CN110804279A - Preparation method of three-dimensional network carbon/epoxy resin heat-conducting composite material based on salt template - Google Patents
Preparation method of three-dimensional network carbon/epoxy resin heat-conducting composite material based on salt template Download PDFInfo
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- CN110804279A CN110804279A CN201911178552.0A CN201911178552A CN110804279A CN 110804279 A CN110804279 A CN 110804279A CN 201911178552 A CN201911178552 A CN 201911178552A CN 110804279 A CN110804279 A CN 110804279A
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Abstract
The invention relates to a preparation method of a three-dimensional network carbon/epoxy resin heat-conducting composite material based on a salt template, which comprises the following steps: preparing a three-dimensional network carbon material precursor by a salt template method: preparing a solution from sodium chloride and glucose according to a certain proportion, and performing spray drying to obtain white precursor powder. And (3) catalyzing graphene growth by a calcination method: and placing the obtained white precursor powder into a tubular furnace, heating to 700-. And removing the salt template to obtain the three-dimensional network carbon material. Preparing a composite material by compounding with epoxy resin: the three-dimensional network carbon material/epoxy resin composite material is prepared by using a melt blending method and curing and molding the three-dimensional network carbon material serving as a heat-conducting filler and epoxy resin according to a certain proportion.
Description
The technical field is as follows:
the invention belongs to the field of heat-conducting composite materials, and particularly relates to preparation of a three-dimensional network carbon/epoxy resin composite material and research on heat-conducting performance of the three-dimensional network carbon/epoxy resin composite material.
Background art:
modern instruments and equipment tend to be miniaturized and integrated, and equipment can produce a large amount of heats in the operation process, if not get rid of in time, not only can influence the job stabilization nature of equipment, more can seriously shorten the working life of equipment. Accordingly, an increasing number of researchers are focusing their attention on thermally conductive composites. Compared with metal materials or ceramic materials, the high molecular polymer has good chemical stability because of easy molding and light weight, and is widely applied to the fields of electronics, electrics, aerospace and the like. However, the low thermal conductivity and low thermal stability (especially of thermoplastic polymers) limit their application in the field of thermal conduction. The epoxy resin as a thermosetting plastic has strong mechanical strength, chemical stability and high temperature resistance after being cured and molded, and is widely applied to the industrial field and the actual production. However, the data show that similar to most high molecular materials, the thermal conductivity of epoxy resin is very low, which severely limits the application of epoxy resin in the field of thermal conduction, and therefore, the research for enhancing the thermal conductivity of epoxy resin has important practical significance.
The heat-conducting composite material is formed by compounding heat-conducting filler with a matrix according to a certain method, so that the heat-conducting property of the matrix is improved. The heat-conducting carbon materials commonly used at present comprise traditional carbon materials such as graphite and carbon black and novel materials such as carbon nanotubes and graphene. In the application process, as the heat-conducting property of the traditional materials such as graphite is lower, the heat-conducting property of the matrix can be well improved only by using larger addition amount, and the larger addition amount can cause higher brittleness of the composite material and influence the mechanical property of the material. Although the novel materials such as the carbon nanotube and the graphene have good heat conductivity and can greatly improve the heat conductivity of the matrix under the condition of low addition amount, the materials such as the carbon nanotube and the graphene have high preparation cost and limit large-scale application, and are easy to agglomerate due to strong van der waals force in the use process and cannot well exert the excellent heat conductivity.
The literature research shows that the three-dimensional network carbon material has larger specific surface area compared with the traditional carbon material (graphite, carbon black) and the like, and in the forming process, the three-dimensional carbon material is easier to contact with each other to form a heat conduction path, so that more paths are provided for the transfer of carriers, and the addition amount is reduced. Meanwhile, due to the formation of the three-dimensional structure, the agglomeration phenomenon of materials such as carbon nanotubes and graphene in the matrix can be reduced to a certain extent, the contact area with the matrix is increased, and the interface thermal resistance between the heat-conducting filler and the matrix is reduced.
The three-dimensional network carbon material is prepared by using a salt template auxiliary calcination method and is used as a heat-conducting filler to improve the heat-conducting property of the epoxy resin. Compared with materials such as carbon nano tubes, graphene and the like, the preparation cost is greatly reduced, and the heat-conducting filler is a heat-conducting filler with higher cost performance.
The invention content is as follows:
the invention provides a method for preparing a three-dimensional network carbon material at low cost, and the three-dimensional network carbon material is used as a heat-conducting filler to prepare a three-dimensional network carbon/epoxy resin composite material. The technical scheme of the invention is as follows:
a preparation method of a three-dimensional network carbon/epoxy resin heat-conducting composite material based on a salt template comprises the following steps:
(1) preparing a three-dimensional network carbon material precursor by a salt template method: preparing a solution from sodium chloride and glucose according to a certain proportion, and performing spray drying to obtain white precursor powder.
(2) And (3) catalyzing graphene growth by a calcination method: and placing the obtained white precursor powder into a tubular furnace, heating to 700-.
(3) Removing the salt template to obtain a three-dimensional network carbon material: and removing the sodium chloride template on the surface of the graphene by using a suction filtration and washing method for black precursor powder, and then drying in vacuum to obtain the three-dimensional network carbon material.
(4) Preparing a composite material by compounding with epoxy resin: the three-dimensional network carbon material/epoxy resin composite material is prepared by using a melt blending method and curing and molding the three-dimensional network carbon material serving as a heat-conducting filler and epoxy resin according to a certain proportion.
In the step (1), the ratio of Na atom: preparing solution with C atom of 100 (8-40).
In the step (2), the temperature is preferably raised to 750 ℃.
In conclusion, the core of the invention is to prepare the three-dimensional network carbon material by using a salt template auxiliary calcination method,
and then used as a heat-conducting filler to enhance the heat-conducting property of the epoxy resin.
Compared with the prior art, the invention has the advantages that:
(1) the three-dimensional network carbon material is successfully prepared by using a salt template auxiliary calcination method.
(2) The preparation cost is low, and the experimental materials are low in price and wide in source.
(3) The invention has simple equipment and simple and convenient process.
(4) The invention has high reliability, strong repeatability, good application prospect and environmental protection.
Drawings
Fig. 1 is an SEM image of a three-dimensional network carbon material.
FIG. 2 is a TEM image of a three-dimensional network carbon material.
FIG. 3 is a comparison of thermal conductivity of the three-dimensional network carbon/epoxy resin composite material prepared by the present invention and a pure epoxy material.
Detailed Description
Example 1:
sodium chloride (template) and glucose (solid carbon source) were mixed as Na atoms: mixing the carbon atoms with deionized water in a ratio of 100:20, magnetically stirring the mixture at normal temperature for 5 hours, and drying the obtained solution by using a laboratory vacuum spray dryer (temperature: 170 ℃) to obtain white three-dimensional network carbon material precursor powder. Then, an appropriate amount of the powder was placed in a boat and subjected to CVD treatment in a tube furnace. And introducing Ar into the tubular furnace at the flow rate of 240sccm, heating the furnace temperature to 750 ℃ at the speed of 10 ℃/min, preserving the temperature for 2 hours, and then cooling to room temperature to obtain black three-dimensional network carbon material precursor powder. And putting the obtained black powder into a beaker, adding deionized water, magnetically stirring for 10 minutes, and repeatedly washing for 2-3 times by using a suction filtration method to remove the sodium chloride template to obtain the three-dimensional network carbon material. And curing and molding the three-dimensional network carbon material and the epoxy resin to obtain the composite material.
Example 2:
sodium chloride (template) and glucose (solid carbon source) were mixed as Na atoms: mixing the carbon atoms with deionized water in a ratio of 100:30, magnetically stirring the mixture at normal temperature for 5 hours, and drying the obtained solution by using a laboratory vacuum spray dryer (temperature: 170 ℃) to obtain white three-dimensional network carbon material precursor powder. Then, an appropriate amount of the powder was placed in a boat and subjected to CVD treatment in a tube furnace. And introducing Ar into the tubular furnace at the flow rate of 240sccm, heating the furnace temperature to 750 ℃ at the speed of 10 ℃/min, preserving the temperature for 2 hours, and then cooling to room temperature to obtain black three-dimensional network carbon material precursor powder. And putting the obtained black powder into a beaker, adding deionized water, magnetically stirring for 10 minutes, and repeatedly washing for 2-3 times by using a suction filtration method to remove the sodium chloride template to obtain the three-dimensional network carbon material. And curing and molding the three-dimensional network carbon material and the epoxy resin to obtain the composite material.
Example 3:
sodium chloride (template) and glucose (solid carbon source) were mixed as Na atoms: mixing the carbon atoms with deionized water in a ratio of 100:10, magnetically stirring the mixture at normal temperature for 5 hours, and drying the obtained solution by using a laboratory vacuum spray dryer (temperature: 170 ℃) to obtain white three-dimensional network carbon material precursor powder. Then, an appropriate amount of the powder was placed in a boat and subjected to CVD treatment in a tube furnace. And introducing Ar into the tubular furnace at the flow rate of 240sccm, heating the furnace temperature to 750 ℃ at the speed of 10 ℃/min, preserving the temperature for 2 hours, and then cooling to room temperature to obtain black three-dimensional network carbon material precursor powder. And putting the obtained black powder into a beaker, adding deionized water, magnetically stirring for 10 minutes, and repeatedly washing for 2-3 times by using a suction filtration method to remove the sodium chloride template to obtain the three-dimensional network carbon material. And curing and molding the three-dimensional network carbon material and the epoxy resin to obtain the composite material.
Claims (3)
1. A preparation method of a three-dimensional network carbon/epoxy resin heat-conducting composite material based on a salt template comprises the following steps:
(1) preparing a three-dimensional network carbon material precursor by a salt template method: preparing a solution from sodium chloride and glucose according to a certain proportion, and performing spray drying to obtain white precursor powder.
(2) And (3) catalyzing graphene growth by a calcination method: and placing the obtained white precursor powder into a tubular furnace, heating to 700-.
(3) Removing the salt template to obtain a three-dimensional network carbon material: and removing the sodium chloride template on the surface of the graphene by using a suction filtration and washing method for black precursor powder, and then drying in vacuum to obtain the three-dimensional network carbon material.
(4) Preparing a composite material by compounding with epoxy resin: the three-dimensional network carbon material/epoxy resin composite material is prepared by using a melt blending method and curing and molding the three-dimensional network carbon material serving as a heat-conducting filler and epoxy resin according to a certain proportion.
2. The production method according to claim 1, wherein in the step (1), the ratio of the Na atom: preparing solution with C atom of 100 (8-40).
3. The production method according to claim 1, wherein in the step (2), the temperature is raised to 750 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061322A (en) * | 2021-04-15 | 2021-07-02 | 安徽大学 | CNT @ Co/epoxy resin composite material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291312A (en) * | 2014-09-25 | 2015-01-21 | 天津大学 | Method for preparing hierarchical porous carbon material based on sea salt template |
| CN106433133A (en) * | 2016-08-23 | 2017-02-22 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material, and preparation method and application thereof |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
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- 2019-11-27 CN CN201911178552.0A patent/CN110804279A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104291312A (en) * | 2014-09-25 | 2015-01-21 | 天津大学 | Method for preparing hierarchical porous carbon material based on sea salt template |
| WO2017219944A1 (en) * | 2016-06-20 | 2017-12-28 | 山东欧铂新材料有限公司 | Method for preparing graphene-epoxy resin composite material |
| CN106433133A (en) * | 2016-08-23 | 2017-02-22 | 广东工业大学 | Polymer matrix/three-dimensional graphene thermal interface composite material, and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061322A (en) * | 2021-04-15 | 2021-07-02 | 安徽大学 | CNT @ Co/epoxy resin composite material and preparation method thereof |
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Application publication date: 20200218 |