CN108047822B - Utilize the method for shear thickening system removing preparing graphite alkene heat conduction and heat radiation composite material - Google Patents
Utilize the method for shear thickening system removing preparing graphite alkene heat conduction and heat radiation composite material Download PDFInfo
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Abstract
The invention discloses a kind of methods using shear thickening system removing preparing graphite alkene heat conduction and heat radiation composite material.Contain heat filling in the shear thickening system, after it is mixed with graphite raw material, mixing liquid is set to be in the high viscosity state of shear thickening by mechanical shearing, constantly graphene is stripped out from graphite, greatly improve the charge stripping efficiency and yield of graphene, and synchronizing realizes the evenly dispersed of graphene and heat filling, and the heat conduction and heat radiation coefficient of composite material can be improved.Furthermore, the present invention is combined into one by the preparation of graphene and its with the dispersion two procedures of heat filling, graphene heat conduction and heat radiation composite material is prepared by a step process, avoid the twice dispersing process for isolating and purifying process and graphene of graphene, to greatly simplifie production procedure, the production cycle is shortened, production cost can be greatly reduced.
Description
Technical field
The present invention relates to a kind of graphene heat conduction and heat radiation composite material and preparation methods, particularly relate to a kind of utilize and shear
The method of thickened systems removing preparing graphite alkene heat conduction and heat radiation composite material.
Background technique
A large amount of heat can be generated in electronic device operational process, the heat conduction and heat radiation efficiency for improving material can increase electronics device
The stability of part and service life.Such as LED chip temperature reduces by 10 DEG C, the service life will double.For the heat dissipation of electronic component
Problem main thought is itself thermal resistance and increase external cooling mechanism for including reduction electronic component.Wherein, itself is reduced
Thermal resistance method has: selecting suitable Heat Conduction Material, increases interface Heat Conduction Material, improves manufacture craft etc., but these methods drop
Temp effect is limited and increases device application cost.The main method for increasing external cooling mechanism is fin technology.Fin
Technology is most popular heat transfer enhancement technology in electronic equipment dissipating heat and engineering, is primarily referred to as depending on base by increasing
Extended surface on plinth surface strengthens heat-sinking capability, i.e. gilled radiator.Coating technology is applied to gilled radiator,
Its heat dissipation performance can be enhanced, while heat radiation coating can preferably meet electronic equipment lightweight and portable requirement.
Conventional heat radiation coating is made of high radiant rate and high thermal conductivity filler and binder.Graphene is by single layer of carbon atom
Constitute, have the characteristics that high heat conductance, high conductivity, high-specific surface area, high mechanical strength, can be widely applied to environment, the energy,
The fields such as composite material, composite coating.Graphene has extraordinary heat-conductive characteristic, and the thermal coefficient of single-layer graphene is up to
5300W/mK, thermal emissivity rate are excellent heat conduction and heat radiation fillers close to 1.Chinese invention patent CN201610414796.4 is by stone
Black alkene and high radiant rate filler are compound, and are aided with hard functional material, and binder then is added and auxiliary reagent obtains graphene
Heat radiation coating, the material have good thermal coefficient and excellent wear-resisting property.Chinese invention patent
CN201610660212.1 discloses a kind of graphene heat radiation coating and preparation method thereof, including mixed uniformly A agent and B agent,
The A agent includes fluorocarbon resin, graphene 5-15% and dispersing agent etc., and the B agent includes mixed solvent and curing agent, is used
It is preceding A agent and B agent are mixed evenly, filtered, cure after could use.Chinese invention patent CN201610282181.0 hair
It is bright that a kind of graphene heat radiation coating applied to LED light is provided, be by pure water, water-based acrylic resin, waterborne polyurethane resin,
YH-82 modified amine, cobalt naphthenate, bortz powder, bentonite powder, silicon powder, titanate coupling agent, titanium dioxide and graphene etc.
It is sufficiently mixed and is made.
It is all to mix graphene powder with heat filling, binder that above all patents of invention, which prepare the mode of heat radiation coating,
Obtain graphene heat-dissipation paint.Wherein, it prepares graphene powder and the complicated procedures of forming such as is separated, purified, dried, together
When, should during graphene nanometer sheet can inevitably reunite, this necessarily causes the secondary of graphene and heat filling to mix point
It dissipates unevenly, greatly affected the performance of graphene composite radiating coating.
Summary of the invention
In view of the above problems, removing preparing graphite using shear thickening system the purpose of the present invention is to provide a kind of
The method of alkene heat conduction and heat radiation composite material, this method can simplify the preparation process of graphene heat conduction and heat radiation composite material, simultaneously
Improve the heat conduction and heat radiation performance of material.
To achieve the above object, provided by the present invention to be dissipated using shear thickening system removing preparing graphite alkene is thermally conductive
The method of hot composite material includes the following steps: to mix the graphite raw material containing heat filling with shear thickening system
It to mixing liquid, is acted on by mechanical shearing, so that mixing liquid is in the high viscosity state of shear thickening, so that graphene be shelled
From into mixing liquid, obtaining the composite fluid containing graphene and heat filling, as graphene heat conduction and heat radiation composite material.
Wherein, shear thickening system is when by extraneous graviational interaction, and system viscosity value occurs significant, nonlinear with stress increase
It sharply increases, and with the disappearance of stress, viscosity is rapidly reduced to the special system restored again.The system is by extraneous high
Viscosity steeply rises when speed shearing, to efficiently remove graphite at graphene, when extraneous shear rate is removed, system viscosity
It reduces, restores, facilitate application and coating.
Preferably, the shear thickening system includes that ionic liquid-heat filling system, polyvinyl alcohol-Boratex-are thermally conductive
Filler systems, polyethylene glycol-heat filling system.Wherein, ionic liquid-heat filling system is by ionic liquid and heat filling
It configures, polyethylene glycol-heat filling system is configured by polyethylene glycol and heat filling, and polyvinyl alcohol-Boratex-is led
Hot filler systems are configured by polyvinyl alcohol, Boratex and heat filling.
Preferably, the ionic liquid is made of cation and anion, and the cation is quaternary ammonium salt cationic, quaternary phosphonium
One of salt cation, pyridine salt cation and imidazoles salt cation are a variety of, and the anion is AlCl4 -, FeCl4 -、
BF4 -、PF6 -、CF3COO-、CF3SO3 -、(CF3SO2)2N-、SbF6 -、Cl-、Br-One of or it is a variety of.
Preferably, the ionic liquid includes 1- butyl -3- methylimidazole hexafluorophosphate, 1- butyl -3- methylimidazole
Tetrafluoroborate, 1- ethyl-3-methylimidazole tetrafluoroborate, 1- hexyl -3- methyl imidazolium tetrafluoroborate and 1- ethoxy -
One of 3- methyl imidazolium tetrafluoroborate is a variety of.
Preferably, the heat filling includes silica, aluminium oxide, boron nitride, aluminium nitride, magnesia, zinc oxide, oxygen
Change one of nickel, copper oxide, beryllium oxide, carbon ball, polymer microballoon and carbon nanotube or a variety of, the size of the heat filling
For 1nm~100 μm, shape includes spherical, tubulose, sheet etc..Above-mentioned heat filling has high-heating radiation characteristic, further increases
Thermally conductive, the heat dissipation performance of material.
Preferably, further include the steps that binder is added into the mixing liquid, to improve the bonding energy of composite coating
Power and mechanical strength.
Preferably, the binder include epoxy resin, it is polyaminoester emulsion, acrylic emulsion, SBR emulsion, aqueous
One of epoxy emulsion, ptfe emulsion, solvent borne polyurethane solution, solvent-type acrylic solution are a variety of.
Preferably, the additional amount of the shear thickening system is 50 mass parts, the additional amount of the graphite raw material is 3~
10 mass parts, the additional amount of the binder are 20~80 mass parts.
Preferably, the shearing equipment include three-roller open mill, mixer, Haake torque rheometer, ball mill, in sand mill
It is one or more.
Preferably, the graphite raw material includes natural graphite, micro crystal graphite, amorphous graphite, expanded graphite, highly directional stone
It is black, artificial graphite one or more.
The beneficial effects of the present invention are: the present invention is closed by the preparation of graphene and its with the dispersion two procedures of heat filling
Two be one, passes through the excellent graphene heat conduction and heat radiation composite material of a step process processability.This method utilizes shear thickening body
The shear thickening of system acts on, and greatly improves the charge stripping efficiency and yield of graphene；Eliminate the separation of graphene, purifying,
The complicated procedures of forming such as dry avoid graphene sheet layer and self aggregation occur, and promote graphene in the evenly dispersed of heat filling,
Promote the heat conduction and heat radiation performance of composite material；Twice dispersing process of the graphene in heat filling is eliminated, production is shortened
The production cost of graphene heat conduction and heat radiation composite material can be greatly reduced in period；Heat filling in shear thickening system plays
Double action improved the charge stripping efficiency of graphene both as the functional reagent in shear thickening system, and as auxiliary heat transfer
Functional stuffing, improve the heat conduction and heat radiation performance of composite material；The composite material can also be further mixed with binder and/or auxiliary agent
Dispersion is closed, the graphene heat conduction and heat radiation composite material for being suitble to different application scene is obtained, extends its application field.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the graphene in graphene heat conduction and heat radiation composite material prepared by embodiment 3.
Fig. 2 is the scanning electron microscope of the graphene in graphene heat conduction and heat radiation composite material prepared by embodiment 5
Picture.
Specific embodiment
Side provided by the present invention using shear thickening system removing preparing graphite alkene heat conduction and heat radiation composite material
Method includes the following steps: graphite raw material and the shear thickening system containing heat filling being mixed to get mixing liquid, pass through
Mechanical shearing effect makes mixing liquid be in the high viscosity state of shear thickening, constantly removes graphene from graphite raw material
Out, the composite fluid containing graphene and heat filling is obtained, binder is added, is uniformly mixed, as graphene is compound
Heat-dissipation paint.
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1
The present embodiment is led using ionic liquid-heat filling system as shear thickening system removing preparing graphite alkene
Hot heat dissipation composite material the steps include: to take nano silica 15g, be added to the 1- butyl -3- methylimidazole tetrafluoro boron of 50mL
In hydrochlorate, 3g graphite is added in ultrasonic disperse 1h, and ball milling shears 8h in ball grinder, continuously adds 20g SBR emulsion, mixes ball
1h is ground, graphene composite heat-conducting heat radiation coating can be obtained.
Embodiment 2
The present embodiment is using polyvinyl alcohol-Boratex-heat filling system as the removing graphite preparation of shear thickening system
Graphene heat conduction and heat radiation composite material the steps include: to take 15g boron nitride and 30g Boratex, and being added to 300g mass fraction is
In the polyvinyl alcohol water solution of 10wt%, 10g graphite is added in ultrasonic disperse 1h, is transferred to ball milling in ball grinder and is sheared 8h, continues to add
Enter 80g aqueous polyurethane emulsion, mixing and ball milling 1h obtains graphene composite heat-conducting heat radiation coating.
Embodiment 3
The present embodiment is led using polyethylene glycol-heat filling system as shear thickening system removing preparing graphite alkene
Hot heat dissipation composite material the steps include: to take nano magnesia 15g, nano silica 15g, addition 50g polyethylene glycol, ultrasound
Disperse 1h, 5g graphite is added, be transferred in ball grinder ball milling and shear 8h, continuously adds 50g acrylic acid ester emulsion, mixing and ball milling 1h,
Obtain graphene composite heat-conducting heat radiation coating.
Embodiment 4
The present embodiment is led using ionic liquid-heat filling system as shear thickening system removing preparing graphite alkene
Hot heat dissipation composite material the steps include: to take nano aluminium oxide 30g, -3 methyl tetrafluoroborate of 30mL 1- hydroxyethyl imidazole be added
In, 10g graphite is added in ultrasonic disperse 1h, is transferred to high-speed shearing machine shearing 8h, continuously adds 110g aqueous polyurethane emulsion, mix
It closes ball milling 1h and obtains graphene composite heat-conducting heat radiation coating.
Embodiment 5
The present embodiment is led using ionic liquid-heat filling system as shear thickening system removing preparing graphite alkene
Hot heat dissipation composite material the steps include: to take nano silica 15g, and the 1- butyl -3- methylimidazole tetrafluoro boric acid of 50mL is added
In salt, 5g graphite is added in ultrasonic disperse 1h, is transferred to high-speed shearing machine shearing 8h, is continuously added 50g aqueous epoxy resins, mix
Ball milling 1h obtains graphene composite heat-conducting heat radiation coating.
Test case
The graphene heat radiation coating that each embodiment is prepared is subjected to heat dissipation performance test as follows: will be tested
Component coats heat radiation coating, is placed into heat generating components (heating power 50W, heat dissipation area about 100cm2) on, continual and steady 1h is surveyed
Heat generating components temperature is tried, record temperature of heating elements obtains heat radiation coating heat dissipation effect.
Test result is listed in the table below:
The test of 1 graphene heat conduction and heat radiation composite material heat dissipation performance of table
| Each sample number | Heater element equilibrium temperature | Opposite blank sample temperature difference |
| Reference sample is without heat radiation coating | 65℃ | 0℃ |
| 1 graphene heat conduction and heat radiation composite coating of embodiment | 55℃ | 10℃ |
| 2 graphene heat conduction and heat radiation composite coating of embodiment | 56℃ | 9℃ |
| 3 graphene heat conduction and heat radiation composite coating of embodiment | 54℃ | 11℃ |
| 4 graphene heat conduction and heat radiation composite coating of embodiment | 57℃ | 8℃ |
| 5 graphene heat conduction and heat radiation composite coating of embodiment | 55℃ | 10℃ |
As can be seen from the above table, the graphene composite heat-conducting heat radiation coating prepared by the present invention can reduce heater element and stablize
8-11 DEG C of temperature, there is excellent heat conduction and heat radiation performance.
Graphene in graphene composite heat-conducting heat radiation coating that embodiment 3, embodiment 5 obtain is separated, respectively
It is observed by transmission electron microscope, scanning electron microscope, gained picture is shown in Fig. 1, Fig. 2 respectively.It can from Fig. 1
Out, embodiment 3 has prepared the graphene of few number of plies structural integrity.Figure it is seen that embodiment 5 successfully shells graphite
From having obtained the complete graphene nanometer sheet of structure.
Claims (8)
1. a kind of method using shear thickening system removing preparing graphite alkene heat conduction and heat radiation composite material, feature exist
In method includes the following steps: the shear thickening system containing heat filling and graphite raw material are mixed to get mixed liquor
Body makes mixing liquid be in the high viscosity state of shear thickening, to removing graphene to mixing liquid by mechanical shearing
In, obtain the composite fluid containing graphene and heat filling, as graphene heat conduction and heat radiation composite material；The shear thickening
System includes ionic liquid-heat filling system, polyvinyl alcohol-Boratex-heat filling system, polyethylene glycol-heat filling
System；The heat filling includes silica, aluminium oxide, boron nitride, aluminium nitride, silicon carbide, magnesia, zinc oxide, oxidation
One of nickel, copper oxide, beryllium oxide, carbon ball, polymer microballoon and carbon nanotube are a variety of, and the size of the heat filling is
1nm~100 μm.
2. according to claim 1 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: this method further includes the steps that binder is added into the mixing liquid.
3. according to claim 2 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: the binder includes epoxy resin, polyaminoester emulsion, acrylic emulsion, SBR emulsion, water
One of property epoxy emulsion, ptfe emulsion, solvent borne polyurethane solution, solvent-type acrylic solution are a variety of.
4. according to claim 2 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: the additional amount of the shear thickening system is 50 mass parts, and the additional amount of the graphite raw material is 3
~10 mass parts, the additional amount of the binder are 20~80 mass parts.
5. according to claim 1 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: the ionic liquid-heat filling system is configured by ionic liquid and heat filling；It is described poly-
Vinyl alcohol-Boratex-heat filling system is configured by polyvinyl alcohol, Boratex and heat filling；The polyethylene glycol-is led
Hot filler systems are configured by polyethylene glycol and heat filling.
6. according to claim 5 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: the ionic liquid by cation and anion constitute, wherein it is described cation be quaternary ammonium salt sun from
One of son, quaternary phosphonium salt cation, pyridine salt cation and imidazoles salt cation are a variety of, and the anion is AlCl4 -,
FeCl4 -、BF4 -、PF6 -、CF3COO-、CF3SO3 -、(CF3SO2)2N-、SbF6 -、Cl-、Br-One of or it is a variety of.
7. according to claim 6 remove preparing graphite alkene heat conduction and heat radiation composite material using shear thickening system
Method, it is characterised in that: the ionic liquid includes 1- butyl -3- methylimidazole hexafluorophosphate, 1- butyl -3- methylimidazole
Tetrafluoroborate, 1- ethyl-3-methylimidazole tetrafluoroborate, 1- hexyl -3- methyl imidazolium tetrafluoroborate and 1- ethoxy -
One of 3- methyl imidazolium tetrafluoroborate is a variety of.
8. according to any one of claims 1 to 4 dissipate using shear thickening system removing preparing graphite alkene is thermally conductive
The method of hot composite material, it is characterised in that: used mechanized clipping equipment includes three-roller open mill, mixer, Haake stream
Become one of instrument, ball mill, sand mill or a variety of.
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| CN104327795A (en) * | 2014-01-08 | 2015-02-04 | 中物功能材料研究院有限公司 | Preparation method of shear thickening liquid |
| CN105819438A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for preparing nanometer graphene materials in large scale mode through hydraulic shearing |
| CN106564890A (en) * | 2016-11-11 | 2017-04-19 | 中南民族大学 | Method for preparing graphene by assisting graphite stripping with salt mixture |
| CN106744870A (en) * | 2016-10-25 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of abrasive media that Graphene is peeled off for slurry grinding |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014062226A1 (en) * | 2012-10-19 | 2014-04-24 | Rutgers, The State University Of New Jersey | In situ exfoliation method to fabricate a graphene-reinforced polymer matrix composite |
| CN104327795A (en) * | 2014-01-08 | 2015-02-04 | 中物功能材料研究院有限公司 | Preparation method of shear thickening liquid |
| CN105819438A (en) * | 2016-05-06 | 2016-08-03 | 成都新柯力化工科技有限公司 | Method for preparing nanometer graphene materials in large scale mode through hydraulic shearing |
| CN106744870A (en) * | 2016-10-25 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of abrasive media that Graphene is peeled off for slurry grinding |
| CN106564890A (en) * | 2016-11-11 | 2017-04-19 | 中南民族大学 | Method for preparing graphene by assisting graphite stripping with salt mixture |
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