CN112552754A - Preparation method of graphene heat dissipation coating - Google Patents
Preparation method of graphene heat dissipation coating Download PDFInfo
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- CN112552754A CN112552754A CN202011457253.3A CN202011457253A CN112552754A CN 112552754 A CN112552754 A CN 112552754A CN 202011457253 A CN202011457253 A CN 202011457253A CN 112552754 A CN112552754 A CN 112552754A
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Abstract
The invention provides a preparation method of a graphene heat dissipation coating, which comprises the following steps: s1, modifying graphene and carbon nanotubes to obtain a modified graphene-carbon nanotube composite; step S2, uniformly mixing the modified graphene-carbon nanotube composite with a heat-conducting filler to obtain mixed powder; and S3, uniformly mixing the mixed powder, the binder, the solvent and the coating auxiliary agent to obtain the graphene heat dissipation coating. According to the preparation method, the carbon nano tubes are introduced into the raw materials, the surfaces of the graphene and the carbon nano tubes are modified, and the addition sequence of the raw materials is adjusted to be combined, so that the agglomeration of the graphene is reduced, the heat conduction performance among graphene layers is improved, the stability and the dispersibility of the graphene and the carbon nano tubes in the water-based heat dissipation coating are improved, and the heat conductivity of the graphene heat dissipation coating is improved.
Description
Technical Field
The invention relates to the technical field of heat dissipation coatings, and particularly relates to a preparation method of a graphene heat dissipation coating.
Background
With the continuous development of the modern electronic industry, electronic products are continuously developed towards miniaturization, light weight and high power, a large amount of heat can be generated in the use process of the electronic products, and if the heat cannot be rapidly dissipated, the temperature of the electronic products during working can be continuously increased, so that the working reliability and the service life of electronic devices are greatly influenced. At present, in order to enhance the heat dissipation effect of the electronic product radiator, the purpose of improving the heat dissipation effect is achieved mainly by designing the structure of the electronic product radiator, increasing the area of the radiator, changing the material of the radiator and the like, but the methods generally have the problems of complex processing technology, high processing cost, strict equipment requirement and the like, and the heat dissipation effect is difficult to satisfy at the same time.
The heat dissipation coating is a functional coating which can enhance the infrared radiance of the surface of a heat source so as to improve the heat dissipation efficiency of the surface of an object. The heat transfer mode of heat mainly has three kinds, it is heat-conduction respectively, thermal convection and heat radiation, this mode of heat-conduction is mainly used for deriving the heat that electron device produced to electronic product radiator surface fast, and heat convection and heat radiation are mainly with the heat on radiator surface to go in giving off the air, in the radiating field of many needs high efficiency, owing to receive the space, the restriction of size and environment, the mode that can't adopt the convection acceleration exchanges away the heat, consequently, it is first-selected solution to strengthen the infrared radiation heat dissipation through the coating technique, also is the important way that improves radiator heat dispersion.
Graphene has very excellent thermal conductivity, and the theoretical thermal conductivity of single-layer graphene is as high as 5300W/(m.K), which is one of the best thermal conductivity materials known in the world at present. In addition, Matsumoto t. et al found that the thermal radiation emissivity of graphene is 0.99 in the infrared range, very close to the thermal radiation emissivity 1 of theoretical blackbody radiation, and thus has considerable potential as a thermal radiation heat dissipation material; compared with the lower thermal radiation coefficient of metal copper or aluminum, the graphene has the characteristics of heat conduction and heat radiation in the heat dissipation application. However, due to the two-dimensional structure and the huge specific surface area of the graphene material, the graphene material is difficult to disperse in the matrix material and easy to agglomerate, and the agglomeration is irreversible, so that the heat conductivity of the graphene heat dissipation coating is greatly influenced, the heat conductivity of the existing water-based graphene heat dissipation coating is about 3W/(m.K), the heat conductivity is relatively low, the achieved heat dissipation effect is poor, and the heat dissipation requirement of an electronic product is difficult to meet.
Disclosure of Invention
The invention aims to solve the problems that graphene in the existing graphene heat dissipation coating is easy to agglomerate, so that the graphene heat dissipation coating is poor in heat conduction performance and poor in heat dissipation effect.
In order to solve the above problems, the invention provides a preparation method of a graphene heat dissipation coating, which comprises the following steps:
s1, modifying graphene and carbon nanotubes to obtain a modified graphene-carbon nanotube composite;
step S2, uniformly mixing the modified graphene-carbon nanotube composite with a heat-conducting filler to obtain mixed powder;
and S3, uniformly mixing the mixed powder, the binder, the solvent and the coating auxiliary agent to obtain the graphene heat dissipation coating.
Preferably, the step S1 includes: and uniformly mixing the graphene, the carbon nano tube and a modifier, carrying out modification treatment under an ultrasonic condition, and filtering and drying to obtain the modified graphene-carbon nano tube compound, wherein the mass ratio of the graphene to the carbon nano tube is 5:1-1: 1.
Preferably, the modifier is one or a mixture of benzene, ether, oleic acid and glycol; the temperature of the modification treatment is not higher than 50 ℃.
Preferably, the step S1 is preceded by: and soaking the graphene and the carbon nano tube in a soaking solution for 2-4h, and continuously stirring the soaking solution in the soaking process, wherein the soaking solution is a trifluoroacetic acid solution.
Preferably, the particle size of the graphene and the carbon nanotube is not more than 10 um.
Preferably, the step S2 includes: the modified graphene-carbon nanotube composite and the heat conducting filler are subjected to ball milling and are uniformly mixed to obtain the mixed powder, wherein the modified graphene-carbon nanotube composite and the heat conducting filler are mixed according to the following parts by weight: 20-60 parts of modified graphene-carbon nanotube compound and 10-40 parts of heat-conducting filler.
Preferably, the step S3 includes: uniformly dispersing the mixed powder, the binder, the solvent and the coating auxiliary agent to obtain the graphene heat dissipation coating, wherein the mixed powder, the binder, the solvent and the coating auxiliary agent are mixed according to the following parts by weight: 30-100 parts of mixed powder, 10-30 parts of binder, 10-40 parts of solvent and 0.3-5 parts of coating auxiliary agent.
Preferably, the mixed powder, the binder, the solvent and the coating auxiliary agent are uniformly dispersed through a non-uniform dispersion rate, wherein the non-uniform dispersion rate is in the range of 1000-5000r/min, and the dispersion temperature is not higher than 50 ℃.
Preferably, the binder is a hydrophilic binder, and the hydrophilic binder is one or a mixture of more of fluorine modified silicone resin, aqueous acrylic emulsion, aqueous polyurethane resin, aqueous polyurethane emulsion, aqueous epoxy resin and aqueous epoxy emulsion;
the solvent is deionized water and/or ethanol.
Preferably, the coating auxiliary agent comprises a leveling agent, a dispersing agent and an antifoaming agent, and the leveling agent, the dispersing agent and the antifoaming agent are mixed according to the following parts by weight: 0.1-1 part of leveling agent, 0.1-2 parts of dispersing agent and 0.1-2 parts of defoaming agent, wherein the leveling agent is polyether modified organic silicon; the dispersant is one or a mixture of more of sodium oleate, carboxylate, sulfate ester salt and sulfonate; the defoaming agent is dimethyl silicone oil or polyether modified silicon.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the graphene heat dissipation coating, provided by the invention, the graphene and the carbon nano tubes are mixed, and the carbon nano tubes form a heat transfer bridge between graphene sheets, so that the graphene and the carbon nano tubes form a three-dimensional heat conduction network, a contact interface in a graphene film is increased, the distance between graphene layers is reduced, the thermal resistance between graphene sheets is reduced, the heat conduction performance between graphene layers is obviously improved, and the agglomeration between the graphene is effectively prevented; the graphene and the carbon nano tube are subjected to surface modification to prepare a modified graphene-carbon nano tube compound, and the graphene and the carbon nano tube can be more uniformly dispersed in the water-based heat dissipation coating by improving the surface properties of the graphene and the carbon nano tube, so that the stability of the graphene and the carbon nano tube in the water-based heat dissipation coating is enhanced, and the heat conduction is facilitated; mixing the modified graphene-carbon nanotube composite with a heat-conducting filler, then mixing the mixture with a binder, a solvent and a coating additive to ensure that the graphene-carbon nanotube composite and the heat-conducting filler are fully dispersed, and then mixing the mixture with the binder, the solvent and the coating additive to avoid agglomeration caused by directly adding the graphene-carbon nanotube composite and the heat-conducting filler into the binder, the solvent and the coating additive to influence heat conduction of the graphene heat-dissipating coating; according to the preparation method, the carbon nano tubes are introduced into the raw materials, the surfaces of the graphene and the carbon nano tubes are modified, and the addition sequence of the raw materials is adjusted to be combined, so that the agglomeration of the graphene is reduced, the heat conduction performance among graphene layers is improved, the stability and the dispersibility of the graphene and the carbon nano tubes in the water-based heat dissipation coating are improved, and the heat conductivity of the graphene heat dissipation coating is improved.
2. According to the preparation method of the graphene heat dissipation coating, provided by the invention, the graphene and the carbon nano tube are combined through the three-dimensional network, and the interaction among the graphene, the carbon nano tube and the binder is enhanced through the hydrogen bond and the covalent bond, so that the mechanical strength of the graphene heat dissipation coating is enhanced.
3. The preparation method of the graphene heat dissipation coating provided by the invention is simple in preparation process and low in cost, ethanol and/or deionized water is used as a solvent, the environment is protected, the prepared graphene heat dissipation coating is good in heat conduction performance and obvious in heat dissipation effect, and the heat conductivity of the prepared graphene heat dissipation coating is up to 500-class 600W/(m.k).
4. The graphene heat dissipation coating provided by the invention has good application prospects in various fields, is mainly applied to heat dissipation device coatings (such as electronic devices in the fields of mobile phones, computers, spaceflight or military) in the electronic industry and LED heat dissipation device coatings (such as high-power LED illuminating lamps) and is beneficial to the miniaturization development of electronic products.
Drawings
Fig. 1 is a flowchart of preparing a graphene thermal dissipation coating according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In addition, the terms "comprising," "including," "containing," and "having" are intended to be non-limiting, i.e., that other steps and other ingredients can be added that do not affect the results. Materials, equipment and reagents are commercially available unless otherwise specified.
In addition, although the invention has described the forms of S1, S2, S3 and the like for each step in the preparation, the description is only for the convenience of understanding, and the forms of S1, S2, S3 and the like do not represent the limitation of the sequence of each step.
Fig. 1 is a flowchart for preparing a graphene heat dissipation coating according to the present invention. With reference to fig. 1, an embodiment of the present invention provides a preparation method of a graphene heat dissipation coating, including the following steps:
s1, modifying graphene and carbon nanotubes to obtain a modified graphene-carbon nanotube composite;
step S2, uniformly mixing the modified graphene-carbon nanotube composite with a heat-conducting filler to obtain mixed powder;
and S3, uniformly mixing the mixed powder, the binder, the solvent and the coating auxiliary agent to obtain the graphene heat dissipation coating.
Graphene has a regular carbon six-membered ring structure and has excellent heat conduction performance, however, a graphene film formed by stacking graphene has higher heat conduction performance in the in-plane direction, but the heat conduction performance in the thickness direction is very low, the carbon nanotube is a coaxial circular tube formed by curling a carbon atomic layer in graphite, graphene and the carbon nanotube with different structures are combined, and through the synergistic effect between graphene in a lamellar structure and the carbon nanotube in a circular tube structure, the carbon nanotube bridges a heat transfer bridge between graphene sheets, so that the graphene and the carbon nanotube form a three-dimensional heat conduction network, a contact interface in the graphene film is increased, the distance between graphene layers is reduced, the thermal resistance between graphene sheets is reduced, the heat conduction performance between graphene layers is remarkably improved, and the agglomeration between graphene layers is also effectively prevented; the graphene and the carbon nano tube are subjected to surface modification to prepare a modified graphene-carbon nano tube compound, and the graphene and the carbon nano tube can be more uniformly dispersed in the water-based heat dissipation coating by improving the surface properties of the graphene and the carbon nano tube, so that the stability of the graphene and the carbon nano tube in the water-based heat dissipation coating is enhanced, and the heat conduction is facilitated; mixing the modified graphene-carbon nanotube composite with a heat-conducting filler, then mixing the mixture with a binder, a solvent and a coating additive to ensure that the graphene-carbon nanotube composite and the heat-conducting filler are fully dispersed, and then mixing the mixture with the binder, the solvent and the coating additive to avoid agglomeration caused by directly adding the graphene-carbon nanotube composite and the heat-conducting filler into the binder, the solvent and the coating additive to influence heat conduction of the graphene heat-dissipating coating; the carbon nano tubes are introduced into the raw materials, the surfaces of the graphene and the carbon nano tubes are modified, and the adding sequence of the raw materials is adjusted to combine, so that the agglomeration of the graphene is reduced, the heat conduction performance between graphene layers is improved, and the stability and the dispersibility of the graphene and the carbon nano tubes in the water-based heat dissipation coating are improved, so that the heat conductivity of the graphene heat dissipation coating is increased, and the problems of poor heat conduction performance and poor heat dissipation effect of the graphene heat dissipation coating are solved.
Specifically, in step S1, graphene, carbon nanotubes and a modifier are uniformly mixed, modified under ultrasonic conditions, and filtered and dried to obtain a modified graphene-carbon nanotube composite, wherein the mass ratio of graphene to carbon nanotubes is 5:1-1: 1.
The number of layers of the graphene is not higher than 5, so that the influence on the electric conductivity and the thermal conductivity of the graphene due to the fact that the number of layers of the graphene is too high is avoided. The carbon nanotubes can be single-walled carbon nanotubes or multi-walled carbon nanotubes, which is not further limited in the present invention and can be adjusted by those skilled in the art according to actual situations.
In order to generate more active sites on the surfaces of the graphene and the carbon nanotubes so as to modify the graphene and the carbon nanotubes, before step S1, the graphene and the carbon nanotubes are further subjected to a soaking treatment, specifically, the graphene and the carbon nanotubes are soaked in a soaking solution for 2 to 4 hours, the soaking solution is continuously stirred during the soaking process, and the contact area between the soaking solution and the graphene and the carbon nanotubes is increased, wherein the soaking solution is a trifluoroacetic acid solution. In some preferred embodiments of the invention, the concentration of the trifluoroacetic acid solution is 0.5-2%.
Before the graphene and the carbon nanotubes are subjected to soaking treatment and modification treatment, the graphene and the carbon nanotubes can be further subjected to crushing treatment, so that the particle sizes of the graphene and the carbon nanotubes are not more than 10um, wherein the crushing treatment includes but is not limited to ball milling and grinding, and a person skilled in the art can select a suitable crushing treatment mode according to actual conditions as long as the particle sizes of the graphene and the carbon nanotubes are not more than 10 um. Of course, those skilled in the art may also directly select graphene and carbon nanotubes with a particle size of not greater than 10um as a raw material, and before the soaking treatment and the modification treatment, the particle size of the graphene and the carbon nanotubes is controlled to be not greater than 10um, on one hand, to increase the contact area of the graphene and the carbon nanotubes with the soaking solution and the modifier, and expose more active sites in the modifier, so as to more fully modify the graphene and the carbon nanotubes, and on the other hand, to reduce the difficulty of the subsequent grinding treatment, and to avoid the agglomeration of the graphene and the carbon nanotubes in the subsequent grinding process.
And taking out the soaked graphene and the carbon nano tubes, drying, uniformly mixing the graphene and the carbon nano tubes with a modifier, and carrying out modification treatment under an ultrasonic condition.
Wherein, the modifier is one or a mixture of more of benzene, ether, oleic acid and glycol, the benzene includes but is not limited to toluene and ethylbenzene, and the ether includes but is not limited to diethyl ether. Preferably, the modifier is toluene, the surfaces of the graphene and the carbon nanotubes soaked in the soaking solution have more active sites, and the active sites can easily enable the toluene, the graphene and the carbon nanotubes to be mutually wound and combined to form a macromolecular network structure, so that the graphene, the graphene and the carbon nanotubes can be uniformly and stably dispersed in the coating, and the stability of the graphene and the carbon nanotubes in the coating is enhanced. It should be noted that the amount of the modifier used in the present invention is not further limited as long as the modifier is used in an amount sufficient to modify graphene and carbon nanotubes, and can be adjusted by those skilled in the art according to actual situations.
The modification treatment is carried out under the ultrasonic condition, and the ultrasonic frequency is 50-70 kHZ.
In order to prevent the graphene and the carbon nano tube from agglomerating due to overhigh temperature, the modification treatment temperature is not higher than 50 ℃. Preferably, the modification treatment temperature is 20-40 ℃, and the modification treatment time is 1-3h, so that graphene and carbon nanotubes are more fully modified, and the graphene and the carbon nanotubes are prevented from being agglomerated.
Specifically, in step S2, the modified graphene-carbon nanotube composite and the heat conductive filler are ball-milled and uniformly mixed to obtain a mixed powder.
The modified graphene-carbon nanotube composite and the heat-conducting filler are mixed according to the following parts by weight: 20-60 parts of modified graphene-carbon nanotube compound and 10-40 parts of heat conducting filler, so that the heat conducting filler can fully disperse graphene and carbon nanotubes, the agglomeration of the graphene and the carbon nanotubes is reduced, and the influence of excessive heat conducting filler on the heat conductivity of the graphene is avoided.
The heat-conducting filler is one or a mixture of more of silicon carbide, copper powder, aluminum oxide, aluminum nitride, boron oxide, boron nitride, silicon dioxide, monocrystalline silicon, silver powder, magnesium oxide and zinc oxide, and if the heat-conducting filler is a mixture of more than one substance, the mixing ratio of the more than one substance is the same, for example, when the heat-conducting filler is silicon carbide and boron nitride, the silicon carbide and the boron nitride are mixed according to the weight ratio of 1: 1. The fillers can well prevent the graphene and the carbon nano tube from agglomerating, so that the graphene and the carbon nano tube powder are uniformly dispersed in the whole coating system.
The ball milling rotation speed is 200-. In the embodiment of the present invention, the ball milling time is not further limited as long as the particle size of the mixed powder can be finally ball milled to less than 10um, and those skilled in the art can adjust the ball milling time according to actual conditions.
Specifically, in step S3, the mixed powder, the binder, the solvent, and the coating auxiliary agent are dispersed and mixed uniformly to obtain the graphene heat dissipation coating.
The dispersion temperature is not higher than 50 ℃, and the graphene and the carbon nano tube are prevented from reunion again when the temperature is too high. Preferably, the dispersion temperature is 20-30 ℃, and the dispersion time is 1h, so as to ensure that the graphene and the carbon nanotubes are uniformly dispersed in the binder and the solvent.
In order to mix the mixed powder, the binder, the solvent and the coating auxiliary agent more uniformly, the mixed powder, the binder, the solvent and the coating auxiliary agent are dispersed uniformly by using a non-uniform dispersion rate, that is, in the process of dispersing the mixed powder, the binder, the solvent and the coating auxiliary agent uniformly, the dispersion rate is adjusted according to the state (for example, viscosity) of the dispersion mixed liquid, rather than being dispersed by a fixed dispersion rate. Wherein the range of the non-uniform dispersion rate is 1000-. Specifically, the non-uniform dispersion speed can be realized by a variable frequency dispersion machine, and the rotating speed of the variable frequency dispersion machine is 1000-5000 r/min. The type of the variable frequency dispersion machine is not further limited, and a person skilled in the art can select the variable frequency dispersion machine according to actual conditions, as long as the non-uniform dispersion rate can be realized, and the range of the non-uniform dispersion rate is maintained at 1000-.
The mixed powder, the binder, the solvent and the coating additive are mixed according to the following parts by weight: 30-100 parts of mixed powder, 10-30 parts of binder, 10-40 parts of solvent and 0.3-5 parts of coating auxiliary agent. By adjusting the proportion of the mixed powder, the binder, the solvent and the coating auxiliary agent, the graphene and the carbon nano tube can be stably dispersed in the solvent, the heat dissipation performance of the heat dissipation coating is improved, and the heat dissipation coating has good adhesive force and mechanical performance.
The adhesive is a hydrophilic adhesive, specifically, the adhesive is a mixture of one or more of fluorine modified silicone resin (for example, DN-296D of Dinopo chemical Co., Ltd., Zhongshan Europe), aqueous acrylic resin, aqueous acrylic emulsion, aqueous polyurethane resin, aqueous polyurethane emulsion, aqueous epoxy resin and aqueous epoxy emulsion, if the adhesive is a mixture of several substances, the mixing ratio of the several substances is the same, for example, when the adhesive is the aqueous acrylic resin and the aqueous polyurethane resin, the aqueous acrylic resin and the aqueous polyurethane resin are mixed according to the weight ratio of 1: 1. The binders can form a similar net or chain structure, so that contact and interaction are formed between the dispersed graphene and the carbon nano tubes, the heat dissipation performance is improved, and the coating can be well attached to a substrate.
The solvent is deionized water and/or ethanol, and when the solvent is the deionized water and the ethanol, the deionized water and the ethanol are miscible in any proportion.
The coating auxiliary agent includes, but is not limited to, a leveling agent, a dispersing agent and a defoaming agent, and a person skilled in the art can add a suitable coating auxiliary agent according to the actual situation, and can select the coating auxiliary agent according to the actual situation. In some preferred embodiments of the present invention, the coating auxiliary comprises a leveling agent, a dispersing agent and a defoaming agent, and in order to make the coating auxiliary suitable for the coating system of the present invention and to better perform the corresponding functions, the coating auxiliary is mixed according to the following parts by weight: 0.1-1 part of flatting agent, 0.1-2 parts of dispersant and 0.1-2 parts of defoaming agent.
Wherein, the leveling agent is polyether modified organic silicon, such as: polyether/amino silicone SPEAS-1. The polyether modified organic silicon flatting agent can promote the water-based paint to form a flat, smooth and uniform coating film in the drying film-forming process, can effectively reduce the surface tension of the coating liquid, and improves the flatting property and uniformity of the coating liquid.
The dispersant is one or a mixture of several of sodium oleate, carboxylate, sulfate ester salt and sulfonate, and if the dispersant is a mixture of several substances, the several substances can be mixed in a proper proportion as long as the dispersant can perform a dispersing function, and the dispersant is not further limited in the invention. The dispersing agents can play a role in stabilizing a dispersing medium in a water-soluble environment and improving the surface property of the mixed powder.
The defoaming agent is dimethyl silicone oil or polyether modified silicon. Both of these defoaming agents can reduce the surface tension, suppress the generation of foam in the coating material or eliminate foam that has been generated.
In order to ensure that the particle size of the prepared graphene heat dissipation coating is smaller than 10um, the graphene heat dissipation coating is convenient to spray, the particle size of the prepared graphene heat dissipation coating needs to be detected, if the particle size of the graphene heat dissipation coating is larger than 10um, the graphene heat dissipation coating is ground and then detected until the particle size of the graphene heat dissipation coating is smaller than 10 um.
The temperature for grinding the graphene heat dissipation coating is not more than 50 ℃, the phenomenon that the graphene and the carbon nano tube are agglomerated again due to the overhigh temperature is avoided, the specific grinding temperature can be adjusted by a person skilled in the art according to actual conditions, and the grinding temperature is not more than 50 ℃.
The rotation speed for grinding the graphene heat dissipation coating is 500-1000r/min, the grinding time is determined according to the particle size of the graphene heat dissipation coating, and the grinding can be stopped as long as the particle size of the graphene heat dissipation coating is less than 10 microns.
In order to avoid the influence of particle sedimentation in the graphene heat dissipation coating on the service performance of the coating, the graphene heat dissipation coating is uniformly dispersed before the graphene heat dissipation coating is used, and then spraying or brushing is carried out.
In order to further illustrate the present invention, the following examples are given to further illustrate the present invention. The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified; materials, reagents and the like used in examples of the present invention are commercially available unless otherwise specified.
Example 1
The embodiment provides a preparation method of a graphene heat dissipation coating, which comprises the following steps:
1.1 weighing graphene and carbon nanotubes according to a mass ratio of 5:1, crushing the graphene and the carbon nanotubes to a particle size of not more than 10um, placing the graphene and the carbon nanotubes in a trifluoroacetic acid solution (with a concentration of 1%) for soaking for 3h, taking out, drying, mixing the graphene and the carbon nanotubes with toluene, carrying out ultrasonic modification treatment at normal temperature (25 ℃) at an ultrasonic frequency of 60kHZ for 2h, and filtering and drying to obtain a modified graphene-carbon nanotube composite;
1.2 weighing 30 parts of modified graphene-carbon nanotube composite and 20 parts of silicon carbide according to parts by weight, placing the modified graphene-carbon nanotube composite and the silicon carbide in a ball mill, and carrying out ball milling for 30min at a ball milling rotation speed of 500r/min to obtain mixed powder with the particle size of less than 10 um;
1.3 weighing 50 parts of mixed powder, 15 parts of water-based acrylic resin, 30 parts of ethanol solution, 1 part of polyether modified organic silicon flatting agent, 2 parts of sodium oleate and 2 parts of dimethyl silicone oil according to parts by weight, placing the mixed powder, the water-based acrylic resin, the ethanol solution, the polyether modified organic silicon flatting agent, the sodium oleate and the dimethyl silicone oil into a container with a water cooling device, dispersing the mixture in the container for 1h by using a variable frequency dispersion machine with the rotation speed of 1000-5000r/min at normal temperature (25 ℃), detecting the particle size of the mixture by using a scraper particle size instrument, transferring the mixture into a three-roll grinding machine if the particle size is more than 10um, and grinding at 600r/min until the particle size of the mixture is less than 10um to obtain the graphene heat dissipation coating.
Example 2
This example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that, in the preparation of the modified graphene-carbon nanotube composite, graphene and carbon nanotubes are mixed in a mass ratio of 5:2, and other preparation steps are the same as the preparation steps in example 1.
Example 3
This example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that, in the preparation of the modified graphene-carbon nanotube composite, graphene and carbon nanotubes are mixed in a mass ratio of 5:3, and other preparation steps are the same as the preparation steps in example 1.
Example 4
This example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that, in the preparation of the modified graphene-carbon nanotube composite, graphene and carbon nanotubes are mixed according to a mass ratio of 5:4, and other preparation steps are the same as the preparation steps in example 1.
Example 5
This example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that, in the preparation of the modified graphene-carbon nanotube composite, graphene and carbon nanotubes are mixed in a mass ratio of 1:1, and other preparation steps are the same as the preparation steps in example 1.
Example 6
The embodiment provides a preparation method of a graphene heat dissipation coating, which comprises the following steps:
6.1 weighing graphene and carbon nanotubes according to a mass ratio of 5:3, crushing the graphene and the carbon nanotubes to a particle size of not more than 10um, placing the graphene and the carbon nanotubes in a trifluoroacetic acid solution (with a concentration of 1%) for soaking for 3h, taking out, drying, mixing the graphene and the carbon nanotubes with toluene, carrying out ultrasonic modification treatment at normal temperature (25 ℃) at an ultrasonic frequency of 60kHZ for 2h, and filtering and drying to obtain a modified graphene-carbon nanotube composite;
6.2 weighing 30 parts of the modified graphene-carbon nanotube composite and 10 parts of copper powder according to the parts by weight, placing the modified graphene-carbon nanotube composite and the copper powder into a ball mill, and carrying out ball milling for 50min at a ball milling rotating speed of 300r/min to obtain mixed powder with the particle size of less than 10 um;
6.3 weighing 40 parts of mixed powder, 15 parts of fluorine modified silicon resin, 40 parts of deionized water, 1 part of polyether modified organic silicon flatting agent, 2 parts of sodium carboxylate and 2 parts of polyether modified silicon defoaming agent according to parts by weight, placing the mixed powder, the fluorine modified silicon resin, the deionized water, the polyether modified organic silicon flatting agent, the sodium carboxylate and the polyether modified silicon defoaming agent in a container with a water cooling device, dispersing the mixture in the container for 1h by using a variable frequency dispersion machine with the rotating speed of 1000 plus 5000r/min at normal temperature (25 ℃), detecting the particle size of the mixture by using a scraper particle size analyzer, transferring the mixture into a three-roll grinding machine if the particle size is larger than 10um, and grinding at 800r/min until the particle size of the mixture is smaller than 10um to obtain the graphene heat dissipation coating.
Example 7
The embodiment provides a preparation method of a graphene heat dissipation coating, which comprises the following steps:
7.1 weighing graphene and carbon nanotubes according to a mass ratio of 5:3, crushing the graphene and the carbon nanotubes to a particle size of not more than 10um, placing the graphene and the carbon nanotubes in a trifluoroacetic acid solution (with a concentration of 1%) for soaking for 3h, taking out, drying, mixing the graphene and the carbon nanotubes with toluene, carrying out ultrasonic modification treatment at normal temperature (25 ℃) at an ultrasonic frequency of 60kHZ for 2h, and filtering and drying to obtain a modified graphene-carbon nanotube composite;
7.2 weighing 30 parts of the modified graphene-carbon nanotube composite and 30 parts of aluminum nitride according to the parts by weight, placing the modified graphene-carbon nanotube composite and the aluminum nitride in a ball mill, and carrying out ball milling for 50min at the ball milling rotating speed of 300r/min to obtain mixed powder with the particle size of less than 10 um;
7.3 weighing 60 parts of mixed powder, 15 parts of waterborne polyurethane resin, 20 parts of deionized water, 1 part of polyether modified organosilicon leveling agent, 2 parts of sodium sulfonate and 2 parts of polyether modified silicon defoaming agent according to parts by weight, placing the mixed powder, the waterborne polyurethane resin, the deionized water, the polyether modified organosilicon leveling agent, the sodium sulfonate and the polyether modified silicon defoaming agent in a container with a water cooling device, dispersing the mixture in the container for 1h by using a variable frequency dispersion machine with the rotation speed of 1000 plus 5000r/min at normal temperature (25 ℃), detecting the particle size of the mixture by using a scraper particle size analyzer, transferring the mixture to a three-roll grinding machine if the particle size is larger than 10um, and grinding at 1000r/min until the particle size of the mixture is smaller than 10um to obtain the graphene heat dissipation coating.
Example 8
The embodiment provides a preparation method of a graphene heat dissipation coating, which comprises the following steps:
8.1 weighing graphene and carbon nanotubes according to a mass ratio of 5:3, crushing the graphene and the carbon nanotubes to a particle size of not more than 10um, placing the graphene and the carbon nanotubes in a trifluoroacetic acid solution (with a concentration of 1%) for soaking for 3h, taking out, drying, mixing the graphene and the carbon nanotubes with toluene, carrying out ultrasonic modification treatment at normal temperature (25 ℃) at an ultrasonic frequency of 60kHZ for 2h, and filtering and drying to obtain a modified graphene-carbon nanotube composite;
8.2 weighing 30 parts of modified graphene-carbon nanotube composite and 20 parts of silicon dioxide according to parts by weight, placing the modified graphene-carbon nanotube composite and the silicon dioxide in a ball mill, and performing ball milling for 60min at a ball milling rotating speed of 200r/min to obtain mixed powder with the particle size of less than 10 um;
8.3 weighing 50 parts of mixed powder, 25 parts of water-based acrylic emulsion, 20 parts of deionized water, 1 part of polyether modified organic silicon flatting agent, 2 parts of sodium oleate and 2 parts of polyether modified silicon defoaming agent according to the parts by weight, placing the mixed powder, the water-based acrylic emulsion, the deionized water, the polyether modified organic silicon flatting agent, the sodium oleate and the polyether modified silicon defoaming agent in a container with a water cooling device, dispersing the mixture in the container for 1h by using a variable frequency dispersion machine with the rotation speed of 1000-5000r/min at normal temperature (25 ℃), detecting the particle size of the mixture by using a scraper particle size analyzer, transferring the mixture into a three-roll grinding machine if the particle size is larger than 10um, and grinding at 600r/min until the particle size of the mixture is smaller than 10um to obtain the graphene heat dissipation coating.
Comparative example 1
The comparative example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 8, except that in step 3, 50 parts by weight of mixed powder, 5 parts by weight of aqueous acrylic emulsion, 40 parts by weight of deionized water, 1 part by weight of polyether modified silicone leveling agent, 2 parts by weight of sodium oleate and 2 parts by weight of polyether modified silicone defoaming agent are weighed, and the mixed powder, the aqueous acrylic emulsion, the deionized water, the polyether modified silicone leveling agent, the sodium oleate and the polyether modified silicone defoaming agent are uniformly dispersed to obtain the graphene heat dissipation coating, and other preparation steps are the same as those in example 8.
Comparative example 2
The comparative example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that graphene and carbon nanotubes are not soaked in a trifluoroacetic acid solution, the graphene and carbon nanotubes are directly mixed with toluene, and then subjected to ultrasonic modification treatment at normal temperature (25 ℃) for 2 hours at an ultrasonic frequency of 60kHZ, and after filtration and drying, a modified graphene-carbon nanotube composite is obtained; the other preparation steps were the same as those in example 1.
Comparative example 3
The comparative example provides a preparation method of a graphene heat dissipation coating, which is the same as the preparation method in example 1, except that the graphene and the carbon nanotubes are not soaked in a trifluoroacetic acid solution and are not modified by a modifier, that is, the graphene and the carbon nanotubes are directly mixed with a heat conductive filler to obtain mixed powder, and then the mixed powder, a binder, a solvent and a coating auxiliary agent are dispersed and uniformly mixed to obtain the graphene heat dissipation coating.
Comparative example 4
The comparative example provides a preparation method of a graphene heat dissipation coating, which comprises the steps of weighing the raw materials according to the proportion of the raw materials in the example 1, directly placing graphene, carbon nanotubes, a heat conduction filler, a binder, a solvent and a coating auxiliary agent in a container with a water cooling device, dispersing a mixture in the container for 1h at normal temperature (25 ℃) by using a variable frequency dispersion machine with the rotation speed of 1000-5000r/min, detecting the particle size of the mixture by using a scraper particle sizer, transferring the mixture to a three-roll grinder if the particle size is larger than 10um, and grinding at 600r/min until the particle size of the mixture is smaller than 10um to obtain the graphene heat dissipation coating.
The graphene heat dissipation coatings of examples 1 to 8 and comparative examples 1 to 4 were sprayed on the substrate, and the performances of the graphene heat dissipation coatings of examples 1 to 8 and comparative examples 1 to 4 were tested, specifically, the following test methods were adopted:
thermal conductivity: measuring the thermal diffusion coefficient alpha of a sample to be measured by a laser heat dissipation instrument; and measuring the specific heat capacity C of the coating by using a Differential Scanning Calorimeter (DSC)pDuring the test, a reference sample which has the same interface shape, similar thickness, similar thermal physical property, same surface structure smoothness and known specific heat value as the sample to be tested is subjected to surface coating with the sample to be tested at the same time to test the specific heat capacity C of the coatingp(ii) a The formula of the density is rho-m/V, and the formula of the volume is V-pi r2d, measuring the density rho of the sample to be measured, wherein m is the mass of the sample, V is the volume of the sample, r is the radius of the sample, and d is the thickness; because the thickness most possibly affects the thermal conductivity, the thickness of the sample to be measured is measured by using a scanning electron microscope, at least 10 different positions are selected for subsequent measurement during measurement, and then the average value is calculated to obtain more accurate thickness. Measuring to obtain the thermal diffusion coefficient alpha,Specific heat capacity CpAnd after the density rho, according to a calculation formula of the thermal conductivity: λ ═ α Cpρ, the thermal conductivity λ is calculated.
Adhesion force: refer to the national standard GB/T9286 1998 paint and varnish paint film marking test.
Strength: refer to the national standard GB/T1732-1993 paint film impact resistance determination method.
Hardness: the hardness of the paint film is tested by referring to the national standard GB/T6739-.
The test results are shown in Table 1.
Table 1 performance index of different graphene heat-dissipating coatings
It can be seen from the above examples and comparative examples that the graphene heat dissipation coating prepared by the preparation method of the present invention has a high thermal conductivity, the thermal conductivity is as high as 500-. In addition, as can be seen from the examples and comparative examples, when the amount of the binder added is too small, the mechanical properties of the graphene heat dissipation coating are affected, and the thermal conductivity of the graphene heat dissipation coating prepared from the graphene and the carbon nanotubes which are not soaked in the soaking solution and are not modified by the modifier is significantly lower than that of the graphene heat dissipation coating prepared from the graphene and the carbon nanotubes which are soaked in the soaking solution and are modified by the modifier.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4306820A1 (en) * | 2022-07-12 | 2024-01-17 | Marcin Golec | Brake pad for a bicycle or a motorbike disc brake assembly |
| CN115181462A (en) * | 2022-08-29 | 2022-10-14 | 陕西邦希化工有限公司 | Graphene heat dissipation coating and preparation method thereof |
| CN115505309A (en) * | 2022-10-26 | 2022-12-23 | 天津中电立正石墨烯科技有限公司 | Water-based graphene heat dissipation coating and preparation method thereof |
| CN115926573A (en) * | 2022-12-05 | 2023-04-07 | 广东电网有限责任公司 | Super-hydrophilic composite coating and preparation method and application thereof |
| CN115926573B (en) * | 2022-12-05 | 2023-08-18 | 广东电网有限责任公司 | Super-hydrophilic composite coating and preparation method and application thereof |
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