powder with different particle sizes and comprises the following components in parts by mass: 4 parts of magnesium hydroxide powder, 4 parts of boron nitride powder and 1 part of silicon carbide powder.
2. The thermally conductive gel with high flexibility and low exudation of claim 1, wherein: the particle size range of the magnesium hydroxide is 5-15 mu m, the particle size range of the boron nitride is 5-20 mu m, and the particle size of the silicon carbide powder is 0.5-5 mu m.
3. The thermally conductive gel with high flexibility and low exudation of claim 1, wherein: the preferable proportion of the heat-conducting gel is as follows: 65 parts of heat-conducting filler, 15 parts of vinyl silicone oil, 1.2 parts of alkoxy silicone oil, 3.2 parts of side hydrogen silicone oil, 1.0 part of end hydrogen silicone oil and 0.1 part of catalyst, wherein the catalyst is CAT-PL-56 type catalyst produced by shin-Yuan corporation, and the inhibitor is 2-phenyl-3-butyn-2-ol.
4. The high flexibility low exudation thermally conductive gel of claim 1, wherein: the ratio of silicon hydrogen to vinyl in the heat-conducting gel is 1.5-3.2.
5. The high flexibility low exudation thermally conductive gel of claim 1, wherein: the viscosity of the vinyl silicone oil at 25 ℃ is 200-450mpa.s, and the vinyl content is 0.28-3.0 mmol/g; the viscosity of the lateral hydrogen silicone oil at 25 ℃ is 20-100mpa.s, and the hydrogen base content is 1.0-2.5 mmol/g; the viscosity of the hydrogen-terminated silicone oil at 25 ℃ is 4-20mpa.s, and the hydrogen content is 0.2-0.33 mmol/g.
6. The method for preparing a thermally conductive gel with high flexibility and low exudation according to any one of claims 1 to 5, wherein: the preparation method of the heat-conducting gel comprises the following steps:
s1, modifying a heat-conducting filler: performing functional group modification treatment on the boron nitride powder by adopting a method of modifying boron nitride by cane sugar-assisted ball milling to obtain boron nitride powder containing hydroxyl functional groups;
s2, adding the heat-conducting filler into the vinyl silicone oil according to a proportion, adding absolute ethyl alcohol for wetting, shearing and dispersing the crystal form, adding the alkoxy silicone oil modifier, mixing uniformly and defoaming;
s3, adding an auxiliary cross-linking agent and a chain extender, uniformly stirring, adding a catalyst, stirring for 30min, drying, and carrying out cross-linking reaction for 1-6 hours under the normal pressure or vacuum condition;
step S4, calendering and curing: and (3) reducing the temperature of the crosslinked gel to 30 ℃, calendering by a calender, and finally curing at high temperature in an oven at 120-150 ℃ to obtain the cured heat-conducting gel.
7. The preparation method of the high-flexibility low-exudation heat-conducting gel according to claim 5, wherein the modification of the boron nitride comprises the following steps: firstly, weighing boron nitride powder, putting the boron nitride powder into vacuum drying performance, and carrying out vacuum drying for 12 hours at 80 ℃ for later use; then weighing the dried boron nitride powder and sucrose, uniformly mixing according to the proportion of 1; and (4) removing the cane sugar after ball milling to obtain modified or post-processed boron nitride powder.
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CN116426172A (en) * | 2023-04-12 | 2023-07-14 | 广东吉美帮新材料有限公司 | Corrosion-resistant acid-alkali-resistant water-based rubber coating and preparation method thereof |
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CN113429796A (en) * | 2021-07-27 | 2021-09-24 | 湖南创瑾技术研究院有限公司 | Single-component high-thermal-conductivity silicone gel and preparation method thereof |
CN113817178A (en) * | 2021-10-18 | 2021-12-21 | 深圳市德镒盟电子有限公司 | Low-oil-permeability high-heat-conductivity heat-conducting gel and preparation method thereof |
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CN113429796A (en) * | 2021-07-27 | 2021-09-24 | 湖南创瑾技术研究院有限公司 | Single-component high-thermal-conductivity silicone gel and preparation method thereof |
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CN116426172A (en) * | 2023-04-12 | 2023-07-14 | 广东吉美帮新材料有限公司 | Corrosion-resistant acid-alkali-resistant water-based rubber coating and preparation method thereof |
CN116426172B (en) * | 2023-04-12 | 2024-01-12 | 广东吉美帮新材料有限公司 | Corrosion-resistant acid-alkali-resistant water-based rubber coating and preparation method thereof |
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