CN115594977A - Graphene heat-conducting silicone grease for high-power LED and preparation method thereof - Google Patents
Graphene heat-conducting silicone grease for high-power LED and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 101
- 239000004519 grease Substances 0.000 title claims abstract description 95
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 239000007822 coupling agent Substances 0.000 claims abstract description 7
- 239000000080 wetting agent Substances 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- RUQIYMSRQQCKIK-UHFFFAOYSA-M sodium;2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 RUQIYMSRQQCKIK-UHFFFAOYSA-M 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 4
- AXTGDCSMTYGJND-UHFFFAOYSA-N 1-dodecylazepan-2-one Chemical compound CCCCCCCCCCCCN1CCCCCC1=O AXTGDCSMTYGJND-UHFFFAOYSA-N 0.000 claims description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229940083037 simethicone Drugs 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 6
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 230000017525 heat dissipation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a graphene heat-conducting silicone grease for a high-power LED and a preparation method thereof, belonging to the technical field of heat-conducting silicone grease, and specifically comprising the following raw materials in parts by weight: 15-60 parts of component A and 41-87 parts of component B; wherein the component A comprises the following raw materials in parts by weight: 1-3 parts of activated graphene, 0.1-1 part of ammonia water, 1-3 parts of a coupling agent and 100-300 parts of ethanol; the component B comprises the following raw materials in parts by weight: 40-85 parts of dimethyl silicone oil and 1-2 parts of wetting agent. Meanwhile, the invention also discloses the following preparation method: carrying out drying and activating treatment on graphene before adding heat-conducting silicone grease, taking the heat-conducting silicone grease as a base material, and adding and uniformly dispersing activated graphene powder into the heat-conducting silicone grease in a vacuum stirring manner to form the graphene heat-conducting silicone grease. The graphene heat-conducting silicone grease prepared by the invention has good stability, and the service life and the heat-conducting property are both remarkably improved.
Description
Technical Field
The invention relates to the technical field of heat-conducting silicone grease, in particular to graphene heat-conducting silicone grease for a high-power LED and a preparation method thereof.
Background
The heat-conducting silicone grease is a paste-shaped thermal interface heat-conducting material, can be used for heat dissipation of heating or heat dissipation elements, has good heat-conducting property, and is often applied to the fields of electronic products and the like. The heat-dissipating device can be applied to quickly releasing heat generated when electronic products are used, and can also be applied to parts needing heat dissipation, heat transfer or insulation in the fields of aerospace, electronics and electricity and the like; the heat dissipation device can timely remove a large amount of heat generated in the use process of electronic equipment, and has important effects on the aspects of densification, miniaturization, reliability, precision, service life and the like of electronic products. The heat-conducting silicone grease has good fluidity and can fill the gap, thereby ensuring the close contact between the electronic element and the radiating fin, increasing the contact area, improving the heat transfer efficiency, further quickly and uniformly transferring the heat generated by the heating element during the work to the radiating fin to the maximum extent, and ensuring the best radiating effect. The performance of the heat-conducting silicone grease has great influence on the heat dissipation performance of the electronic element, and the graphene has excellent thermal stability, weather resistance, aging resistance, mechanical strength and the like, so that the graphene is added into the silicone grease, and the heat-conducting heat dissipation performance of the product is theoretically improved.
However, in the prior art, the used graphene is directly loaded in the heat-conducting silicone grease as the heat-conducting filler, the graphene in the heat-conducting silicone grease is agglomerated, and the graphene cannot be uniformly dispersed, so that the heat-conducting uniformity of the heat-conducting silicone grease is affected. Meanwhile, the compatibility between the graphene and the heat-conducting silicone grease is poor, so that the improvement of the heat-conducting performance of the heat-conducting silicone grease is not facilitated.
Therefore, how to provide a graphene thermal silicone grease with uniform dispersion is an urgent problem to be solved by those skilled in the art.
Disclosure of Invention
In view of this, the invention provides the graphene thermal conductive silicone grease which is uniformly dispersed and has good thermal conductivity and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the graphene heat-conducting silicone grease for the high-power LED comprises the following raw materials in parts by weight:
15-60 parts of component A and 41-87 parts of component B;
wherein the content of the first and second substances,
the component A comprises the following raw materials in parts by weight: 1-3 parts of activated graphene, 0.1-1 part of ammonia water, 1-3 parts of a coupling agent and 100-300 parts of ethanol;
the component B comprises the following raw materials in parts by weight: 40-85 parts of dimethyl silicone oil and 1-2 parts of wetting agent.
Preferably, the mass concentration of the ammonia water is 28%; the viscosity of the simethicone is 300-1000cps.
Preferably, the coupling agent is one of y-aminopropyltriethoxysilane, y-glycidoxypropyltrimethoxysilane, y-methacryloxypropyltrimethoxysilane or y-aminopropyltriethoxysilane.
Preferably, the wetting agent is one of sodium diisopropylnaphthalenesulfonate, 1-n-dodecylazacycloheptane-2-one, polyoxyethylene sorbitan monooleate or nonylphenol polyoxyethylene.
Has the advantages that: due to the addition of the graphene, the heat conduction effect of the silicone grease is greatly improved.
A preparation method of graphene heat-conducting silicone grease for a high-power LED comprises the following steps:
(1) Carrying out vacuum drying on graphene at 65-90 ℃ for 1-2 h to remove residual moisture in the graphene and activate the graphene to obtain activated graphene;
(2) The raw materials are weighed according to the graphene heat-conducting silicone grease for the high-power LED of claim 1 or 2, the activated graphene, the coupling agent and the concentrated ammonia water are sequentially added into ethanol, and then the mixture is stirred for 12-24 hours at normal temperature, filtered and dried to obtain a component A;
(3) Sequentially adding dimethyl silicone oil and a wetting agent into 15-60 parts of the component A at 60-100 ℃, uniformly stirring, and performing ultrasonic treatment for 30-60min to obtain a graphene heat-conducting silicone grease precursor;
(4) Heating and curing the graphene heat-conducting silicone grease precursor for l-2 h in vacuum at constant temperature to obtain a cured graphene heat-conducting silicone grease precursor;
(5) And (3) stirring the cured graphene heat-conducting silicone grease precursor for 12-48h in vacuum to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
Preferably, the graphene in the step (1) is prepared by a liquid-phase ultrasonic exfoliation method.
Has the advantages that: the graphene prepared by the stripping method keeps the characteristics of the graphene and has good improvement on the heat conduction effect.
Preferably, the stirring rate in the step (2) is 100 to 300rmp;
the drying temperature is 80-110 ℃; drying for 10-20min; the water content after drying is 0.01-0.05%.
Preferably, the stirring speed in the step (3) is 300-1000rmp, and the stirring time is 0.5-2h;
the ultrasonic power is 80%.
Has the beneficial effects that: under the conditions, the graphene heat-conducting silicone grease precursor can be uniformly mixed preliminarily.
Preferably, the curing temperature in the step (4) is 120-180 ℃, and the vacuum degree is-0.1 Mpa.
Preferably, the vacuum degree of the vacuum stirring in the step (5) is-0.1 Mpa, and the stirring speed is 800-1500rpm.
According to the technical scheme, compared with the prior art, the graphene heat-conducting silicone grease for the high-power LED and the preparation method thereof are disclosed. Meanwhile, the heat-conducting performance of the heat-conducting silicone grease can be greatly improved by adding a small amount of graphene powder, and the performance and the value of the heat-conducting silicone grease are improved. In addition, the graphene heat-conducting silicone grease provided by the invention is simple in preparation process, can be directly added on the basis of the existing heat-conducting silicone grease finished product, is convenient to operate, is low in cost, and has a wide market prospect.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the standard of thermal conductivity testing is the Heat flow method ASTM D5470-2017.
Example 1
A preparation method of graphene heat-conducting silicone grease for a high-power LED comprises the following steps:
(1) Placing graphene powder prepared by a liquid-phase ultrasonic stripping method in a vacuum oven at 80 ℃, and performing vacuum drying for 2h to remove residual moisture in graphene and activate the graphene to obtain activated graphene;
(2) Weighing 1 part of activated graphene and 1 part of Y-aminopropyltriethoxysilane, sequentially adding the activated graphene and the Y-aminopropyltriethoxysilane into 100 parts of ethanol, then adding 0.1 part of 28% concentrated ammonia water, stirring for 12 hours at normal temperature and 100rmp of rotation speed, and performing suction filtration and drying to obtain a component A;
(3) Sequentially adding 15 parts of the component A and 1 part of sodium diisopropylnaphthalene sulfonate into 85 parts of dimethyl silicone oil with the viscosity of 300cpm at 60 ℃, stirring for 0.5h at the rotating speed of 300rmp, and performing ultrasonic treatment for 30min to obtain a graphene heat-conducting silicone grease precursor;
(4) Placing the graphene heat-conducting silicone grease precursor obtained in the step (3) in a constant-temperature vacuum oven with the temperature of 150 ℃ and the vacuum degree of-0.1 Mpa, heating for 2h, and curing the graphene heat-conducting silicone grease precursor;
(5) And (5) placing the cured graphene heat-conducting silicone grease precursor in the step (4) in a vacuum stirrer with the vacuum degree of-0.1 Mpa, and continuously stirring for 24 hours at the rotating speed of 1000r/min to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
The heat conductivity coefficient of the graphene heat-conducting silicone grease for the high-power LED prepared by the embodiment is 5W/m.K, the graphene heat-conducting silicone grease is aged for 1000 hours at 200 ℃, and the viscosity of the graphene heat-conducting silicone grease changes by V10%.
Example 2
A preparation method of graphene heat-conducting silicone grease for a high-power LED comprises the following steps:
(1) Placing graphene powder prepared by a liquid-phase ultrasonic stripping method in a vacuum oven at 80 ℃, and carrying out vacuum drying for 2h to remove residual moisture in graphene and activate the graphene to obtain activated graphene;
(2) Weighing 2 parts of activated graphene and 2 parts of y-aminopropyltriethoxysilane, adding the activated graphene and 2 parts of y-aminopropyltriethoxysilane into 200 parts of ethanol, adding 0.5 part of 28% concentrated ammonia water, stirring at normal temperature and 200rmp of rotation speed for 18 hours, and performing suction filtration and drying to obtain a component A;
(3) Adding 30 parts of the component A and 1.5 parts of sodium diisopropylnaphthalenesulfonate into 70 parts of dimethyl silicone oil with the viscosity of 650cpm at the temperature of 80 ℃, stirring for 1h at the rotating speed of 650rmp, and performing ultrasonic treatment for 45min to obtain a graphene heat-conducting silicone grease precursor;
(4) Placing the graphene heat-conducting silicone grease precursor obtained in the step (3) in a constant-temperature vacuum oven with the temperature of 150 ℃ and the vacuum degree of-0.1 Mpa, heating for 2 hours, and curing the graphene heat-conducting silicone grease precursor;
(5) And (5) placing the cured graphene heat-conducting silicone grease precursor in the step (4) in a vacuum stirrer with the vacuum degree of-0.1 Mpa, and continuously stirring for 24 hours at the rotating speed of 1000r/min to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
The heat conductivity coefficient of the graphene heat-conducting silicone grease for the high-power LED prepared by the embodiment is 8W/m.K, the graphene heat-conducting silicone grease is aged for 1000 hours at 200 ℃, and the viscosity of the graphene heat-conducting silicone grease is changed by V7%.
Example 3
A preparation method of graphene heat-conducting silicone grease for a high-power LED comprises the following steps:
(1) Placing graphene powder prepared by a liquid-phase ultrasonic stripping method in a vacuum oven at 80 ℃, and carrying out vacuum drying for 2h to remove residual moisture in graphene and activate the graphene to obtain activated graphene;
(2) Weighing 2.5 parts of activated graphene and 3 parts of y-aminopropyltriethoxysilane, adding the activated graphene and 3 parts of y-aminopropyltriethoxysilane into 300 parts of ethanol, adding 1 part of 28% concentrated ammonia water, stirring for 24 hours at normal temperature and 300rmp of rotation speed, performing suction filtration, and drying to obtain a component A;
(3) Sequentially adding 60 parts of the component A and 2 parts of sodium diisopropylnaphthalene sulfonate into 40 parts of dimethyl silicone oil with viscosity of 1000cpm at 100 ℃, stirring for 2h at the rotating speed of 1000rmp, and performing ultrasonic treatment for 60min to obtain a graphene heat-conducting silicone grease precursor;
(4) Placing the graphene heat-conducting silicone grease precursor obtained in the step (3) in a constant-temperature vacuum oven with the temperature of 150 ℃ and the vacuum degree of-0.1 Mpa, heating for 2h, and curing the graphene heat-conducting silicone grease precursor;
(5) And (3) placing the cured graphene heat-conducting silicone grease precursor in the step (4) in a vacuum stirrer with the vacuum degree of-0.1 Mpa, and continuously stirring for 24 hours at the rotating speed of 1000r/min to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
The thermal conductivity coefficient of the graphene thermal-conductive silicone grease prepared in the embodiment is 10W/m.K, and the viscosity of the graphene thermal-conductive silicone grease is changed by V5% after the graphene thermal-conductive silicone grease is aged for 1000 hours at 200 ℃.
Example 4
A preparation method of graphene heat-conducting silicone grease for a high-power LED comprises the following steps:
(1) Placing graphene powder prepared by a liquid-phase ultrasonic stripping method in a vacuum oven at 80 ℃, and performing vacuum drying for 2h to remove residual moisture in graphene and activate the graphene to obtain activated graphene;
(2) Weighing 0.5 part of activated graphene and 1 g of y-glycidoxypropyltrimethoxysilane, adding the activated graphene and the y-glycidoxypropyltrimethoxysilane into 100 parts of ethanol, adding 0.1 part of 28% concentrated ammonia water, stirring at normal temperature and 100rmp of rotation speed for 12 hours, and performing suction filtration and drying to obtain a component A;
(3) At 60 ℃, sequentially adding 15 parts of the component A and 1 part of 1-n-dodecyl azacycloheptane-2-ketone into 85 parts of dimethyl silicone oil with the viscosity of 300cpm, stirring at the rotating speed of 300rmp for 0.5h, and performing ultrasonic treatment for 30min to obtain a graphene heat-conducting silicone grease precursor;
(4) Placing the graphene heat-conducting silicone grease precursor obtained in the step (3) in a constant-temperature vacuum oven with the temperature of 150 ℃ and the vacuum degree of-0.1 Mpa, heating for 2 hours, and curing the graphene heat-conducting silicone grease precursor;
(5) And (3) placing the cured graphene heat-conducting silicone grease precursor in the step (4) in a vacuum stirrer with the vacuum degree of-0.1 Mpa, and continuously stirring for 24 hours at the rotating speed of 1000r/min to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
The thermal conductivity coefficient of the graphene thermal-conductive silicone grease prepared in the embodiment is 4.5W/m.K, the graphene thermal-conductive silicone grease is aged for 1000 hours at 200 ℃, and the viscosity of the graphene thermal-conductive silicone grease changes by V15%.
Comparative example 1
A preparation method of graphene heat-conducting silicone grease comprises the following steps:
(1) Weighing 1 g of y-glycidol oxygen-wake propyl trimethoxy silane, adding the y-glycidol oxygen-wake propyl trimethoxy silane into 100 parts of ethanol, adding 0.1 part of 28% concentrated ammonia water, stirring for 12 hours at normal temperature and 100rmp of rotation speed, and performing suction filtration and drying to obtain a component A;
(3) At 60 ℃, sequentially adding 15 parts of the component A and 1 part of 1-n-dodecyl azacyclo heptane-2-ketone into 85 parts of dimethyl silicone oil with the viscosity of 300cpm, stirring for 0.5h at the rotating speed of 300rmp, and performing ultrasonic treatment for 30min to obtain a heat-conducting silicone grease precursor;
(4) Placing the heat-conducting silicone grease precursor obtained in the step (3) in a constant-temperature vacuum oven with the temperature of 150 ℃ and the vacuum degree of-0.1 Mpa, heating for 2 hours, and curing the heat-conducting silicone grease precursor;
(5) And (3) placing the cured heat-conducting silicone grease precursor in the step (4) in a vacuum stirrer with the vacuum degree of-0.1 Mpa, and continuously stirring for 24 hours at the rotating speed of 1000r/min to obtain the heat-conducting silicone grease which is uniformly stirred and stably dispersed.
Table 1 thermal conductivity coefficient of graphene thermal grease
| Sample numbering | Test temperature (. Degree. C.) | Thermal conductivity W/(m.k) |
| Comparative example 1 | 25 | 0.5 |
| Example 1 | 25 | 5 |
| Example 2 | 25 | 8 |
| Example 3 | 25 | 10 |
| Example 4 | 25 | 4.5 |
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The graphene heat-conducting silicone grease for the high-power LED is characterized by comprising the following raw materials in parts by weight:
15-60 parts of component A and 41-87 parts of component B;
wherein the content of the first and second substances,
the component A comprises the following raw materials in parts by weight: 1-3 parts of activated graphene, 0.1-1 part of ammonia water, 1-3 parts of a coupling agent and 100-300 parts of ethanol;
the component B comprises the following raw materials in parts by weight: 40-85 parts of dimethyl silicone oil and 1-2 parts of wetting agent.
2. The graphene heat-conducting silicone grease for the high-power LED as recited in claim 1, wherein the mass concentration of the ammonia water is 28%; the viscosity of the simethicone is 300-1000cps.
3. The graphene thermal silicone grease for the high-power LED as recited in claim 1, wherein the coupling agent is one of y-aminopropyltriethoxysilane, y-glycidoxypropyltrimethoxysilane, y-methacryloxypropyltrimethoxysilane or y-propyltriethoxysilane.
4. The graphene thermal silicone grease as claimed in claim 1, wherein the wetting agent is one of sodium diisopropylnaphthalene sulfonate, 1-n-dodecylazacycloheptane-2-one, polyoxyethylene sorbitan monooleate or nonylphenol polyoxyethylene.
5. A preparation method of graphene heat-conducting silicone grease for a high-power LED is characterized by comprising the following steps:
(1) Carrying out vacuum drying on graphene at 65-90 ℃ for 1-2 h to obtain activated graphene;
(2) Weighing the raw materials according to any one of claims 1 to 4, wherein the raw materials are used for standby;
(3) Sequentially adding the activated graphene, the coupling agent and ammonia water into ethanol, stirring at normal temperature for 12-24 h, carrying out suction filtration, and drying to obtain a component A;
(4) Sequentially adding dimethyl silicone oil and a wetting agent into 15-60 parts of the component A at 60-100 ℃, uniformly stirring, and performing ultrasonic treatment for 30-60min to obtain a graphene heat-conducting silicone grease precursor;
(5) Heating and curing the graphene heat-conducting silicone grease precursor for l-2 h in vacuum at constant temperature to obtain a cured graphene heat-conducting silicone grease precursor;
(6) And (3) stirring the cured graphene heat-conducting silicone grease precursor for 12-48h in vacuum to obtain the graphene heat-conducting silicone grease which is uniformly stirred and stably dispersed.
6. The preparation method of the graphene heat-conducting silicone grease for the high-power LED according to claim 5, wherein the graphene in the step (1) is prepared by a liquid-phase ultrasonic stripping method.
7. The preparation method of the graphene thermal silicone grease for the high-power LED according to claim 5, wherein in the step (3), the stirring rate is 100-300rmp;
the drying temperature is 80-110 ℃; drying for 10-20min; the water content after drying is 0.01-0.05%.
8. The preparation method of the graphene heat-conducting silicone grease for the high-power LED according to claim 5, wherein in the step (4), the stirring speed is 300-1000rmp, and the stirring time is 0.5-2h;
the ultrasonic power is 80%.
9. The method for preparing graphene heat-conducting silicone grease for high-power LEDs according to claim 5, wherein in the step (5), the curing temperature is 120-180 ℃ and the vacuum degree is-0.1 Mpa.
10. The preparation method of the graphene heat-conducting silicone grease for the high-power LED according to claim 5, wherein the vacuum degree of stirring in the step (6) is-0.1 Mpa, and the stirring speed is 800-1500rpm.
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