CN112831245A - Graphene carbon nanotube heat conduction slurry and preparation method thereof - Google Patents
Graphene carbon nanotube heat conduction slurry and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/08—Cellulose derivatives
- C09D101/26—Cellulose ethers
- C09D101/28—Alkyl ethers
- C09D101/286—Alkyl ethers substituted with acid radicals
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/61—Additives non-macromolecular inorganic
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Abstract
The invention discloses graphene carbon nanotube heat conduction slurry which comprises the following components in parts by weight: 1 to 5 parts of graphite; 1 to 5 parts of carbon nanotubes; 0.5 to 2 parts of dimethylformamide; 0.1 to 1.5 portions of n-butyl alcohol; 5 to 15 parts of epoxy resin; 80 to 95 parts of N-methylpyrrolidone; the invention also discloses a preparation method of the heat-conducting slurry, wherein the carbon nano tubes are mixed between graphene layers in the process of in-situ stripping of graphite into graphene; according to the invention, the carbon nanotubes are directionally inserted between the graphene layers to form ordered arrangement of the graphene and the carbon nanotubes, so that the heat conduction effect is improved.
Description
Technical Field
The invention relates to the technical field of graphene heat conduction materials, in particular to graphene carbon nanotube heat conduction slurry and a preparation method thereof.
Background
The heat dissipation slurry has wide application and convenient use, can be coated in a thin layer or a thick layer, and can also be made into a heat dissipation device. And simultaneously has excellent protection and decoration functions. The main application fields are the following:
the objects needing heat dissipation and temperature reduction can be coated on the objects needing heat dissipation from heat sources, such as CPUs, LED lamps, electrical appliances, cabinets, wires and cables, radiators, fan fans, thermal pipelines, tanks, industrial equipment, buildings, water tanks, vehicles and the like.
And secondly, products needing enhanced heat exchange, such as a vacuum furnace, a vacuum radiator, a vacuum pipeline, a dryer, a heat exchanger, and object equipment with small help conduction area and small convection space, and the like, accelerate heat exchange.
Thirdly, the heat spreading and cooling can be accelerated by using objects with not very high conductivity coefficients, such as plastics, rubber, PVC, ceramics, cement, cloth, leather, paper, glass, wood and the like to accelerate the heat dissipation of the objects.
Fourthly, the heat-dissipating device can be applied to the environment with the ambient temperature higher than the temperature of the object to be cooled, and the object to be cooled is brushed for a plurality of times, so that the heat outside is prevented from being conducted to the object and the heat dissipation and cooling of the object are facilitated.
Chinese patent application publication No. CN104557138A discloses a method for preparing a heat conductive coating of silanized graphene, which comprises activating carboxyl groups on graphene oxide, forming amide bonds between the activated carboxyl groups and amino groups on silane, and coating a solution of silanized graphene oxide on the surface of a substrate by using a spraying method instead of an immersion method, so that the upper groups of silane are connected with the substrate by chemical bonds, thereby effectively improving the adsorption force between graphene and the substrate, and further improving the heat conductivity of the material attached to the substrate. However, the silane upper group is combined with the substrate by high-temperature firing, the heat dissipation performance of the graphene can be weakened after the silane coupling agent is combined with the graphene, the high-temperature sintering cost and the energy consumption are high, and in addition, the silane coupling agent belongs to organic silicon and is easy to crack under high-temperature baking, so that the sintering process difficulty is high.
Disclosure of Invention
The invention provides graphene carbon nanotube heat conduction slurry, wherein carbon nanotubes are directionally inserted between graphene layers to form ordered arrangement of graphene and the carbon nanotubes, so that the heat conduction effect is improved.
In order to solve the technical problem, the technical scheme of the invention is as follows: the graphene carbon nanotube heat conduction slurry comprises the following components in parts by weight:
preferably, the composition also comprises the following components in parts by weight:
5 to 15 portions of sodium carboxymethyl cellulose.
The invention adds sodium carboxymethyl cellulose into the composition, on one hand, the uniformity of dispersion in a system is improved, and on the other hand, the resistance value of a film body is improved.
Further preferably comprises the following components in parts by weight:
most preferably comprises the following components in parts by weight:
in the invention, the same weight parts of graphite and carbon nano tubes are preferably selected, so that the full insertion and arrangement between the graphene and the carbon nano tubes are ensured, a reliable heat conduction path is favorably formed, and the heat conduction effect is improved.
The second purpose of the invention is to provide a preparation method of the graphene carbon nanotube heat conduction slurry, the carbon nanotubes are gradually inserted between graphene layers in the process of layering graphite into graphene to form ordered arrangement of the graphene and the carbon nanotubes, the graphene and the carbon nanotubes are prevented from agglomerating, and the preparation process is simple and convenient.
In order to solve the technical problem, the technical scheme of the invention is as follows: a preparation method of graphene carbon nanotube heat conduction slurry comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, epoxy resin and N-methylpyrrolidone according to the weight parts, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
adding the graphite powder in parts by weight into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and allowing the carbon nano tubes to enter the graphite interlayer gaps along with liquid in the system along with the gradual increase of the graphite interlayer gaps until the graphite is stripped into graphene in a liquid system;
and step three, removing part of the N-methyl pyrrolidone to obtain the graphene carbon nanotube heat conduction slurry with proper viscosity.
The process conditions of the ultrasound in the second step are preferably as follows:
1200W to 2000W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is 15 to 25 minutes. According to the invention, the carbon nano tubes are effectively and uniformly dispersed in an organic liquid system through strong ultrasound, and are uniformly dispersed in an N-methyl pyrrolidone solution of epoxy resin under the action of dimethylformamide and N-butyl alcohol, so that the carbon nano tubes are prevented from being agglomerated.
Preferably, steps one through three are performed under vacuum. According to the invention, graphite is stripped into graphene in liquid, the preparation environment is controlled to be a vacuum condition, so that oxygen in the external environment is reduced, the graphene oxide and the carbon nano tube are oxidized, and the heat conduction effect of the heat conduction slurry after the heat conduction slurry is solidified into a film is weakened.
Preferably, the graphene carbon nanotube thermal conductive slurry subjected to the third step has a viscosity of 60 to 70Pa ×.s. The heat-conducting slurry prepared by the invention has proper viscosity, is beneficial to coating in actual production and keeps good uniformity.
Preferably, the thermal conductivity of the graphene carbon nanotube thermal conductive slurry hardened in the third step is 3000W/mK to 5000W/mK, and the thermal conductive slurry prepared by the method disclosed by the invention has a good thermal conductive effect after being cured into a film.
By adopting the technical scheme, the invention has the beneficial effects that:
the heat-conducting slurry prepared by the invention is characterized in that carbon nanotubes uniformly dispersed in an organic liquid system are gradually inserted between graphene layers along with organic liquid in the graphite stripping process, and dimethylformamide, n-butanol and epoxy resin are added between the graphene layers; the n-butyl alcohol plays an emulsification role to disperse the graphene and the carbon nanotubes and stably disperse the graphene and the carbon nanotubes distributed between the graphene layers, and effectively prevents the graphene and the carbon nanotubes from re-agglomerating due to the attraction of Van der Waals force respectively; thereby obtaining the heat-conducting slurry with uniformly dispersed graphene and carbon nano tubes;
secondly, epoxy resin is uniformly dispersed in an organic solution system in which carbon nano tubes are uniformly dispersed, along with the graphite stripping and layering process, the linear structures of the carbon nano tubes enter between graphene layers along with the continuous increase of gaps between the graphite layers, and the epoxy resin is also guided to be uniformly dispersed between graphene and the carbon nano tubes; the existence of the epoxy resin can also effectively avoid the agglomeration of graphene or carbon nano tubes; the graphene carbon nanotube heat conduction slurry with uniform dispersion is obtained;
after the heat-conducting slurry prepared by the invention is cured, epoxy resin uniformly dispersed between graphene and carbon nano tubes in the slurry is used as a binder to effectively improve the mechanical strength of the cured heat-conducting film, and meanwhile, the carbon nano tubes and the graphene are directionally inserted and arranged to form a film layer, the heat conductivity of the film layer is 3000W/mK-5000W/mK, and the heat-conducting effect is good; the adhesive force of the film layer of the heat-conducting slurry after curing is good.
Thereby achieving the above object of the present invention.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Example 1
The embodiment discloses a preparation method of graphene carbon nanotube heat-conducting slurry and the prepared heat-conducting slurry, and the preparation method specifically comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, epoxy resin and N-methylpyrrolidone according to the weight parts recorded in table 1, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound in the first step are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is between 5 and 15 minutes.
Step two, adding graphite powder in parts by weight recorded in table 1 into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and gradually increasing the interlayer gap of the graphite, wherein the carbon nano tube enters the interlayer gap of the graphite along with liquid in the system until the graphite is stripped into graphene in a liquid system;
the process conditions of the ultrasound in the step two are as follows:
1200W to 2000W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is 15 to 25 minutes.
And step three, removing part of the solvent to obtain the graphene carbon nanotube heat-conducting slurry with the viscosity of 60-70 Pa s.
Example 2
The main differences between this example and example 1 are detailed in table 1.
Example 3
The main differences between this example and example 1 are detailed in table 1.
Example 4
The main differences between this example and example 1 are detailed in table 1.
Example 5
The main differences between this example and example 1 are detailed in table 1.
Example 6
The main differences between this example and example 1 are detailed in table 1.
Example 7
The main differences between this example and example 1 are detailed in table 1.
Example 8
The main differences between this example and example 1 are detailed in table 1.
Example 9
The main differences between this example and example 1 are detailed in table 1.
Comparative example 1
The raw materials used in the embodiment comprise the following components in parts by weight:
2.2 parts of graphene, 2.2 parts of carbon nanotubes, 88 parts of NMP and 13 parts of CMC;
the preparation method of the embodiment is as follows:
under the vacuum condition, the raw material components are mixed according to the parts by weight and then are subjected to ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is from 5 minutes to 15 minutes,
and (4) obtaining uniformly dispersed heat-conducting slurry, and removing the solvent to adjust the proper viscosity.
Comparative example 2
The raw materials used in the embodiment comprise the following components in parts by weight:
2.2 parts of graphene, 2.2 parts of carbon nano tube, 1.5 parts of DMF (dimethyl formamide), 0.8 part of n-butanol, 88 parts of NMP (N-methyl pyrrolidone), and 13 parts of CMC.
The preparation method of the embodiment is as follows:
under the vacuum condition, the raw material components are mixed according to the parts by weight and then are subjected to ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is from 5 minutes to 15 minutes,
and (4) obtaining uniformly dispersed heat-conducting slurry, and removing the solvent to adjust the proper viscosity.
Example 3
The raw materials used in the embodiment comprise the following components in parts by weight:
2.2 parts of graphene, 2.2 parts of carbon nanotubes, 10 parts of epoxy resin, 88 parts of NMP and 13 parts of CMC.
The preparation method of the embodiment is as follows:
under the vacuum condition, the raw material components are mixed according to the parts by weight and then are subjected to ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is from 5 minutes to 15 minutes,
and (4) obtaining uniformly dispersed heat-conducting slurry, and removing the solvent to adjust the proper viscosity.
Example 4
The raw materials used in the embodiment comprise the following components in parts by weight:
2.2 parts of graphene, 2.2 parts of carbon nanotubes, 1.5 parts of DMF (dimethyl formamide), 0.8 part of n-butanol, 10 parts of epoxy resin, 88 parts of NMP (N-methyl pyrrolidone), and 13 parts of CMC.
The preparation method of the embodiment is as follows:
under the vacuum condition, the raw material components are mixed according to the parts by weight and then are subjected to ultrasonic treatment to obtain a uniformly dispersed system;
the process conditions of the ultrasound are as follows:
600W to 1200W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is from 5 minutes to 15 minutes,
and (4) obtaining uniformly dispersed heat-conducting slurry, and removing the solvent to adjust the proper viscosity.
Table 1 examples 1 to 9 and comparative examples 1 to 4 thermally conductive paste raw material components and parts by weight
| Item | Graphite | Carbon nanotube | DMF | N-butanol | Epoxy resin | NMP | CMC |
| Example 1 | 1.0 | 2.0 | 0.5 | 0.1 | 5 | 80 | 5 |
| Example 2 | 1.2 | 1.0 | 0.9 | 0.6 | 8 | 86 | 8 |
| Example 3 | 1.6 | 1.6 | 1.7 | 0.8 | 12 | 90 | / |
| Example 4 | 1.8 | 3.6 | 2 | 1.1 | 6 | 82 | / |
| Example 5 | 2.2 | 2.2 | 1.5 | 0.8 | 10 | 88 | 13 |
| Example 6 | 3.0 | 3.0 | 1.7 | 1.5 | 12 | 92 | 10 |
| Example 7 | 3.5 | 3.5 | 0.9 | 1.5 | 15 | 95 | 15 |
| Example 8 | 4.0 | 4.0 | 0.5 | 1.5 | 15 | 80 | 10 |
| Example 9 | 5.0 | 5.0 | 2 | 1.5 | 8 | 88 | 5 |
| Comparative example 1 | 2.2 | 2.2 | / | / | / | 88 | 13 |
| Comparative example 2 | 2.2 | 2.2 | 1.5 | 0.8 | / | 88 | 13 |
| Comparative example 3 | 2.2 | 2.2 | / | / | 10 | 88 | 13 |
| Example 4 | 2.2 | 2.2 | 1.5 | 0.8 | 10 | 88 | 13 |
Respectively coating the heat-conducting slurry prepared in the embodiment and the comparative example on copper foil, curing and forming a film, and then sequentially testing the adhesive force, the heat conductivity coefficient and the volume resistance by using a flexibility tester, a hundred-grid cutter and a heat conductivity coefficient tester; the flexibility test execution standard refers to GB 1731-.
TABLE 2 tabulation of the hardened performance indexes of the thermally conductive pastes obtained in examples 1 to 9 and comparative examples 1 to 4
| Item | Viscosity (Pa.s) | Adhesion (grade) | Thermal conductivity (W/m.K) | Volume resistance (omega. cm) |
| Example 1 | 60 | 0 | 2450 | 3.1×1010 |
| Example 2 | 63 | 0 | 2300 | 3.5×1010 |
| Example 3 | 61 | 0 | 2600 | 3.0×1010 |
| Example 4 | 70 | 0 | 3200 | 2.5×1010 |
| Example 5 | 68 | 0 | 3300 | 5.1×1010 |
| Example 6 | 65 | 0 | 4400 | 3.8×1010 |
| Example 7 | 66 | 0 | 4800 | 3.6×1010 |
| Example 8 | 64 | 0 | 5100 | 3.2×1010 |
| Example 9 | 70 | 0 | 5200 | 2.6×1010 |
| Comparative example 1 | 58 | 1 | 1750 | 1.8×1010 |
| Comparative example 2 | 56 | 1 | 1600 | 1.7×1010 |
| Comparative example 3 | 54 | 1 | 1700 | 1.8×1010 |
| Comparative example 4 | 56 | 0 | 1800 | 1.9×1010 |
As can be seen from tables 1 and 2 and the preparation process, in examples 1 to 9, in the in-situ graphite delamination process, the carbon nanotubes uniformly dispersed in the liquid phase system continuously enter between the graphene along with DMF, n-butanol, CMC and epoxy resin under the promotion of ultrasound, the DMF, n-butanol and CMC synergistically promote the stable dispersion of the thermal conductive slurry, and the carbon nanotubes are distributed between the graphene, so that the graphene or the carbon nanotubes are effectively prevented from being agglomerated; graphene and carbon nano-particles are uniformly dispersed in NMP dissolved with DMF, n-butyl alcohol, CMC and epoxy resin, and after the graphene and the carbon nano-particles are hardened as a film, the epoxy resin is uniformly distributed between the graphene and the carbon nano-particles to serve as a binder, so that the adhesive force of the film layer is effectively improved.
Comparative examples 1 to 4 heat conductive pastes were prepared by mixing the same amount of graphene as in example 5 with carbon nanotubes; from the data of the heat-conducting film layer after hardening, the heat-conducting performance and the volume resistance of the comparative examples 1 to 4 are both obviously lower than those of the example 5 and are far lower than the film layer performance of the heat-conducting slurry obtained in the other examples; the method has the advantages that the graphite is more uniformly mixed with the carbon nano tube in the process of in-situ stripping and layering to form the graphene, and the heat-conducting slurry with excellent performance is favorably obtained.
The invention also improves the stability of the system by adding CMC into the liquid phase system, improves the volume resistance of the film layer after the heat-conducting slurry is hardened, and is beneficial to improving the further application of the heat-conducting slurry.
Claims (9)
1. The graphene carbon nanotube heat conduction slurry is characterized in that:
comprises the following components in parts by weight:
2. the graphene-carbon nanotube thermal conductive paste according to claim 1, wherein:
the composition also comprises the following components in parts by weight:
5 to 15 portions of sodium carboxymethyl cellulose.
3. The graphene-carbon nanotube thermal conductive paste according to claim 2, wherein:
comprises the following components in parts by weight:
4. the graphene-carbon nanotube thermal conductive paste according to claim 2, wherein:
comprises the following components in parts by weight:
5. a method for preparing the graphene carbon nanotube thermal conductive paste of any one of claims 2 to 4, wherein:
the method comprises the following steps:
step one, mixing carbon nano tubes, dimethylformamide, N-butanol, epoxy resin, N-methylpyrrolidone and sodium carboxymethylcellulose according to the weight parts, and then carrying out ultrasonic treatment to obtain a uniformly dispersed system;
adding the graphite powder in parts by weight into the uniformly dispersed system obtained in the step one, gradually layering graphite under the action of ultrasound, and allowing the carbon nano tubes to enter the graphite interlayer gaps along with liquid in the system along with the gradual increase of the graphite interlayer gaps until the graphite is stripped into graphene in a liquid system;
and step three, removing part of the N-methyl pyrrolidone to obtain the graphene carbon nanotube heat conduction slurry with proper viscosity.
6. The method for preparing the graphene-carbon nanotube thermal conductive paste according to claim 5, wherein: the process conditions of the ultrasound in the step two are as follows:
1200W to 2000W;
the ultrasonic starting/stopping time is 3s/5s respectively;
the total duration of sonication is 15 to 25 minutes.
7. The method for preparing the graphene-carbon nanotube thermal conductive paste according to claim 5, wherein: the first step to the third step are carried out under vacuum condition.
8. The method for preparing the graphene-carbon nanotube thermal conductive paste according to claim 5, wherein: and the viscosity of the graphene carbon nanotube heat-conducting slurry obtained in the third step is 60-70 Pa s.
9. The method for preparing the graphene-carbon nanotube thermal conductive paste according to claim 5, wherein: and the thermal conductivity of the graphene carbon nanotube heat conduction slurry hardened in the third step is 3000W/m K to 5000W/m K.
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