CN108373592B - Heat-conducting silicone grease composition, heat-conducting silicone grease and LED lighting device - Google Patents
Heat-conducting silicone grease composition, heat-conducting silicone grease and LED lighting device Download PDFInfo
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Abstract
The invention relates to a heat-conducting silicone grease composition, heat-conducting silicone grease and LED lighting equipment, wherein the composition comprises silicone oil, a first filler, a second filler and an optional auxiliary agent, wherein 100 parts by weight of the silicone oil is taken as a reference, the content of the first filler is 10-60 parts by weight, the content of the second filler is 50-150 parts by weight, and the content of the auxiliary agent is 0-20 parts by weight; the first filler comprises a metal heat conductor and a phase-change material, and the weight ratio of the metal heat conductor to the phase-change material is 1: (0.2 to 2.5); the second filler is carbon nano tube and graphene, and the weight ratio of the carbon nano tube to the graphene is 1: (1-20). The heat-conducting silicone grease prepared from the heat-conducting silicone grease composition disclosed by the invention has the advantages of higher heat conductivity coefficient, lower thermal resistance, good heat dissipation efficiency, long service life, and excellent practical value and economic value.
Description
Technical Field
The disclosure relates to the field of thermal interface materials, in particular to a heat-conducting silicone grease composition, heat-conducting silicone grease and LED lighting equipment.
Background
With the rapid development of computer technology, the operation speed of a Central Processing Unit (CPU) as a core of a computer system is faster and faster, and the heat generation amount thereof is increased. If the CPU does not dissipate heat well and the temperature is too high, the problems of hot start, crash and the like of the computer in the running process are easily caused. Therefore, providing a good heat dissipation system for the CPU is one of the important conditions for ensuring the normal operation of the computer. The LED is a novel injection electroluminescent device, and has the advantage of energy conservation. Currently, the power of a single LED device has stepped from the first milliwatt level to the present tens of watts level. It has been tested that the electro-optic conversion efficiency of a single LED device is only 15%, and the remaining approximately 85% of the electrical energy is converted into thermal energy. When a plurality of LEDs are densely arranged to form a lighting system, the conversion of electrical energy into thermal energy is more serious. Therefore, solving the heat dissipation problem of high power LEDs has become a prerequisite for its wide application.
In order to solve the problem of heat dissipation of heat sources such as CPU chips and high-power LED lighting systems, a common method is to mount a heat sink on the heat source. Even if the surface-to-surface contact between the heat source such as a CPU and the heat sink is smooth, a certain gap inevitably exists, and the existence of the gap seriously affects the heat dissipation effect.
Thermal interface materials are widely used because they can effectively reduce the thermal interface resistance between the heat source and the heat sink. The heat-conducting silicone grease is one of the most commonly used heat-conducting media, and is a material used for filling a gap between a heat source and a heat sink, so that heat emitted by the heat source is conducted to the heat sink, the temperature of the heat source is kept at a level capable of stably working, the service life of a device is prolonged, and the heat source is prevented from being damaged due to poor heat dissipation.
The heat-conducting silicone grease is generally formed by mixing silicone oil and heat-conducting filler. In the existing high-end heat-conducting silicone grease, the heat-conducting filler is generally silver powder and graphite materials. The thermal conductivity of graphite powder is generally 150-300W/(M.K), the thermal conductivity of silver powder is only 429W/(M.K), and the graphite powder is expensive and has limited contribution to improving the overall thermal conductivity of silicone grease. In addition, in the long-term use process, the phenomenon that the silicone oil is separated from the heat-conducting filler often occurs, so that the heat-conducting silicone grease coating is differentiated and cracked, the heat-conducting performance is deteriorated and the like; if high-viscosity base oil is adopted, the heat-conducting filler with high solid content is difficult to add, and the heat-conducting performance of the product is poor.
Disclosure of Invention
The purpose of the present disclosure is to provide a heat conductive silicone grease composition, a heat conductive silicone grease, and an LED lighting device, wherein the heat conductive silicone grease has high heat conduction efficiency and good heat dissipation effect.
To achieve the above object, a first aspect of the present disclosure: providing a heat-conducting silicone grease composition, which comprises 10-60 parts by weight of silicone oil, 50-150 parts by weight of a first filler, 50-150 parts by weight of a second filler and 0-20 parts by weight of an optional auxiliary agent, wherein 100 parts by weight of the silicone oil is taken as a reference; the first filler comprises a metal heat conductor and a phase-change material, and the weight ratio of the metal heat conductor to the phase-change material is 1: (0.2 to 2.5); the second filler is carbon nano tube and graphene, and the weight ratio of the carbon nano tube to the graphene is 1: (1-20).
Optionally, the first filler is contained in an amount of 20 to 40 parts by weight, the second filler is contained in an amount of 80 to 120 parts by weight, and the auxiliary is contained in an amount of 0 to 10 parts by weight, based on 100 parts by weight of the silicone oil.
Alternatively, R is 6.5 to 35.5 as calculated by the formula:
r ═ 0.656w (second filler) -1.581w (first filler) +0.11w (adjuvant),
wherein w (first filler) represents parts by weight of the first filler relative to 100 parts by weight of the silicone oil,
w (second filler) represents parts by weight of the second filler relative to 100 parts by weight of the silicone oil,
w (adjuvant) represents the parts by weight of adjuvant with respect to 100 parts by weight of silicone oil.
Optionally, the metal heat conductor is at least one selected from the group consisting of a metal, a metal oxide, a metal carbide and a metal nitride, and the metal in the metal heat conductor is at least one selected from the group consisting of platinum, silver, copper, aluminum, tin, zinc, calcium, lanthanum, yttrium and cerium;
the phase-change temperature of the phase-change material is 20-80 ℃, the phase-change material is at least one selected from paraffin, polyethylene glycol, stearic acid and urea, and the paraffin is at least one selected from microcrystalline wax, liquid paraffin, polyethylene wax and semi-refined paraffin.
Optionally, the phase change material is polyethylene glycol.
Optionally, the phase change material is polyethylene glycol, the metal heat conductor is zinc oxide, and the weight ratio of the zinc oxide to the polyethylene glycol is 1: (1-1.5).
Optionally, the phase change material is polyethylene wax.
Optionally, the phase change material is polyethylene wax, the metal heat conductor is copper, and the weight ratio of the copper to the polyethylene wax is 1: (1.5-2).
Optionally, the first filler is a capsule formed by wrapping the phase change material with the metal heat conductor, and the particle size of the capsule is 1-100 nm.
Optionally, the average particle size of the graphene is 0.1-20 μm, and the graphene is at least one selected from the group consisting of reduced graphene, oxidized graphene, graphene nanoplatelets and modified graphene.
Optionally, the modified graphene is obtained by mixing graphene oxide, silicate, an inorganic alkali solution, a water-soluble high molecular compound and a surfactant, reacting at 10-50 ℃ for 0.1-10 hours, and drying.
Optionally, the weight ratio of the graphene oxide, the organosilicate, the inorganic alkali solution, the water-soluble high molecular compound and the surfactant is 1: (0.5-6): (0.1-10): (0.02-0.5): (0.02-1).
Optionally, the silicate is at least one selected from the group consisting of tetramethyl orthosilicate, tetraethyl orthosilicate, isopropyl orthosilicate, and trimethylsiloxysilicate;
the concentration of the inorganic alkali solution is 30-100 g/L, and the inorganic alkali solution is at least one selected from a sodium hydroxide solution, a potassium hydroxide solution, a calcium hydroxide solution, a sodium carbonate solution, a sodium bicarbonate solution and a potassium carbonate solution;
the water-soluble high molecular compound is at least one selected from polyacrylamide, polyacrylic acid, polyvinyl alcohol, polymaleic anhydride, epoxy resin, alkyd resin and amino resin;
the surfactant is at least one selected from triethanolamine, cetyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide, dodecyl aminopropionic acid, methyl acrylate and alkyl dimethyl hydroxypropyl phosphate betaine.
Alternatively, the silicate is tetramethyl orthosilicate and trimethylsiloxysilicate, and the weight ratio of the tetramethyl orthosilicate to the trimethylsiloxysilicate is 1: (0.1 to 1);
the water-soluble high molecular compound is polyacrylic acid, and the weight-average molecular weight of the polyacrylic acid is 5000-20000.
Optionally, the purity of the carbon nanotube is not less than 95 wt%, the ash content is not more than 0.2 wt%, and the specific surface area is 40-300 m2/g。
Optionally, the silicone oil is at least one selected from dimethyl silicone oil, vinyl silicone oil, hydrogen-containing silicone oil, benzyl silicone oil, hydroxyl silicone oil, methyl long-chain alkyl silicone oil and quaternary ammonium salt hydrocarbon-based modified silicone oil.
Optionally, the silicone oil has a viscosity of 50000-500000 cSt at 25 ℃.
Optionally, the adjuvant is at least one selected from the group consisting of antioxidants, corrosion inhibitors, antiwear agents, and lubrication enhancers.
In a second aspect of the disclosure, a heat-conducting silicone grease prepared from the composition of the first aspect of the disclosure is provided, wherein the heat-conducting silicone grease has a heat conductivity of 4.5-8W/m.K and a thermal resistance of 5.8 × 10-6-1×10-5K·m2/W。
In a third aspect of the present disclosure, there is provided an LED lighting device comprising an LED light source and a heat sink assembly connected thereto, the heat sink assembly comprising the thermally conductive silicone grease of the second aspect of the present disclosure.
Through the technical scheme, the heat-conducting silicone grease composition disclosed by the invention adopts the metal heat conductor and the phase-change material as the first filler, and compared with the traditional heat-conducting silicone grease only adopting the metal heat conductor as the filler, the heat-conducting silicone grease composition can effectively improve the absorption rate of heat of a heat source and has the effects of quickly absorbing heat and transferring heat; meanwhile, the carbon nano tube and the graphene are used as second fillers, so that the heat conductivity coefficient is greatly improved, the compatibility with silicone oil is facilitated, and the quality and the performance of the product are further improved. The heat-conducting silicone grease prepared from the heat-conducting silicone grease composition disclosed by the invention has the advantages of higher heat conductivity coefficient, lower thermal resistance, good heat dissipation efficiency, long service life, and excellent practical value and economic value. The heat-conducting silicone grease disclosed by the invention is used for LED heat-radiating equipment, so that the heat-radiating capacity of the equipment can be obviously improved, and the service life of the equipment is prolonged.
Additional features and advantages of the disclosure will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present disclosure. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
The first aspect of the disclosure: providing a heat-conducting silicone grease composition, which comprises 10-60 parts by weight of silicone oil, 50-150 parts by weight of a first filler, 50-150 parts by weight of a second filler and 0-20 parts by weight of an optional auxiliary agent, wherein 100 parts by weight of the silicone oil is taken as a reference; the first filler comprises a metal heat conductor and a phase-change material, and the weight ratio of the metal heat conductor to the phase-change material is 1: (0.2 to 2.5); the second filler is carbon nano tube and graphene, and the weight ratio of the carbon nano tube to the graphene is 1: (1-20).
The heat-conducting silicone grease composition disclosed by the invention adopts the metal heat conductor and the phase-change material as the first filler, and compared with the traditional heat-conducting silicone grease only adopting the metal heat conductor as the filler, the heat-conducting silicone grease composition can effectively improve the absorption rate of heat of a heat source and has the effects of quickly absorbing heat and transferring heat; meanwhile, the carbon nano tube and the graphene are used as second fillers, so that the heat conductivity coefficient is greatly improved, the compatibility with silicone oil is facilitated, and the quality and the performance of the product are further improved.
According to the present disclosure, in order to further improve the thermal conductivity of the heat conductive silicone grease and reduce the thermal resistance value, preferably, the content of the first filler is 20 to 40 parts by weight, the content of the second filler is 80 to 120 parts by weight, and the content of the auxiliary agent is 0 to 10 parts by weight, based on 100 parts by weight of the silicone oil.
According to the present disclosure, in order to further improve the thermal conductivity of the thermal grease and reduce the thermal resistance value, R calculated by the following formula may be 6.5 to 35.5:
r ═ 0.656w (second filler) -1.581w (first filler) +0.11w (adjuvant),
wherein w (first filler) represents parts by weight of the first filler relative to 100 parts by weight of the silicone oil,
w (second filler) represents parts by weight of the second filler relative to 100 parts by weight of the silicone oil,
w (adjuvant) represents the parts by weight of adjuvant with respect to 100 parts by weight of silicone oil.
According to the present disclosure, the weight ratio of the metal heat conductor and the phase change material is preferably 1: (1-2), for example, may be 1: (1.2-1.5), 1: (1.8-2). The first filler composed of the metal heat conductor and the phase-change material in the proportioning range can improve the heat conductivity coefficient and the heat transfer effect of the heat-conducting silicone grease to the greatest extent.
According to the present disclosure, the metal heat conductor is a common metal material having a heat conductive property, and for example, may be at least one selected from a metal, a metal oxide, a metal carbide, and a metal nitride, and the metal in the metal heat conductor may be at least one selected from platinum, silver, copper, aluminum, tin, zinc, calcium, lanthanum, yttrium, and cerium.
According to the present disclosure, in order to achieve an ideal effect, the phase transition temperature of the phase change material may be 20 to 80 ℃. The phase change material may be a general species having a phase change temperature within the above range, and for example, may be at least one selected from paraffin, polyethylene glycol, stearic acid, and urea. The paraffin wax may be at least one selected from the group consisting of microcrystalline wax, liquid paraffin wax, polyethylene wax, and semi-refined paraffin wax.
According to a preferred embodiment of the present disclosure, the phase change material is polyethylene glycol. In this embodiment, further, the metal thermal conductor may be zinc oxide, and in this case, the weight ratio of the zinc oxide to the polyethylene glycol may be 1: (1-1.5). This preferred embodiment is advantageous for achieving a higher thermal conductivity and a lower thermal resistance value.
According to another preferred embodiment of the present disclosure, the phase change material is polyethylene wax. In this embodiment, the metal heat conductor is copper, and in this case, the weight ratio of copper to polyethylene wax may be 1: (1.5-2). This preferred embodiment is advantageous for obtaining a better heat absorption rate and heat transfer effect.
According to the disclosure, the first filler is preferably a capsule formed by wrapping the phase change material with the metal heat conductor, and the particle size of the capsule is 1-100 nm. Therefore, the first filler in the capsule form has larger specific surface area, is favorable for further exerting the heat absorption performance of the phase-change material, and improves the heat absorption rate of a heat source. At this time, the size of the metal heat conductor is in the order of nanometers.
According to the present disclosure, the thermal conductivity of the thermal grease can be greatly improved by adding graphene. In order to achieve the above object, the average particle diameter of the graphene may be 0.1 to 20 μm. The graphene may be various types of graphene, for example, reduced graphene, oxidized graphene, graphene nanoplatelets, or modified graphene obtained by modifying the graphene.
According to the present disclosure, in order to obtain an ideal heat conductive silicone grease, the modified graphene may be obtained by modifying graphene for the purposes of increasing the heat conductivity coefficient of graphene, improving the surface properties of graphene, and reducing the electrical conductivity. In research, the inventors of the present disclosure found that modified graphene obtained by modifying graphene oxide by a specific method not only has improved thermal conductivity, but also has improved insulation properties (i.e., reduced electrical conductivity), and at the same time has good compatibility with silicone oil, and is more suitable for use in the thermal conductive silicone grease of the present disclosure. Therefore, in a preferred embodiment of the present disclosure, the modified graphene is obtained by mixing graphene oxide, silicate, an inorganic alkaline solution, a water-soluble polymer compound, and a surfactant, reacting at 10 to 50 ℃ for 0.1 to 10 hours, and then drying.
In the above embodiment, in order to achieve a desired effect, the weight ratio of the graphene oxide, the organosilicate, the inorganic alkali solution, the water-soluble polymer compound, and the surfactant may be 1: (0.5-6): (0.1-10): (0.02-0.5): (0.02 to 1), preferably 1: (1-1.5): (0.5-5): (0.1-0.3): (0.05-0.5).
In the above embodiment, the silicate may be at least one selected from the group consisting of tetramethyl orthosilicate, tetraethyl orthosilicate, isopropyl orthosilicate, and trimethylsiloxysilicate. According to a preferred embodiment, the silicate is tetramethyl orthosilicate and trimethylsiloxysilicate, which may be present in a weight ratio of 1: (0.1-1), the silicate ester with the combination and the proportion can form an insulating film layer coated on the surface of the graphene oxide in a modification reaction, so that the conductivity of the graphene is reduced.
In the above embodiment, the inorganic base solution may be a common aqueous solution of various inorganic bases, and for example, may be at least one selected from a sodium hydroxide solution, a potassium hydroxide solution, a calcium hydroxide solution, a sodium carbonate solution, a sodium bicarbonate solution, and a potassium carbonate solution. The concentration of the inorganic alkali solution can be 30-100 g/L.
In the above embodiment, the water-soluble polymer compound may be a polymer resin and/or a condensation resin, and is preferably at least one selected from the group consisting of polyacrylamide, polyacrylic acid, polyvinyl alcohol, polymaleic anhydride, an epoxy resin, an alkyd resin, and an amino resin. In order to further improve the compatibility with silicone oil, the water-soluble polymer compound is preferably polyacrylic acid, and the weight average molecular weight of the polyacrylic acid may be 5000 to 20000.
In the above embodiment, the surfactant may be a cationic surfactant and/or a zwitterionic surfactant, preferably at least one selected from triethanolamine, cetyltrimethylammonium bromide, tetradecyltrimethylammonium bromide, dodecylaminopropionic acid, methyl acrylate, and alkyldimethylhydroxypropylated phosphate betaine, and most preferably, cetyltrimethylammonium bromide.
In the above embodiment, the reaction temperature is preferably 20 to 40 ℃, and the reaction time is preferably 2 to 4 hours. The drying conditions may be: the temperature is 80-150 ℃, and preferably 90-120 ℃; the time is 1-24 h, preferably 2-4 h.
According to the present disclosure, in order to achieve a desired effect, the purity of the carbon nanotube may be not less than 95 wt%, the ash content may be not more than 0.2 wt%, and the specific surface area may be 40 to 300m2/g。
According to the present disclosure, the silicone oil may be a commonly used kind for preparing the heat conductive silicone grease, for example, at least one selected from the group consisting of dimethyl silicone oil, vinyl silicone oil, hydrogen-containing silicone oil, benzyl silicone oil, hydroxy silicone oil, methyl long-chain alkyl silicone oil, and quaternary ammonium salt hydrocarbon-modified silicone oil. The viscosity of the silicone oil at 25 ℃ can be 50000-500000 cSt.
According to the present disclosure, the auxiliary may be a conventional auxiliary for preparing a heat conductive silicone grease, and for example, may be at least one selected from an antioxidant, a corrosion inhibitor, an antiwear agent, and a lubrication improver. The antioxidant may be, for example, an amine antioxidant, a phenol antioxidant, a phosphite antioxidant, or the like. The corrosion inhibitor may be, for example, a naphthenate salt or the like. The antiwear agent may be, for example, a sulfur-containing compound, a phosphorus-containing compound, or the like. The lubrication enhancer may be, for example, mineral oil or the like. The present disclosure is not particularly limited with respect to the type of adjuvant and the selection of particular materials.
In a second aspect of the present disclosure: there is provided a thermally conductive silicone grease prepared from the composition according to the first aspect of the present disclosure. The preparation method of the heat conductive silicone grease may be conventional in the art, and the present disclosure is not particularly limited. The heat-conducting silicone grease prepared by the composition of the first aspect of the disclosure has a higher heat conductivity coefficient and a lower thermal resistance value: the above-mentionedThe heat conductivity coefficient of the heat-conducting silicone grease can be 4.5-8W/m.K, and the thermal resistance is 5.8 × 10-6-1×10-5K·m2and/W. The heat-conducting silicone grease has good heat dissipation efficiency, long service life and excellent practical value and economic value.
In a third aspect of the present disclosure, there is provided an LED lighting device comprising an LED light source and a heat sink assembly connected thereto, the heat sink assembly comprising the thermally conductive silicone grease of the second aspect of the present disclosure. The LED lighting device provided by the third aspect of the disclosure has good heat dissipation capability and obviously prolonged service life.
The present disclosure is further described below by way of examples, but the present disclosure is not limited thereto in any way.
In the examples, graphene oxide was prepared according to the method of example 1 in CN102153075B, and the average particle size was 0.1 to 20 μm. Other raw materials are all commercial products.
Examples 1-18 are provided to illustrate thermally conductive silicone grease compositions provided by the present disclosure and thermally conductive silicone greases prepared therefrom.
Example 1
In the heat conductive silicone grease composition of the present example, the silicone oil was dimethyl silicone oil (viscosity at 25 ℃ C. was 450000 cSt); the first filler is zinc oxide and polyethylene glycol (molecular weight is 6000, phase transition temperature is 60-65 ℃), and the weight ratio is 1: 1.2; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2/g) and graphene oxide in a weight ratio of 1: 10.
100 parts by weight of silicone oil, 30 parts by weight of the first filler and 100 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 2
In the heat conductive silicone grease composition of the present example, the silicone oil was a vinyl silicone oil (viscosity at 25 ℃ C. was 400000 cSt); the first filler is copper and polyethylene wax (the phase transition temperature is 56-60 ℃), and the weight ratio of the first filler to the polyethylene wax is 1: 1.8; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2Per g) and graphite oxideAlkene, the weight ratio of which is 1: 15.
100 parts by weight of silicone oil, 24 parts by weight of the first filler and 108 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 3
In the heat conductive silicone grease composition of the present example, the silicone oil was a hydroxyl silicone oil (viscosity at 25 ℃ C. was 250000 cSt); the first filler is zinc oxide and polyethylene glycol (molecular weight is 6000, phase transition temperature is 60-65 ℃), and the weight ratio of the first filler to the second filler is 1: 1.5; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2/g) and graphene oxide in a weight ratio of 1: 6.
100 parts by weight of silicone oil, 35 parts by weight of the first filler and 96 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 4
The components of the thermally conductive silicone grease composition of this example were the same as in example 1.
100 parts by weight of silicone oil, 40 parts by weight of the first filler and 80 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 5
The components of the thermally conductive silicone grease composition of this example were the same as in example 1.
100 parts by weight of silicone oil, 20 parts by weight of the first filler and 120 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 6
The components of the thermally conductive silicone grease composition of this example were the same as in example 1.
100 parts by weight of silicone oil, 10 parts by weight of the first filler and 130 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinder to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 7
The components of the thermally conductive silicone grease composition of this example were the same as in example 1.
100 parts by weight of silicone oil, 50 parts by weight of the first filler and 60 parts by weight of the second filler are mixed and stirred for 30min, and then the mixture is put into a double-roller grinding machine to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Example 8
The heat-conducting silicone grease is prepared according to the method of example 1, except that the first filler is a capsule with the particle size of 50-80 nm formed by wrapping polyethylene glycol with zinc oxide. The thermally conductive silicone grease of this example was prepared according to the method of example 1.
Example 9
The heat-conductive silicone grease composition of the present example is different from example 1 in that the first filler is alumina and liquid paraffin (phase transition temperature is 55-58 ℃) and the weight ratio is 1: 1.2. The thermally conductive silicone grease of this example was prepared according to the method of example 1.
Example 10
The heat-conducting silicone grease composition of the embodiment is different from the embodiment 1 in that the first filler is silver and urea (the phase transition temperature is 50-56 ℃) and the weight ratio is 1: 1.8. The thermally conductive silicone grease of this example was prepared according to the method of example 1.
Example 11
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, sodium hydroxide solution (concentration of 30g/L), polyacrylic acid (weight average molecular weight of 5000), and hexadecyl trimethyl ammonium bromide were mixed in a weight ratio of 1: 1: 0.2: 2.5: 0.2: 0.2, mixing, reacting at 40 ℃ for 2h, and then drying at 120 ℃ for 2h to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 12
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, sodium carbonate solution (the concentration is 60g/L), polyacrylic acid (the weight-average molecular weight is 5000) and triethanolamine are mixed according to the weight ratio of 1: 0.5: 0.5: 1.3: 0.1: 0.4, reacting for 4 hours at 30 ℃, and then drying for 2 hours at 120 ℃ to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 13
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, sodium hydroxide solution (with the concentration of 30g/L), polyacrylic acid (with the weight-average molecular weight of 5000) and hexadecyl trimethyl ammonium bromide are mixed according to the weight ratio of 1: 1.2: 2.5: 0.2: 0.2, mixing, reacting at 40 ℃ for 2h, and then drying at 120 ℃ for 2h to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 14
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, sodium hydroxide solution (concentration of 30g/L), polyacrylic acid (weight average molecular weight of 5000), and hexadecyl trimethyl ammonium bromide were mixed in a weight ratio of 1: 1: 1: 0.2: 0.5: 0.02 mixing, reacting for 2h at 40 ℃, and then drying for 2h at 120 ℃ to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 15
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, sodium hydroxide solution (concentration of 30g/L), polyacrylic acid (weight average molecular weight of 5000), and hexadecyl trimethyl ammonium bromide were mixed in a weight ratio of 1: 0.3: 0.2: 3: 0.05: 1, mixing, reacting at 40 ℃ for 2h, and then drying at 120 ℃ for 2h to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 16
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, sodium hydroxide solution (concentration of 30g/L), polyacrylic acid (weight average molecular weight of 5000), and hexadecyl trimethyl ammonium bromide were mixed in a weight ratio of 1: 1: 0.2: 2.5: 0.2: 0.2, mixing, reacting at 50 ℃ for 1h, and then drying at 120 ℃ for 2h to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 17
The heat conductive silicone grease composition of the present example differs from example 1 in that graphene oxide is modified according to the following method: graphene oxide, tetramethyl orthosilicate, trimethylsiloxy silicate, a sodium hydroxide solution (the concentration is 30g/L), polymaleic anhydride (the weight-average molecular weight is 10000) and hexadecyl trimethyl ammonium bromide are mixed according to the weight ratio of 1: 1: 0.2: 2.5: 0.2: 0.2, mixing, reacting at 40 ℃ for 2h, and then drying at 120 ℃ for 2h to obtain the modified graphene. The modified graphene prepared above is used to replace the graphene oxide in example 1, and the heat conductive silicone grease of this embodiment is prepared according to the method of example 1.
Example 18
In the heat conductive silicone grease composition of the present example, the silicone oil was dimethyl silicone oil (viscosity at 25 ℃ C. was 450000 cSt); the first filler is zinc oxide and polyethylene glycol (molecular weight is 6000, phase transition temperature is 60-65 ℃), and the weight ratio is 1: 1; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2/g) and graphene oxide, whichThe weight ratio is 1: 10; the auxiliary agent is N, N' -diaryl p-phenylenediamine and mineral oil, and the weight ratio of the auxiliary agent to the mineral oil is 1: 0.5.
100 parts by weight of silicone oil, 30 parts by weight of first filler, 100 parts by weight of second filler and 2 parts by weight of auxiliary agent are mixed and stirred for 30min, and then the mixture is placed in a double-roller grinding machine to be ground for 1h, so that the heat-conducting silicone grease prepared in the embodiment is obtained.
Comparative examples 1 to 6 are for explaining heat conductive silicone grease compositions different from the present disclosure and heat conductive silicone greases prepared therefrom.
Comparative example 1
The composition of the heat conductive silicone grease composition of this comparative example was the same as that of example 1, except that 100 parts by weight of silicone oil, 65 parts by weight of the first filler, and 45 parts by weight of the second filler were mixed and stirred for 30min, and then placed in a double roll mill to be ground for 1h, to obtain the heat conductive silicone grease of this comparative example.
Comparative example 2
The composition of the heat conductive silicone grease composition of this comparative example was the same as that of example 1, except that 100 parts by weight of silicone oil, 5 parts by weight of the first filler, and 155 parts by weight of the second filler were mixed and stirred for 30min, and then placed in a double roll mill to be ground for 1h, to obtain the heat conductive silicone grease of this comparative example.
Comparative example 3
In the heat conductive silicone grease composition of the present comparative example, the silicone oil was dimethyl silicone oil (viscosity at 25 ℃ C. was 450000 cSt); the first filler is zinc oxide and polyethylene glycol (molecular weight is 6000, phase transition temperature is 60-65 ℃), and the weight ratio of the first filler to the second filler is 1: 0.1; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2/g) and graphene oxide in a weight ratio of 1: 10.
And mixing and stirring 100 parts by weight of silicone oil, 30 parts by weight of first filler and 100 parts by weight of second filler for 30min, and then placing the mixture in a double-roller grinding machine for grinding for 1h to obtain the heat-conducting silicone grease prepared by the comparative example.
Comparative example 4
In the heat conductive silicone grease composition of the present comparative example, the silicone oil was dimethyl silicone oil (viscosity at 25 ℃ C. was 450000 cSt); the first filler is zinc oxide and polyethylene glycol (molecular weight is 6000, phase transition temperature)The temperature is 60-65 ℃), and the weight ratio is 1: 1.2; the second filler is carbon nano tube (the purity is more than or equal to 95 weight percent, the ash content is less than or equal to 0.2 weight percent, and the specific surface area is 100-200 m2/g) and graphene oxide in a weight ratio of 1: 0.5.
And mixing and stirring 100 parts by weight of silicone oil, 30 parts by weight of first filler and 100 parts by weight of second filler for 30min, and then placing the mixture in a double-roller grinding machine for grinding for 1h to obtain the heat-conducting silicone grease prepared by the comparative example.
Comparative example 5
The thermally conductive silicone grease composition of this comparative example differs from example 1 in that the first filler is zinc oxide throughout. The thermally conductive silicone grease of this comparative example was prepared according to the method of example 1.
Comparative example 6
The thermally conductive silicone grease composition of this comparative example differs from example 1 in that the second filler is entirely graphene oxide. The thermally conductive silicone grease of this comparative example was prepared according to the method of example 1.
Test example 1
The heat conductive greases prepared in examples 1 to 18 and comparative examples 1 to 6 were tested for thermal conductivity and thermal resistance values in accordance with ASTM D5470, and the test results are shown in Table 1.
TABLE 1
As can be seen from table 1, the thermally conductive silicone grease prepared using the composition of the present disclosure has a higher thermal conductivity and a lower thermal resistance. As can be seen from comparison of examples 1 to 3 and examples 4 to 5, when R is 6.5 to 35.5 calculated from 0.656w (second filler) -1.581w (first filler) +0.11w (auxiliary), it is advantageous to further increase the thermal conductivity of the thermal grease and to reduce the thermal resistance thereof. As can be seen from comparison between examples 1 to 3 and examples 6 to 7, when the first filler is contained in an amount of 20 to 40 parts by weight, the second filler is contained in an amount of 80 to 120 parts by weight, and the auxiliary is contained in an amount of 0 to 10 parts by weight, based on 100 parts by weight of the silicone oil, it is advantageous to further increase the thermal conductivity of the heat conductive silicone grease and reduce the thermal resistance thereof. As can be seen from comparison between example 1 and examples 11 to 17, when the modified graphene obtained by the specific method is used, it is advantageous to further increase the thermal conductivity of the thermal grease and reduce the thermal resistance thereof.
Test example 2
The thermally conductive silicone greases prepared in examples 1-18 and comparative examples 1-6 were tested for effectiveness in LED heat dissipation applications. Test objects: the LED chip with power of 30W is provided with a sunflower heat sink with power of 25W. The heat conductive silicone greases prepared in examples 1 to 18 were coated between the LED chips and the radiator fins, respectively, with a coating thickness of 0.06mm, the power supply was started, the temperatures of the LED chips and the fins were measured within 20 minutes (every 2 minutes) of the coating of the heat conductive silicone grease at room temperature (20 ℃), and the temperature difference was calculated. The test results are shown in Table 2.
TABLE 2
As can be seen from table 2, the heat conductive silicone grease of the present disclosure has a high heat conductive rate and a good heat dissipation efficiency. In particular, as can be seen from the comparison between example 1 and example 2, when the phase change material is polyethylene wax and the metal heat conductor is further copper, better heat absorption rate and heat transfer effect are advantageously obtained. As can be seen from the comparison between example 1 and example 8, when the first filler is a capsule formed by wrapping the phase change material with the metal heat conductor, better heat absorption rate and heat transfer effect are obtained.
The preferred embodiments of the present disclosure have been described in detail above, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all fall within the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (10)
1. The heat-conducting silicone grease composition is characterized by comprising 20-40 parts by weight of silicone oil, 80-120 parts by weight of first filler, 80-120 parts by weight of second filler and 0-10 parts by weight of optional auxiliary agent, wherein 100 parts by weight of the silicone oil is taken as a reference; the first filler comprises a metal heat conductor and a phase-change material, and the weight ratio of the metal heat conductor to the phase-change material is 1: (0.2 to 2.5); the second filler is carbon nano tube and graphene, and the weight ratio of the carbon nano tube to the graphene is 1: (1-20); the graphene is modified graphene, and the modified graphene is obtained by mixing graphene oxide, silicate ester, an inorganic alkali solution, a water-soluble high molecular compound and a surfactant, reacting at 10-50 ℃ for 0.1-10 h, and drying;
r is 6.5 to 35.5 calculated by the following formula:
r ═ 0.656w (second filler) -1.581w (first filler) +0.11w (adjuvant),
wherein w (first filler) represents parts by weight of the first filler relative to 100 parts by weight of the silicone oil,
w (second filler) represents parts by weight of the second filler relative to 100 parts by weight of the silicone oil,
w (adjuvant) represents the parts by weight of adjuvant with respect to 100 parts by weight of silicone oil.
2. The composition according to claim 1, wherein the metal thermal conductor is at least one selected from the group consisting of a metal, a metal oxide, a metal carbide and a metal nitride, and the metal in the metal thermal conductor is at least one selected from the group consisting of platinum, silver, copper, aluminum, tin, zinc, calcium, lanthanum, yttrium and cerium;
the phase-change temperature of the phase-change material is 20-80 ℃, the phase-change material is at least one selected from paraffin, polyethylene glycol, stearic acid and urea, and the paraffin is at least one selected from microcrystalline wax, liquid paraffin, polyethylene wax and semi-refined paraffin;
the first filler is a capsule formed by wrapping the phase change material with the metal heat conductor, and the particle size of the capsule is 1-100 nm.
3. The composition of claim 2, wherein the phase change material is polyethylene glycol, the metal thermal conductor is zinc oxide, and the weight ratio of the zinc oxide to the polyethylene glycol is 1: (1-1.5).
4. The composition of claim 2, wherein the phase change material is a polyethylene wax, the metal heat conductor is copper, and the weight ratio of copper to polyethylene wax is 1: (1.5-2).
5. The composition according to claim 1, wherein the graphene has an average particle size of 0.1-20 μm.
6. The composition according to claim 1, wherein the weight ratio of the graphene oxide, the organosilicate, the inorganic alkali solution, the water-soluble high molecular compound, and the surfactant is 1: (0.5-6): (0.1-10): (0.02-0.5): (0.02-1).
7. The composition of claim 6, wherein the silicate is tetramethyl orthosilicate and trimethylsiloxysilicate in a weight ratio of 1: (0.1 to 1);
the concentration of the inorganic alkali solution is 30-100 g/L, and the inorganic alkali solution is at least one selected from a sodium hydroxide solution, a potassium hydroxide solution, a calcium hydroxide solution, a sodium carbonate solution, a sodium bicarbonate solution and a potassium carbonate solution;
the water-soluble high molecular compound is polyacrylic acid, and the weight-average molecular weight of the polyacrylic acid is 5000-20000;
the surfactant is at least one selected from triethanolamine, cetyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide, dodecyl aminopropionic acid, methyl acrylate and alkyl dimethyl hydroxypropyl phosphate betaine.
8. The composition as claimed in claim 1, wherein the carbon nanotubes have a purity of not less than 95% by weight, an ash content of not more than 0.2% by weight, and a specific surface area of 40 to 300m2/g；
The viscosity of the silicone oil at 25 ℃ is 50000-500000 cSt;
the auxiliary agent is at least one selected from an antioxidant, a corrosion inhibitor, an antiwear agent and a lubrication improver.
9. A heat conductive silicone grease prepared from the composition of any one of claims 1-8, wherein the heat conductive silicone grease has a thermal conductivity of 4.5-8W/m-K and a thermal resistance of 5.8 × 10-6-1.1×10-5K·m2/W。
10. An LED lighting device comprising an LED light source and a heat sink assembly connected together, wherein the heat sink assembly comprises the thermally conductive silicone grease of claim 9.
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| CN201810130161.0A CN108373592B (en) | 2018-02-08 | 2018-02-08 | Heat-conducting silicone grease composition, heat-conducting silicone grease and LED lighting device |
| US16/968,744 US11312630B2 (en) | 2018-02-08 | 2018-11-26 | Modification method for graphene, modified graphene, and composition containing graphene |
| KR1020207025846A KR102404243B1 (en) | 2018-02-08 | 2018-11-26 | Method for modifying graphene, modified graphene and composition comprising graphene |
| JP2020564989A JP7043630B2 (en) | 2018-02-08 | 2018-11-26 | Graphene denaturing method, modified graphene and composition containing graphene |
| PCT/CN2018/117496 WO2019153842A1 (en) | 2018-02-08 | 2018-11-26 | Modification method for graphene, modified graphene, and composition containing graphene |
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| CN109307254A (en) * | 2018-11-27 | 2019-02-05 | 湖州明朔光电科技有限公司 | A kind of illumination heat radiator and the light fixture using it |
| CN109913183A (en) * | 2019-04-12 | 2019-06-21 | 哈尔滨理工大学 | A kind of insulating heat-conductive preparation of sections method with phase-change characteristic |
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| CN110591365A (en) * | 2019-09-29 | 2019-12-20 | 太仓陶氏电气有限公司 | High-thermal-conductivity nano silicone grease for heat dissipation of semiconductor chip |
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| CN102634212B (en) * | 2012-04-23 | 2015-11-25 | 湖州明朔光电科技有限公司 | A kind of heat conductive silicone grease composition |
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Application publication date: 20180807 Assignee: Hunan Lanxin Microelectronics Technology Co.,Ltd. Assignor: DONGXU OPTOELECTRONIC TECHNOLOGY Co.,Ltd. Contract record no.: X2023110000110 Denomination of invention: Thermal conductive silicone grease composition and thermal conductive silicone grease, as well as LED lighting equipment Granted publication date: 20201013 License type: Common License Record date: 20230905 |