CN112708169A - Process for preparing high-orientation graphene oxide-based high-thermal-conductivity composite resin by freeze-drying method - Google Patents
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Abstract
The invention discloses a process for preparing high-orientation graphene oxide-based high-thermal-conductivity composite resin by a freeze-drying method, which relates to the field of new materials and comprises the following steps: firstly, preparing a graphene mixed solution, dispersing particle heat conduction fillers in carbon fibers and graphene gaps inside the mixed solution, stirring to prepare a dispersion solution, then placing the dispersion solution in a drying oven for evaporation and concentration to a colloid state, placing the colloid containing the particle heat conduction fillers in the graphene and graphene gaps in an ultra-flat evaporation dish, placing the evaporation dish in freeze drying equipment, setting parameters to obtain particles of the vertically oriented graphene and graphene gaps, and then annealing the particles in a nitrogen atmosphere to obtain a final product. The process for preparing the high-thermal conductivity composite resin with the high-orientation graphene oxide base by the freeze-drying method can greatly improve the thermal conductivity coefficient of the composite resin and improve the thermal conductivity of the composite resin.
Description
Technical Field
The invention relates to the field of new materials, in particular to a process for preparing high-orientation graphene oxide-based high-thermal-conductivity composite resin by a freeze-drying method.
Background
The chip, the 5G communication base station, the new energy automobile electric core and the like are all high-heating components, and whether heat can be quickly led out determines the working performance and reliability of the equipment. Since the rough surface of the component results in limited electrical contact at the interface between the heat source and the heat sink, the heat sink area is very small, and air is a poor conductor of heat, a thermal interface resin material is required to effectively close the interface voids and form a good thermal conduction path.
The current preparation technology of heat-conducting resin is prepared by doping various particle powders, such as aluminum oxide, aluminum nitride, boron nitride and the like, in resin. Because the powder particles are also in point contact and an effective passage is difficult to form, even if more than 90% of powder is doped, the thermal conductivity coefficient of the composite resin is still not ideal, and therefore, a process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by a freeze-drying method is designed to solve the problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a process for preparing a high-orientation graphene oxide-based high-thermal-conductivity composite resin by a freeze-drying method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps:
s1, firstly, preparing a graphene mixed solution, then dispersing carbon fibers and particle heat-conducting fillers in gaps of graphene in the mixed solution, and stirring to obtain a dispersion liquid;
s2, putting the dispersion liquid into an oven to evaporate and concentrate the dispersion liquid to a colloid state;
s3, placing colloid containing the graphene and the particle heat-conducting filler with the graphene gaps in an ultra-flat evaporating dish, placing the evaporating dish in freeze drying equipment, and setting parameters to obtain the particle heat-conducting filler sheets with the vertically-oriented graphene and the graphene gaps;
s4, annealing the substances in a nitrogen atmosphere to obtain a final product, and testing the thermal conductivity coefficient of the composite resin in a thermal resistance instrument;
preferably, the graphene mixed solution in S1 may be water, ethanol, isopropanol, n-propanol, acetone, acetonitrile, and a multi-component mixture, and the ratio thereof is 1: 1.
preferably, the graphene mixed solution in S1 is prepared by stirring water, ethanol, isopropanol, n-propanol, acetone, acetonitrile, and a multi-component mixture for 1 to 3 hours.
Preferably, the number of graphene layers is 1-100, and the graphene is oxidized graphene with an oxidized functional group on the surface.
Preferably, the particulate thermal conductive filler in the graphene voids in S1 is one or more of aluminum oxide, aluminum nitride, boron nitride, silicon carbide, metal nanoparticles, boron nitride nanosheets, and graphene nanosheets.
Preferably, the freeze-drying device parameters in S3 are set to a freezing temperature of-10 ℃ to-200 ℃ and a freezing time of 1h to 48 h.
Preferably, the annealing temperature in S4 is 200-400 ℃, and the annealing time is 0.5-1.5 h.
Preferably, the parameters of the thermal resistance instrument in S4 are set to be the cold electrode temperature of 10-30 ℃, the hot electrode temperature of 70-90 ℃ and the pressure of 40-60N.
The invention has the beneficial effects that:
the invention provides a process for preparing high-orientation graphene oxide-based high-thermal-conductivity composite resin by a freeze-drying method, which aims at solving the problems in the background art and adopts two-dimensional graphene oxide and granular thermal conductive powder such as aluminum oxide and aluminum nitride as fillers, a vertical thermal conductive path is formed by controlling structural orientation, so that the thermal conductivity can be greatly improved, and the two-dimensional graphene and granules form more contact points to further promote thermal conductivity and improve the thermal conductivity.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example one
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: firstly, 1g of carbon fiber and 0.5g of alumina are prepared and dispersed in 50ml of water-ethanol mixed solution, the ratio of water to ethanol is 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and alumina in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, and the freezing temperature of the freezing drying equipment is set to be-10 ℃, the freezing time is set to be 1h, the graphene aluminum oxide sheet with vertical orientation is obtained, and then placing the composite resin in a nitrogen atmosphere to anneal for 0.5h at 200 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is set to be 20 ℃, the hot electrode temperature is set to be 80 ℃, and the pressure is set to be 50N.
Example two
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: firstly, 1g of carbon fiber and 0.5g of boron nitride are prepared and dispersed in 50ml of mixed solution of isopropanol and ethanol, the ratio of the isopropanol to the ethanol is 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and boron nitride in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, setting the freezing temperature of the freezing drying equipment to be-10 ℃ and the freezing time to be 1h to obtain the graphene boron nitride sheet with vertical orientation, and then placing the composite resin in a nitrogen atmosphere to anneal for 0.5h at 200 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is set to be 20 ℃, the hot electrode temperature is set to be 80 ℃, and the pressure is set to be 50N.
EXAMPLE III
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: firstly, 1g of carbon fiber and 0.5g of alumina are prepared and dispersed in 50ml of water-ethanol mixed solution, the ratio of water to ethanol is 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and alumina in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, and the freezing temperature of the freezing drying equipment is set to be-40 ℃, the freezing time is set to be 12h, the graphene aluminum oxide sheet with vertical orientation is obtained, and then placing the composite resin in a nitrogen atmosphere to anneal for 1h at 300 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is 20 ℃, the hot electrode temperature is 80 ℃ and the pressure is 50N.
Example four
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: 2g of carbon fiber and 1g of alumina are prepared, dispersed in 100ml of a mixed solution of water and ethanol in a ratio of 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and alumina in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, and the freezing temperature of the freezing drying equipment is set to be-40 ℃, the freezing time is set to be 12h, the graphene aluminum oxide sheet with vertical orientation is obtained, and then placing the composite resin in a nitrogen atmosphere to anneal for 1h at 300 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is 20 ℃, the hot electrode temperature is 80 ℃ and the pressure is 50N.
EXAMPLE five
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: firstly, 1g of carbon fiber and 0.5g of alumina are prepared and dispersed in 50ml of water-ethanol mixed solution, the ratio of water to ethanol is 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and alumina in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, and the freezing temperature of the freezing drying equipment is set to be-40 ℃, the freezing time is set to be 12h, the graphene aluminum oxide sheet with vertical orientation is obtained, and then placing the composite resin in a nitrogen atmosphere to anneal for 0.5h at 200 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is set to be 20 ℃, the hot electrode temperature is set to be 80 ℃, and the pressure is set to be 50N.
EXAMPLE six
The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method comprises the following steps: firstly, 1g of carbon fiber and 0.5g of alumina are prepared and dispersed in 50ml of water-ethanol mixed solution, the ratio of water to ethanol is 1:1, then stirring for 1h to obtain a dispersion, putting the dispersion in an oven for evaporation and concentration until the dispersion is in a colloidal state and has a mass of 5g, then placing the glue containing graphene and alumina in an ultra-flat evaporation dish, then placing the evaporation dish in a freezing drying device, and the freezing temperature of the freezing drying equipment is set to be-10 ℃, the freezing time is set to be 1h, the graphene aluminum oxide sheet with vertical orientation is obtained, and then placing the composite resin in a nitrogen atmosphere to anneal for 1.5h at 300 ℃ to obtain a final product, and then placing the prepared composite resin in a thermal resistance instrument to detect the thermal conductivity, wherein the cold electrode temperature of the thermal resistance instrument is set to be 20 ℃, the hot electrode temperature is set to be 80 ℃, and the pressure is set to be 50N.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method is characterized by comprising the following steps of:
s1, firstly, preparing a graphene mixed solution, then dispersing carbon fibers and particle heat-conducting fillers in gaps of graphene in the mixed solution, and stirring to obtain a dispersion liquid;
s2, putting the dispersion liquid into an oven to evaporate and concentrate the dispersion liquid to a colloid state;
s3, placing colloid containing the graphene and the particle heat-conducting filler with the graphene gaps in an ultra-flat evaporating dish, placing the evaporating dish in freeze drying equipment, and setting parameters to obtain the particle heat-conducting filler sheets with the vertically-oriented graphene and the graphene gaps;
s4, annealing the materials in a nitrogen atmosphere to obtain a final product, and testing the thermal conductivity coefficient of the composite resin in a thermal resistance instrument.
2. The process for preparing the highly oriented graphene oxide-based composite resin with high thermal conductivity by the lyophilization method according to claim 1, wherein the graphene mixed solution in the S1 can be water, ethanol, isopropanol, n-propanol, acetone, acetonitrile, and multi-component mixture, and the ratio of the graphene mixed solution to the graphene mixed solution is 1: 1.
3. the process for preparing the highly oriented graphene oxide-based composite resin with high thermal conductivity by the lyophilization method according to claim 2, wherein the graphene mixed solution in the S1 is prepared by stirring water, ethanol, isopropanol, n-propanol, acetone, acetonitrile and a multi-component mixture for 1-3 h.
4. The process for preparing the highly-oriented graphene oxide-based highly-heat-conductive composite resin by the freeze-drying method according to claim 1, wherein the number of graphene layers is 1-100, and the graphene is graphene oxide with oxidized functional groups on the surface.
5. The lyophilization process for preparing the highly oriented graphene oxide-based highly heat conductive composite resin according to claim 1, wherein the particulate heat conductive filler in the graphene voids of S1 is one or more of aluminum oxide, aluminum nitride, boron nitride, silicon carbide, metal nanoparticles, boron nitride nanosheets, and graphene nanosheets.
6. The process for preparing the highly oriented graphene oxide-based composite resin with high thermal conductivity by the lyophilization method according to claim 1, wherein the parameters of the lyophilization equipment in the S3 are set to be a freezing temperature of-10 ℃ to-200 ℃, and a freezing time is 1h to 48 h.
7. The process for preparing the highly-oriented graphene oxide-based highly-heat-conductive composite resin according to claim 1, wherein the annealing temperature in the step S4 is 200-400 ℃, and the annealing time is 0.5-1.5 h.
8. The process for preparing the high-orientation graphene oxide-based high-thermal-conductivity composite resin by the freeze-drying method according to claim 1, wherein the parameters of a thermal resistance instrument in the S4 are set to be 10-30 ℃ of cold electrode temperature, 70-90 ℃ of hot electrode temperature and 40-60N of pressure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113881228A (en) * | 2021-09-10 | 2022-01-04 | 中国科学院金属研究所 | High-thermal-conductivity carbon fiber composite material and preparation method thereof |
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| US20180244582A1 (en) * | 2015-08-20 | 2018-08-30 | University Of Virginia Patent Foundation | Method of forming graphene/metal-oxide hybrid reinforced composites and product thereof |
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