CN113527852A - Phase-change heat-conducting silicone grease - Google Patents
Phase-change heat-conducting silicone grease Download PDFInfo
- Publication number
- CN113527852A CN113527852A CN202110828286.2A CN202110828286A CN113527852A CN 113527852 A CN113527852 A CN 113527852A CN 202110828286 A CN202110828286 A CN 202110828286A CN 113527852 A CN113527852 A CN 113527852A
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- Prior art keywords
- phase change
- stirring
- parts
- zinc oxide
- silicone resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Lubricants (AREA)
Abstract
The invention relates to the field of heat dissipation materials, in particular to phase-change heat-conducting silicone grease which comprises the following components: 3-4% of liquid silicone resin, 6-8% of polycaprolactone, 40-55% of zinc oxide and 40-55% of aluminum oxide; the preparation method comprises the following steps: the method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30 min; step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min); step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product; step four: and detecting the product. The product state of the invention changes along with the temperature change, the product is solid at the temperature of 60 ℃ and liquid at the temperature of more than 60 ℃, the situation that the product cannot be smeared due to overlarge viscosity can not occur, the heat conductivity coefficient is high, and the heat conductivity is good.
Description
Technical Field
The invention relates to the field of heat dissipation materials, in particular to phase change heat conduction silicone grease.
Background
The electronic appliance industry develops rapidly, electronic components can emit large amount of heat in the working process, the temperature of the electronic components rises rapidly to cause local high temperature, the performance of the electronic components can be seriously influenced by the high temperature, the service life of the electronic components is shortened, and the heat dissipation requirement on the electronic components is very high. The heat-conducting silicone grease is a common product for heat dissipation of electronic components, can be used for a long time at 120 ℃ and kept in a paste shape, has good insulating property, is nontoxic and tasteless, has stable chemical properties, and does not corrode the electronic components;
the silicone grease is refined by using refined synthetic oil as base oil and adding a structural stabilizer and an anti-corrosion additive, has good waterproof sealing property, water resistance, solvent resistance and anti-creeping property, does not corrode metal, has good adaptability with rubber, is used for waterproof sealing and lubrication of bathroom equipment, sealing rings and the electronic and electrical industry, and is divided into two types, namely heat-conducting silicone grease and lubricating silicone grease;
at present, metal powder and metal oxide are mainly dispersed in liquid silicone resin, and the heat-conducting silicone grease is obtained by fully stirring and grinding, and a patent with the application number of CN201910010508.2 discloses a preparation method and application of thixotropic emulsified silicone grease, which aim to solve the problem that an emulsified silicone oil product prepared by the existing method is poor in placement stability, and the preparation method comprises the following steps: firstly, adding higher fatty acid into an aqueous solution of organic alcohol amine to prepare fatty acid alcohol amine salt; secondly, adding p-cumylphenol polyoxyethylene ether into fatty acid ethanolamine salt to prepare a composite emulsifier; adding water into a composite emulsifier, dissolving to prepare a composite emulsifier aqueous solution, then adding dimethyl silicon oil and fumed silica under stirring to prepare thixotropic emulsified silicone grease with adjustable solid content, adopting a special surfactant formula, and preparing emulsified silicone grease with good thixotropic performance on the basis of not adding a tackifier, wherein the prepared emulsified silicone grease almost has no fluidity, so that the problem of placing stability of emulsified silicone oil is solved, but the existing silicone grease can cause overlarge viscosity and can not be smeared if the powder adding proportion is increased; if the powder addition ratio is reduced, the thermal conductivity is low and the thermal conductivity is poor, and in this case, a phase-change thermal grease has been proposed.
Disclosure of Invention
The invention aims to provide phase change heat conduction silicone grease, which has the advantages that the product state changes along with the temperature change, the product is solid at the temperature of 60 ℃, the product is liquid at the temperature of more than 60 ℃, the situation that the product is too high in viscosity and cannot be smeared is avoided, the heat conduction coefficient is high, and the heat conduction performance is good.
The purpose of the invention can be realized by the following technical scheme:
the phase-change heat-conducting silicone grease comprises the following components: 3-4% of liquid silicone resin, 6-8% of polycaprolactone, 40-55% of zinc oxide and 40-55% of aluminum oxide;
the liquid silicone resin is dimethyl siloxane.
Further, the viscosity of the liquid silicone resin is 500-600 mpa.s.
Further, the polycaprolactone is granular, and the melting point of the polycaprolactone is 60-62 ℃.
Further, the zinc oxide is flaky zinc oxide, and the particle size is 1-3 um.
Further, the alumina is spherical alumina, and the particle size is 5-7 um.
Further, the preparation method of the phase-change heat-conducting silicone grease comprises the following steps:
the method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30 min;
step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min);
step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product;
step four: and detecting the product.
Further, the detection indexes of the fourth step comprise K value, viscosity (70 ℃) and the indexes of about 60 DEG C
Status.
Further, the stirring speed in the first step is 250-300 r/min.
Preferably, the phase-change heat-conducting silicone grease comprises the following components: liquid silicone resin 3 parts, polyhexamethylene
7 parts of lactone, 45 parts of zinc oxide and 45 parts of aluminum oxide.
Preferably, the phase-change heat-conducting silicone grease comprises the following components: liquid silicone resin 4 parts, polyhexamethylene
6 parts of lactone, 50 parts of zinc oxide and 40 parts of aluminum oxide.
The invention has the beneficial effects that:
1. the product state of the invention changes along with the temperature change, the product is solid at the temperature of 60 ℃ and liquid at the temperature of more than 60 ℃, the situation that the product cannot be smeared due to overlarge viscosity can not occur, the heat conductivity coefficient is high, and the heat conductivity is good.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
The phase-change heat-conducting silicone grease comprises the following components: 3-4% of liquid silicone resin, 6-8% of polycaprolactone, 40-55% of zinc oxide and 40-55% of aluminum oxide;
wherein the liquid silicone resin is dimethyl siloxane, and the viscosity is 500-600 mpa.s;
the polycaprolactone is granular, and the melting point is 60-62 ℃;
the zinc oxide is flaky zinc oxide with the particle size of 1-3 um, and the aluminum oxide is spherical aluminum oxide with the particle size of 5-7 um;
the preparation method of the phase-change heat-conducting silicone grease comprises the following steps:
the method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30min (the rotating speed is 250-300 r/min);
step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min);
step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product;
step four: and detecting the product.
Implementing one step:
3 parts of liquid silicone resin, 7 parts of polycaprolactone, 45 parts of zinc oxide and 45 parts of aluminum oxide.
The method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30min (the rotating speed is 250-300 r/min);
step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min);
step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product;
step four: and detecting the product.
The main properties of the prepared phase change heat conduction silicone grease are tested as follows:
the K value is 5.0 w/(m.k);
solid at 60 ℃ and liquid at above 60 ℃;
viscosity (70 ℃): 50.000 mpa.s.
The second implementation:
4 parts of liquid silicone resin, 6 parts of polycaprolactone, 50 parts of zinc oxide and 40 parts of aluminum oxide. The method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30min (the rotating speed is 250-300 r/min);
step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min);
step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product;
step four: and detecting the product.
The main properties of the prepared phase change heat conduction silicone grease are tested as follows:
the K value is 5.5 w/(m.k);
solid at 60 ℃ and liquid at above 60 ℃;
viscosity (70 ℃): 55.000 mpa.s.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (10)
1. Phase change heat conduction silicone grease is characterized by comprising the following components: 3-4% of liquid silicone resin, 6-8% of polycaprolactone, 40-55% of zinc oxide and 40-55% of aluminum oxide;
the liquid silicone resin is dimethyl siloxane.
2. The phase change thermal grease as claimed in claim 1, wherein the viscosity of the liquid silicone resin is 500 to 600 mpa.s.
3. The phase change thermal silicone grease as claimed in claim 1, wherein the polycaprolactone is in the form of particles and has a melting point of 60-62 ℃.
4. The phase change heat conductive silicone grease as claimed in claim 1, wherein the zinc oxide is a flake zinc oxide having a particle size of 1 to 3 um.
5. The phase change thermal grease as claimed in claim 1, wherein the alumina is spherical alumina with a particle size of 5-7 um.
6. The phase change thermal grease as claimed in claim 1, wherein the preparation method of the phase change thermal grease comprises the following steps:
the method comprises the following steps: pouring liquid silicone resin into a planetary dispersion machine, heating to 70 ℃, adding polycaprolactone, and stirring at a low speed for 30 min;
step two: adding zinc oxide into the mixed solution in the first step, stirring for 30min (the rotating speed is 250-300 r/min), then adding aluminum oxide, and stirring for 30min (the rotating speed is 200-300 r/min);
step three: increasing the rotating speed to 800-1000 r/min, and stirring for 2 hours to obtain a final product;
step four: and detecting the product.
7. The phase change thermal grease as claimed in claim 6, wherein the four test indicators include K, viscosity (70 ℃) and temperature of about 60 ℃.
8. The phase change heat conductive silicone grease as claimed in claim 6, wherein the first stirring speed is 250-300 r/min.
9. The phase change thermal grease as claimed in claim 1, wherein the phase change thermal grease comprises the following components: 3 parts of liquid silicone resin, 7 parts of polycaprolactone, 45 parts of zinc oxide and 45 parts of aluminum oxide.
10. The phase change thermal grease as claimed in claim 1, wherein the phase change thermal grease comprises the following components: 4 parts of liquid silicone resin, 6 parts of polycaprolactone, 50 parts of zinc oxide and 40 parts of aluminum oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110828286.2A CN113527852A (en) | 2021-07-18 | 2021-07-18 | Phase-change heat-conducting silicone grease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110828286.2A CN113527852A (en) | 2021-07-18 | 2021-07-18 | Phase-change heat-conducting silicone grease |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113527852A true CN113527852A (en) | 2021-10-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110828286.2A Pending CN113527852A (en) | 2021-07-18 | 2021-07-18 | Phase-change heat-conducting silicone grease |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115160992A (en) * | 2022-07-20 | 2022-10-11 | 昆山纳诺新材料科技有限公司 | Preparation method of phase-change heat-conducting silicone grease |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103214848A (en) * | 2013-04-28 | 2013-07-24 | 深圳市新亚新材料有限公司 | Phase change heat-conducting thermal silicone grease composition for central processing unit (CPU) radiating and preparation method thereof |
| CN106832833A (en) * | 2017-02-13 | 2017-06-13 | 艾伯尔三氐生物科技（重庆）有限公司 | A kind of 3D printing shape memory resin material, preparation method and applications |
| JP2018053025A (en) * | 2016-09-27 | 2018-04-05 | 信越化学工業株式会社 | Thermally conductive silicone grease composition |
| CN108047722A (en) * | 2017-12-07 | 2018-05-18 | 航天特种材料及工艺技术研究所 | A kind of phase-change thermal conduction silicone grease and preparation method thereof |
| CN111303642A (en) * | 2019-11-26 | 2020-06-19 | 东莞市美庆电子科技有限公司 | Low-thermal-resistance phase-change heat conduction material and preparation method thereof |
-
2021
- 2021-07-18 CN CN202110828286.2A patent/CN113527852A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103214848A (en) * | 2013-04-28 | 2013-07-24 | 深圳市新亚新材料有限公司 | Phase change heat-conducting thermal silicone grease composition for central processing unit (CPU) radiating and preparation method thereof |
| JP2018053025A (en) * | 2016-09-27 | 2018-04-05 | 信越化学工業株式会社 | Thermally conductive silicone grease composition |
| CN106832833A (en) * | 2017-02-13 | 2017-06-13 | 艾伯尔三氐生物科技（重庆）有限公司 | A kind of 3D printing shape memory resin material, preparation method and applications |
| CN108047722A (en) * | 2017-12-07 | 2018-05-18 | 航天特种材料及工艺技术研究所 | A kind of phase-change thermal conduction silicone grease and preparation method thereof |
| CN111303642A (en) * | 2019-11-26 | 2020-06-19 | 东莞市美庆电子科技有限公司 | Low-thermal-resistance phase-change heat conduction material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115160992A (en) * | 2022-07-20 | 2022-10-11 | 昆山纳诺新材料科技有限公司 | Preparation method of phase-change heat-conducting silicone grease |
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Application publication date: 20211022 |
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