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Carbon nanotube/zinc oxide/micro-expansion graphite composite heat-conducting silicone grease and preparation method thereof

A technology of micro-expanded graphite and thermally conductive silicone grease, which is applied in the field of carbon nanotube/zinc oxide/micro-expanded graphite composite thermally conductive silicone grease and its preparation, and achieves the effects of good compatibility, excellent thermal stability and good interface contact.

Inactive Publication Date: 2018-02-23
郴州国盛新材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no research on the application of micro-expanded graphite in thermally conductive silicone grease materials in the prior art. How to apply micro-expanded graphite in thermally conductive silicone grease materials and exert its excellent thermal conductivity, softness, resilience and plasticity is worthy of our attention. research

Method used

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  • Carbon nanotube/zinc oxide/micro-expansion graphite composite heat-conducting silicone grease and preparation method thereof
  • Carbon nanotube/zinc oxide/micro-expansion graphite composite heat-conducting silicone grease and preparation method thereof

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Experimental program
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Embodiment 1

[0037] The present embodiment provides a kind of preparation method of micro-expanded graphite material, comprises the following steps::

[0038] S11. Get the microcrystalline graphite raw material with carbon content of 70% and the flake graphite raw material with carbon content of 85%, the mass ratio of flake graphite and microcrystalline graphite is 2:1, crushing and grinding, until particle size is 300 purpose mixed graphite powder;

[0039] S12. Place the mixture obtained in S11 in a muffle furnace, slowly heat up to 350° C. under a nitrogen atmosphere, keep it warm for 30 minutes, and air-cool to room temperature for use;

[0040] S13. Perform chemical intercalation treatment on the mixture after S12 heat treatment to obtain expandable mixed graphite, wherein the specific steps of chemical intercalation treatment are as follows: S131. Mix perchloric acid and microcrystalline graphite powder at a liquid-solid ratio of 10:1L / Kg mix and stir evenly; S132. Add strong oxidan...

Embodiment 2

[0043] This embodiment provides a method for preparing a carbon nanotube / micro-expanded graphite composite material, comprising the following steps:

[0044]Using the micro-expanded graphite prepared in Example 1 as a raw material, immerse the micro-expanded graphite in a 0.1mol / L ferric nitrate aqueous solution, filter after ultrasonic vibration for 2 hours, then vacuum-dry at 90°C for 10 hours, and place the dried material in In a tube furnace, the temperature was raised to 700°C under a nitrogen atmosphere, and then C2H2 gas was introduced, kept for 40 minutes, and then cooled to room temperature under a nitrogen atmosphere to obtain a carbon nanotube / micro-expanded graphite composite material.

Embodiment 3

[0046] This embodiment provides a method for preparing a carbon nanotube / zinc oxide / micro-expanded graphite composite heat-conducting silicone grease, using the carbon nanotube / micro-expanded graphite composite material in Example 2, and the specific steps are as follows:

[0047] S1. Accurately weigh 35 parts of carbon nanotube / micro-expanded graphite composite material and 5 parts of zinc oxide of 0.5~2um, then mix evenly by high-speed mixer at 1800r / min for 10min, and set aside;

[0048] S2. Take 400 parts of absolute ethanol and put it into the reaction kettle, take 3% coupling agent of thermally conductive filler and add it into the reaction kettle, and stir at a constant temperature of 60°C and 100r / min for 10min to obtain an ethanol solution;

[0049] S3. Add the heat-conducting filler in step S1 into the ethanol solution, stir ultrasonically for 2 hours, and wait until the ethanol is completely evaporated to obtain a modified compound heat-conducting filler;

[0050] S...

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Abstract

The invention discloses carbon nanotube / zinc oxide / micro-expansion graphite composite heat-conducting silicone grease and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing a carbon nanotube / micro-expansion graphite composite material with zinc oxide by virtue of a high-speed mixing machine, adding the mixture into an ethanol solution, and carryingout ultrasonic stirring until ethanol is completely evaporated, so as to obtain a heat-conducting filling; and adding the heat-conducting filling, silicone oil, a crosslinking agent, a silane surfactant and an antioxidant into an internal mixer, carrying out internal mixing, so as to obtain the composite heat-conducting silicone grease. According to the preparation method, microcrystalline graphite and crystalline flake graphite are mixed to form a micro-expansion graphite material, settling carbon nanotubes to the surface of micro-expansion graphite and into hole structures by virtue of a CVD sedimentation method, the prepared carbon nanotube / micro-expansion graphite composite material is taken as the heat-conducting filling, the heat-conducting filling is modified by virtue of a coupling agent, has good consistency with silicone oil, does not agglomerate and further has good interface contact property. The prepared heat-conducting silicone grease has excellent thermal stability, islow in oil separation value and does not crack and atomize after being used for a long time.

Description

technical field [0001] The invention relates to a carbon nanotube / zinc oxide / micro-expanded graphite composite heat-conducting silicone grease and a preparation method thereof, which are mainly applicable to the fields of high-power electric appliance packaging and heat dissipation. Background technique [0002] Thermally conductive silicone grease is a kind of high thermal conductive silicone material, which can maintain the paste shape for a long time at the temperature of -50~300°C. It is widely used between the heating element and the heat dissipation base of high-power electronic components, effectively reducing the interface contact heat. resistance. With the development of high-power and intensive electronic components, there is an increasing demand for high-performance thermally conductive silicone grease with high thermal conductivity, excellent thermal stability, and low oil separation value. [0003] Micro-expanded graphite is a kind of graphite interlayer compou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/04C08L83/05C08K13/06C08K9/06C08K7/24C08K3/22C08K5/14C08K7/00C08K9/12C09K5/14
CPCC08K2003/2296C08K2201/011C08K2201/014C08L83/04C08L2205/025C08L2205/035C09K5/14C08K13/06C08K9/06C08K7/24C08K3/22C08K5/14C08K7/00C08K9/12
Inventor 李丽萍
Owner 郴州国盛新材科技有限公司
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