CN115678286A - Easily-filled and easily-repaired heat-conducting gel and preparation method thereof - Google Patents
Easily-filled and easily-repaired heat-conducting gel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heat-conducting gel easy to fill and repair and a preparation method thereof. Comprises the following components: 100 parts of component A, 1-15 parts of component B, 0.01-0.15 part of catalyst C, 400-3500 parts of heat conducting filler D and component E, wherein the component A is alkylene polysiloxane with the viscosity of 10-10000mPa & s at normal temperature; the component B is straight-chain hydrogen-containing polysiloxane, each molecule contains 2-4 Si-H bonds, at least 2 Si-H bonds are on a side chain, and the viscosity is 1-1000mPa & s at normal temperature. The heat-conducting gel obtained by mixing and stirring the components has high heat conductivity, fluidity and adhesiveness, has strong filling capacity to gaps, can be fully contacted no matter how irregular the surface of the heater is, and has good heat-conducting effect. Under given pressure, the heat-conducting gel shows stress relaxation, and can be peeled off in practical application, so that equipment maintenance is facilitated.
Description
Technical Field
The invention relates to the technical field of thermal gel, in particular to a heat-conducting gel easy to fill and repair and a manufacturing method thereof.
Background
Circuit designs for electronic devices such as televisions, radios, computers, medical devices, business machines, communication devices, etc. are now becoming more complex, requiring the use of thousands of transistors for integrated circuits in, for example, electrical appliances. Although the design of circuits is more and more complex, electronic devices are shrinking, and manufacturers are increasingly able to design small electronic components, placing more functional components in a smaller area. In recent years, electronic devices have become smaller and the arrangement of PCB boards has become denser. Heat dissipation in electronic devices presents a significant challenge to designers and manufacturers who attempt to use various approaches for thermal management. Thermal management has evolved to address the increased temperatures that result from the increased processing speeds and power of these electronic devices. New generations of electronic devices compress components into smaller spaces, and thermal management becomes very important.
Thermal management is most fundamentally the selection of a suitable thermal interface material for the device. New heat management designs have invented methods to better dissipate heat and improve the operating efficiency of the equipment. Other thermal management techniques use the concept of a cold plate, or heat sink, that is placed near the heat generating source for heat dissipation purposes. The heat sink should be a dedicated metal heat sink or simply a device chassis or circuit board. To improve heat dissipation efficiency, a thermally conductive, insulating material is often placed between the heat sink and the heat generating source to fill irregular voids and prevent air from entering (as air is a poor conductor of heat). Originally, for this purpose, silicone grease or silica gel filled with a heat conductive filler such as alumina was used as this heat conductive material. These materials are semi-solid or solid at room temperature, but liquefy, flow or soften at high temperatures to less well fill irregular gaps. The aforementioned grease or wax cannot ensure a stable form at normal temperature and may contaminate other devices during use. Later, the materials are manufactured on the film, the manual operation is easy, but the heat dissipation side is stuck with the film, and air bubbles are easily generated when the two sides are stuck. In addition, such operations are entirely manual, which increases labor costs.
Yet another approach is to provide a cured silicone gasket material that is cured into a sheet by dispersing one or more thermally conductive fillers into the silicone. The matrix resin may be silicone, polyurethane, thermoset rubber or other elastomers, and the thermally conductive material may be alumina, aluminum nitride, magnesium oxide, boron nitride, and the like.
In some fields, a fastener such as a spring is required, and the clamp provides enough force to ensure that the heat-conducting gasket is firmly attached to the heat sink, so that a good heat dissipation effect is achieved. This significantly limits the use of thermal pads in electronic devices. In addition, the heat conducting gasket can only be applied to the surface-flattened heat radiating fins and heaters, and the application range of the heat conducting gasket is limited.
Disclosure of Invention
The invention aims to provide a heat-conducting gel easy to fill and repair and a manufacturing method thereof, and aims to solve the problem that a heat-conducting gasket in the prior art can only be applied to a surface-flattened heat radiating fin and a heater and cannot be applied to an irregular structure.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a heat-conducting gel easy to fill and repair, which comprises the following components: 100 parts of component A, 1-15 parts of component B, 0.01-0.15 part of catalyst C, 400-3500 parts of heat conducting filler D and component E, wherein the component A is alkylene polysiloxane with the viscosity of 10-10000mPa & s at normal temperature; the component B is straight-chain hydrogenpolysiloxane, each molecule contains 2-4 Si-H bonds and at least 2 Si-H bonds on a side chain, the viscosity is 1-1000 mPa.s at normal temperature, and the molecular formula of the component E is YnSi (OR) 4-n Wherein Y is an alkyl group of 6 to 18 carbon atoms, R is an alkyl group of 1 to 5 carbon atoms, and n represents an integer of 1 to 2, and said component E is a surface treating agent for component D in an amount of 0.2 to 2% based on D.
Further, the component A is composed of one or more olefin-based polysiloxanes, and the molecular structure of the component A is represented as:
wherein R is 1 Represents a monovalent hydrocarbon radical without labile aliphatic groups, R 2 Is a hydrocarbon radical, R 3 Is alkylene, a represents an integer of 0 to 2, P represents an integer of 1 to 50, and R is 3 Comprises ethenyl, propenyl, butenyl, hexenyl, and also comprises methyl, ethyl, propyl, and aromatic groups.
Further, the catalyst comprises one of platinum catalyst, rhodium catalyst and palladium catalyst, the platinum catalyst comprises platinum fine powder, hydrogen chloride platinic acid, alcohol diluted hydrogen chloride platinic acid, platinum vinyl siloxane coordination compound and platinum carbonate complex, wherein the platinum catalyst is preferably platinum vinyl siloxane coordination compound.
Further, the component D heat conductive filler includes one or more of powder or fiber of metal, metal oxide, metal nitride, metal hydroxide, metal carbide, metal silicide, carbon fiber, soft magnetic alloy and ferrite.
Further, the component D is preferably a metal oxide, a metal nitride, or a carbon fiber.
Further, the component D heat-conducting filler comprises D1, D2, D3 and D4, wherein D1 is flaky boron nitride powder with the average particle size of 0.1-30 microns, D2 is regular boron nitride powder with the average particle size of 0.1-50 microns, D3 is spherical alumina powder with the average particle size of 0.01-50 microns, and D4 is spherical graphite with the average particle size of 0.01-50 microns.
Further, the thermally conductive filler of component D preferably has an average particle diameter of 0.01 to 50 μm.
Further, reaction inhibitors are included for extending the shelf life thereof, including ethynylcyclohexanol, amine groups, carboxylate groups, phosphite group inhibitors.
Further, it is characterized by comprising the following steps: mixing the component D and the component E, carrying out surface treatment on the component D, then pouring the components A and B and the catalyst C, and stirring.
Further, the method is characterized by comprising the following steps: mixing the components A, D and E, mixing the component B and the catalyst C after the surface treatment of the component D is finished, and stirring.
Further, the mixing stirrer used for stirring needs to have a vacuumizing function, the vacuum degree can reach 0.1MPa, and the mixing stirrer comprises a single-blade stirrer, a double-blade stirrer and a kneader.
The invention has the beneficial effects that:
(1) The heat conducting gel is placed between the electronic equipment heater and the heat dissipation unit such as a radiator and a circuit board, and plays a role in conducting heat and cooling the heater. The heat conducting gel can be used on horizontal surfaces and vertical surfaces by controlling the rheological property, and can permeate into the microstructure of a heater to play a good heat conducting role. The heat dissipation structure containing the heat conduction gel can well dissipate heat, and the stability and reliability of the heat dissipation structure in the use process are improved.
(2) The heat-conducting gel has high heat conductivity, fluidity and adhesiveness, and has strong filling capacity to gaps, so the heat-conducting gel can be fully contacted no matter how irregular the surface of the heater is, and a good heat-conducting effect is achieved.
(3) The thermally conductive gel may be applied in an uncured state or in a cured state. The viscosity of the thermally conductive gel is 10-500 pas, preferably 50-400 pas, when uncured at 25 ℃.
(4) The heat-conducting gel has high filling property on the heat-conducting filler and stable performance, and the heat-conducting coefficient of the heat-conducting gel can reach 3-7W/mK.
(5) The polysiloxanes of the present invention contain reactive groups which inhibit thickness when uncured, and also alkyl alcohol or ether groups. In addition to this, it has a function of surface-treating the heat conductive powder, for which reason the thickness and oil bleeding of the heat conductive gel are suppressed while the operability is not affected.
Detailed Description
The heat-conducting gel can be made into a single-component package at the curing temperature of 70-130 ℃. In order to improve the shelf life and operability of the thermally conductive gel, a microencapsulated platinum catalyst may be dispersed in the thermally conductive gel.
When cured at room temperature or below 50 ℃, the thermally conductive gel may be packaged in a single component or in multiple components. After mixing the multi-component thermally conductive gel, it can be cured for 1 hour or even several days at room temperature or below 50 ℃.
The component B is used as a cross-linking agent and is gradually cross-linked into a gel state in the formula of the heat-conducting gel, so that the heat-conducting gel has excellent strippability and elasticity, and is convenient for secondary maintenance of electronic equipment.
Component E contains an alkyl group of 6 or more carbons, preferably 6 to 20 carbon atoms, per molecule, and if the alkyl group is less than 6 carbon atoms, the viscosity of the thermally conductive gel will increase, affecting the fluidity of the thermally conductive gel and the filling property to the gaps. If the carbon atom of the alkyl group is more than 20, the compatibility between the component E and the component A is poor, and it is difficult to carry out industrial production.
Embodiments of the present invention are described in further detail below by way of examples, but the embodiments of the present invention are not limited thereto.
The raw materials used in the examples were as follows:
a-1: dimethylvinylsiloxane-terminated dimethylpolysiloxane having a viscosity of 400mPa.s and a vinyl content of 0.43%.
B-1: trimethylsiloxane terminated methyl hydrosiloxane and dimethylsiloxane copolymers containing two pendant hydrogens per molecule. Viscosity was 20mPa.s, and Si-H content was 0.1%.
NonB-2: the methylhydrogensiloxane and dimethylsiloxane copolymer was endcapped with trimethylsiloxane, containing 5 pendant hydrogens per molecule. Viscosity was 5mPa.s, and the Si-H content was 0.75%.
NonB-3: the dimethylsiloxane is endcapped with a dimethylsiloxane containing two terminal hydrogen groups per molecule and no pendant hydrogen. Viscosity was 10mPa.s, and Si-H content was 0.15%.
C-1: is a complex of platinum and 1, 3-divinyl-1, 3-tetramethyldisiloxane.
Inhibitor (B): ethynylcyclohexanol, concentration 0.6%.
D-1, aluminum oxide powder with the grain size of 2.5 microns.
D-2, aluminum oxide powder with the particle size of 5 microns.
D-3, spherical aluminum oxide powder with the particle size of 50 microns.
E: dodecyl trimethoxy silane.
Example 1
100 parts of A-1, 250 parts of D-1, 280 parts of D-2, 850 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to normal temperature, and 8 parts of B-1 and 0.12 part of C-1 are added after cooling and then mixed and stirred.
Example 2
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 12 parts of B-1 and 0.12 part of C-1 are added for mixing and stirring.
Example 3
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to normal temperature, and 8 parts of B-1, 3.5 parts of NonB-3 and 0.12 part of C-1 are added after cooling for mixing and stirring.
Example 4
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 6 parts of B-1, 5 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Example 5
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 4 parts of B-1, 6 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Example 6
100 parts of A-1, 250 parts of D-1, 280 parts of D-2, 850 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 7 parts of B-1, 0.13 part of NonB-2 and 0.12 part of C-1 are added for mixing and stirring.
Comparative example 1
100 parts of A-1, 250 parts of D-1, 280 parts of D-2, 850 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to normal temperature, and after cooling, 7 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Comparative example 2
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to normal temperature, and then 10 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Comparative example 3
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and then mixed and stirred with 12.5 parts of NonB-3 and 0.12 part of C-1 after being cooled.
Comparative example 4
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 7 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Comparative example 5
100 parts of A-1, 260 parts of D-1, 290 parts of D-2, 860 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to normal temperature, and after cooling, 3 parts of B-1, 7.5 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
Comparative example 6
100 parts of A-1, 250 parts of D-1, 280 parts of D-2, 850 parts of D-3 and E are mixed for 1 hour under the vacuum condition (the vacuum degree is 0.09 MPa) at 160 ℃, then cooled to the normal temperature, and after cooling, 1.5 parts of B-1, 8 parts of NonB-3 and 0.12 part of C-1 are added for mixing and stirring.
The thermally conductive gels of examples 1-6 and comparative examples 1-6 were tested and the results are shown in the table:
| coefficient of thermal conductivity | Hardness of | Percent compression set% | Whether or not to repeatedly maintain | |
| Example 1 | 5 | 25 | 25 | Is that |
| Example 2 | 4 | 80 | 3 | Whether or not |
| Example 3 | 5.5 | 65 | 4 | Is that |
| Example 4 | 5.5 | 54 | 6 | Is that |
| Example 5 | 6 | 30 | 13 | Is that |
| Example 6 | 5 | 37 | 11 | Is that |
| Comparative example 1 | 4.5 | 95 | 0 | Whether or not |
| Comparative example 2 | 4 | 90 | 0 | Whether or not |
| Comparative example 3 | 5 | 40 | 0 | Whether or not |
| Comparative example 4 | 5 | 20 | 0 | Whether or not |
| Comparative example 5 | 5.5 | 50 | 0 | Whether or not |
| Comparative example 6 | 4.5 | 80 | 0 | Whether or not |
Examples 1, 5, 6 the thermally conductive gel exhibited stress relaxation under given pressure conditions, and could be peeled off at the time of practical use, facilitating the maintenance of the equipment. Comparative examples 1 to 6 used hydrogen-terminated polysiloxane, and the gels produced were relatively hard, had poor compression set, were difficult to peel off in practical use, and were inconvenient for maintenance of equipment.
Claims (11)
1. An easily filled and easily reworked thermally conductive gel, which is characterized by comprising the following components:
100 parts of component A, 1-15 parts of component B, 0.01-0.15 part of catalyst C, 400-3500 parts of heat-conducting filler D and component E, wherein the component A is alkylene polysiloxane and has the viscosity of 10-10000mPa & s at normal temperature; the component B is straight-chain hydrogenpolysiloxane, each molecule contains 2-4 Si-H bonds and at least 2 Si-H bonds on a side chain, the viscosity is 1-1000 mPa.s at normal temperature, and the molecular formula of the component E is YnSi (OR) 4-n Wherein Y is an alkyl group of 6 to 18 carbon atoms, R is an alkyl group of 1 to 5 carbon atoms, and n represents an integer of 1 to 2, and said component E is a surface treating agent for component D in an amount of 0.2 to 2% based on D.
2. The easily fillable easily reworkable thermally conductive gel of claim 1, wherein component a is comprised of one or more alkylene polysiloxanes, said component a having a molecular structure represented by:
wherein R is 1 RepresentsMonovalent hydrocarbon radicals free of labile aliphatic groups, R 2 Is a hydrocarbon radical, R 3 Is an alkylene group, a represents an integer of 0 to 2, P represents an integer of 1 to 50, and R 3 Comprises ethenyl, propenyl, butenyl, hexenyl, and also comprises methyl, ethyl, propyl, and aromatic groups.
3. An easily filled and easily reworked thermally conductive gel according to claim 1, wherein the catalyst comprises one of a platinum catalyst, a rhodium-based catalyst, or a palladium-based catalyst, and wherein the platinum catalyst comprises fine platinum powder, hydrochloroplatinic acid, alcohol-diluted hydrochloroplatinic acid, a platinum vinyl siloxane complex, and a platinum carbonate complex, and wherein the platinum catalyst is preferably a platinum vinyl siloxane complex.
4. An easily filled and easily reworked thermally conductive gel according to claim 1, wherein said component D thermally conductive filler comprises one or more powders or fibers of metals, metal oxides, metal nitrides, metal hydroxides, metal carbides, metal silicides, carbon fibers, soft magnetic alloys and ferrites.
5. The easily-filled and easily-repaired heat-conducting gel as claimed in claim 4, wherein the component D heat-conducting filler is preferably metal oxide, metal nitride or carbon fiber.
6. The easily-filled and easily-reworked thermally conductive gel according to claim 1, wherein the thermally conductive filler component D comprises D1, D2, D3 and D4, wherein D1 is flaky boron nitride powder with an average particle size of 0.1-30 microns, D2 is regular boron nitride powder with an average particle size of 0.1-50 microns, D3 is spherical alumina powder with an average particle size of 0.01-50 microns, and D4 is spherical graphite with an average particle size of 0.01-50 microns.
7. The easily filled and easily reworked thermally conductive gel of claim 6, wherein component D thermally conductive filler preferably has an average particle size of 0.01 to 50 microns.
8. An easily fillable easily reworkable thermally conductive gel according to claim 1 further comprising a reaction inhibitor for extending the shelf life thereof, said reaction inhibitor comprising ethynyl cyclohexanol, amine group, carboxylate group, phosphite group inhibitors.
9. The method for preparing the easily-filled and easily-repaired heat-conducting gel according to any one of claims 1 to 8, characterized by comprising the following steps: mixing the component D and the component E, carrying out surface treatment on the component D, then pouring the components A and B and the catalyst C, and stirring.
10. The method for preparing the easily-filled and easily-repaired heat-conducting gel according to any one of claims 1 to 8, characterized by comprising the following steps: mixing the components A, D and E, mixing the component B and the catalyst C after the surface treatment of the component D is finished, and stirring.
11. The method for preparing the easily-filled and easily-repaired heat-conducting gel according to claim 9 or 10, wherein a mixing stirrer used for stirring needs to have a vacuum pumping function, the vacuum degree can reach 0.1MPa, and the method comprises a single-blade stirrer, a double-blade stirrer and a kneader.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116023785A (en) * | 2021-10-27 | 2023-04-28 | 万华化学集团股份有限公司 | Heat-conducting gel and preparation method thereof |
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| CN113248931A (en) * | 2021-05-31 | 2021-08-13 | 广东恒大新材料科技有限公司 | Heat-conducting gel with high heat conductivity and high extrusion rate and preparation method thereof |
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Patent Citations (4)
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| CN111073300A (en) * | 2019-12-13 | 2020-04-28 | 深圳市丰盛源科技有限公司 | Heat-conducting gel easy to repair and preparation method thereof |
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| CN116023785A (en) * | 2021-10-27 | 2023-04-28 | 万华化学集团股份有限公司 | Heat-conducting gel and preparation method thereof |
| CN116023785B (en) * | 2021-10-27 | 2024-04-09 | 万华化学集团股份有限公司 | Heat-conducting gel and preparation method thereof |
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