CN109735308A - Adjustable uncured graphene composite material of thermal conductivity and the preparation method and application thereof - Google Patents
Adjustable uncured graphene composite material of thermal conductivity and the preparation method and application thereof Download PDFInfo
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- CN109735308A CN109735308A CN201811636475.4A CN201811636475A CN109735308A CN 109735308 A CN109735308 A CN 109735308A CN 201811636475 A CN201811636475 A CN 201811636475A CN 109735308 A CN109735308 A CN 109735308A
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- composite material
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- thermal conductivity
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Abstract
The invention belongs to field of material technology, are related to adjustable uncured graphene composite material of thermal conductivity and the preparation method and application thereof.The composite material includes graphene nanometer sheet dispersion liquid and organic solvent, and the mass ratio of the graphene nanometer sheet and dispersing agent is 0.05~0.2:1；The organic solvent includes N-Methyl pyrrolidone；The dispersing agent is polyvinylpyrrolidone.Doped with non-oxidized graphite alkene in the adjustable uncured graphene composite material of thermal conductivity of the invention, makes it in aligning by magnetic field regulation, can according to need and adjust uncured graphene composite material thermal conductivity at any time.
Description
Technical field
The invention belongs to field of material technology, are related to the adjustable composite heat conducting material of thermal conductivity, and in particular to thermal conductivity can
The uncured graphene composite material and the preparation method and application thereof adjusted.
Background technique
Thermally conductive is always the topic that industrial circle and Material Field are paid close attention to.In chemical field, it usually needs pass through
External heat source heats raw material, and when desired heat, which quickly move through container, passes to raw material, container needs to have larger
Thermal conductivity；When heating temperature reaches technique initialization temperature, it usually needs carry out the heat preservation of a period of time, container needs to have at this time
Standby lesser thermal conductivity；Or need container to have lesser thermal conductivity during heating to realize that high efficiency heats, it radiates
Need biggish thermal conductivity in the process to realize and be quickly cooled down.
However, meeting the needs of industrial circle there is no a kind of effective adjustable material of thermal conductivity at present.Height is led
Conductivity material, currently used Heat Conduction Material are mostly the metal materials such as copper, aluminium.Some composite heat conducting materials are for example thermally conductive in recent years
Plastics etc. are attempted due to the advantages that it has low easy plasticity, light weight and cost and high-insulativity applied to LED and lithium electricity
In the fields Related products such as pond heat dissipation.Current Heat Conduction Material is mostly with metal oxide ceramic body, carbon fiber and graphite
As dopant, thermal conductivity small (bulk thermal conductivities such as oxide ceramic are less than 100W/ (mK)), doping are limited (carbon fiber
Peacekeeping graphite dopping amount is excessively high will lead to improve its electric conductivity) etc. factors lead to the heat-conducting plastic thermal conductivity being finally combined
Less than 10W/ (mK).As for thermal insulation material, the main product of last century Mo is perlite, rock cotton insulation material；Current
Main product is the organic insulation materials such as styrofoam, polyurethane；Future, compound, multi-functional heat-insulating heat-preserving material will become
Important developing direction.
Graphene is as being that a kind of two dimension for forming hexagonal cell shape lattice structure by carbon atom with sp2 hybridized orbit is brilliant
Body thin film, only a carbon atom thickness, it is common Heat Conduction Material that thermal conductivity theoretical prediction, which reaches 6000W/ (mK), in face
10-20 times of (room temperature thermal conductivity: copper 393.6W/ (mK)；Aluminium 238.6W/ (mK)).Therefore graphene is compound organic thermally conductive
High heating conduction may be implemented in material.In addition, interact between two-dimensional graphene face by Van der Waals force, secondly
The heating conduction tieed up between graphene face is very poor.
Existing graphene composite heat conduction film needs to be arranged multilayered thermally-conductive film, pyroconductivity horizontally and vertically
Although difference is huge, thermal conductivity is fixed, and can not be adjusted in use.
Summary of the invention
It is an object of the invention to overcome drawbacks described above of the existing technology, using the thermally conductive anisotropy of graphene,
The adjustable organic composite material of thermal conductivity is prepared to meet the needs of industrial.
The present invention, which is that the following technical solution is employed, to be realized:
A kind of adjustable uncured graphene composite material of thermal conductivity, the composite material include graphene nanometer sheet, dispersion
The mass ratio of agent and organic solvent, the graphene nanometer sheet and dispersing agent is 0.05~0.2:1, graphene nanometer sheet and organic
The mass volume ratio of solvent is 1~2mg/mL；
The organic solvent is N-Methyl pyrrolidone；The dispersing agent is polyvinylpyrrolidone.
Specifically, the graphene nanometer sheet is the stratiform accumulation body of non-oxidized graphite alkene.
The present invention provides the preparation methods of the adjustable uncured graphene composite material of above-mentioned thermal conductivity, including following step
It is rapid:
(1) it disperses highly oriented pyrolytic graphite in dispersing agent, the stone of non-oxide reduction is prepared using high-shear emulsion machine
The mass ratio of black alkene nanometer sheet dispersion liquid, highly oriented pyrolytic graphite and dispersing agent is 1:100；
(2) graphene nanometer sheet dispersion liquid made from step (1) is mixed with organic solvent, stirring is uniformly mixed into it
The adjustable uncured graphene composite material of thermal conductivity.
High-shear emulsion machine removes graphene nanometer sheet in above-mentioned steps (1), comprising the following steps:
It is handled graphite flakes 12 hours, 10000rpm/min by FLUKO FA25-25G high shear mixing head, wherein stone
Black scale and N-Methyl pyrrolidone mix；Whole system is put into mixture of ice and water to prevent mistake during shear-mixed
Heat.It is stood overnight after the completion of shearing, supernatant is taken to be centrifuged 1 hour under 7000rpm revolving speed, supernatant is taken to obtain non-oxide go back
Former graphene nanometer sheet dispersion liquid.
It is 100~200mg/ that highly oriented pyrolytic graphite, which is scattered in the concentration in N-Methyl pyrrolidone, in above-mentioned steps (1)
mL。
The present invention also provides the applications of the adjustable uncured graphene composite material of above-mentioned thermal conductivity, are used to prepare and pass through
The heat-transfer device of magnetic field regulation.
Above-mentioned heat-transfer device includes conducting-heat elements and induction coil；
The conducting-heat elements are rectangular parallelepiped structure, including sealing tempered glass, and are sealed in the heat inside tempered glass
The adjustable uncured graphene composite material of conductance, the composite material are completely filled with sealing tempered glass；
The induction coil includes along conducting-heat elements long side, and two for being wound in conducting-heat elements upper and lower part respectively are parallel
Coil, parallel coil intersect at conducting-heat elements broadside；And intersect with parallel coil, one for being wound in tempered glass side is hung down
Linear coil；The both ends of each coil are respectively arranged with wire connecting power anode and cathode.
Specifically, the number of turns of vertical coil is 5~50 circles.
The number of turns of each parallel coil is directly proportional to the conducting-heat elements edge length that parallel coil is vertical, ratio 50
~100mm/ circle.
Compared with prior art, the beneficial effect that the present invention obtains is:
(1) graphene using the material of the method for the present invention preparation because of inside with oriented alignment, therefore heat with higher
Conductance can satisfy the requirement in application to material heat dissipation performance.
(2) material of the method for the present invention preparation is different from traditional solid material, is graphene solution (uncured processing),
It is by way of heat transfer and convection current while to carry out that its is thermally conductive, relative to existing solid union material, greatly improves it and leads
Heating rate.
(3) composite material in the present invention is non-solid, and the arrangement of graphene can influence its heating conduction, therefore, can root
Need to adjust its thermal conductivity according to production, to meet the needs of different.
Detailed description of the invention
Fig. 1 is heat-transfer device positive structure schematic of the present invention；
Fig. 2 is heat-transfer device side structure schematic diagram of the present invention；
Fig. 3 is heat-transfer device cross-sectional view of the present invention.
In figure respectively mark it is as follows: 1 conducting wire, 2 conducting wires, 3 conducting wires, 4 conducting wires, 5 vertical coils, 6 parallel coils, 7 tempered glass,
The adjustable uncured graphene composite material of 8 thermal conductivities.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, but the present invention is not limited thereto.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material,
Using analytical reagents, unless otherwise specified, commercially obtain.
One, the adjustable uncured graphene composite material of thermal conductivity is prepared
Embodiment 1
(1) mass ratio of highly oriented pyrolytic graphite and dispersing agent is 1:100, passes through FLUKO FA25-25G high shear mixing
Head processing graphite flakes 12 hours, 10000rpm/min, wherein graphite flakes and N-Methyl pyrrolidone mix, and concentration is
100mg/mL；Whole system is put into mixture of ice and water to prevent from overheating during shear-mixed.It is placed after the completion of shearing
Overnight, it takes supernatant to be centrifuged 1 hour under 7000rpm revolving speed, supernatant is taken to obtain the graphene nanometer sheet of non-oxide reduction
Dispersion liquid.
(2) dispersion liquid of graphene nanometer sheet is mixed with N-Methyl pyrrolidone, stirring makes it be uniformly mixed into graphite
Alkene organic mixture, the mass volume ratio for controlling graphene nanometer sheet and organic solvent is 1~2mg/mL.
Embodiment 2
(1) mass ratio of highly oriented pyrolytic graphite and dispersing agent is 1:100, passes through FLUKO FA25-25G high shear mixing
Head processing graphite flakes 12 hours, 10000rpm/min, wherein graphite flakes and N-Methyl pyrrolidone mix, and concentration is
150mg/mL；Whole system is put into mixture of ice and water to prevent from overheating during shear-mixed.It is placed after the completion of shearing
Overnight, it takes supernatant to be centrifuged 1 hour under 7000rpm revolving speed, supernatant is taken to obtain the graphene nanometer sheet of non-oxide reduction
Dispersion liquid.
(2) dispersion liquid of graphene nanometer sheet is mixed with N-Methyl pyrrolidone, stirring makes it be uniformly mixed into graphite
Alkene organic mixture, the mass volume ratio for controlling graphene nanometer sheet and organic solvent is 1~2mg/mL.
Embodiment 3
(1) mass ratio of highly oriented pyrolytic graphite and dispersing agent is 1:100, passes through FLUKO FA25-25G high shear mixing
Head processing graphite flakes 12 hours, 10000rpm/min, wherein graphite flakes and N-Methyl pyrrolidone mix, and concentration is
200mg/mL；Whole system is put into mixture of ice and water to prevent from overheating during shear-mixed.It is placed after the completion of shearing
Overnight, it takes supernatant to be centrifuged 1 hour under 7000rpm revolving speed, supernatant is taken to obtain the graphene nanometer sheet of non-oxide reduction
Dispersion liquid.
(2) dispersion liquid of graphene nanometer sheet is mixed with N-Methyl pyrrolidone, stirring makes it be uniformly mixed into graphite
Alkene organic mixture, the mass volume ratio for controlling graphene nanometer sheet and organic solvent is 1~2mg/mL.
Two, using the heat-transfer device of the adjustable organic composite material of thermal conductivity
Embodiment 4
Described in the present embodiment by magnetic field regulate and control heat-transfer device include conducting-heat elements and induction coil；
Wherein, conducting-heat elements are rectangular parallelepiped structure, including sealing tempered glass 7, and are sealed in 7 inside sky of tempered glass
The adjustable uncured graphene composite material 8 of the thermal conductivity of chamber, the composite material 8 are completely filled with inside sealing tempered glass 7
Cavity；
The induction coil includes along conducting-heat elements long side, and two for being wound in conducting-heat elements upper and lower part respectively are parallel
Coil 6, parallel coil 6 intersect at conducting-heat elements broadside；And intersect with parallel coil 6, it is wound in the one of tempered glass side
A vertical coil 5；The both ends of each coil are respectively arranged with wire connecting power anode and cathode.
The sealing means of tempered glass 7 are using in the sealants such as glass cement, glass self-adhesive, medical glass bonding glue
It is a kind of.
The number of turns of vertical coil 5 is 5~50 circles, thermally conductive vertical with parallel coil 5 of the number of turns of each parallel coil 5
Component edge length is directly proportional, and ratio is 50~100mm/ circle.
Induction coil is fixed on 7 surface of tempered glass with sealant.
The specific operation method is as follows for the present embodiment heat-transfer device:
Conducting wire 1 connects DC power supply with conducting wire 2, keeps conducting wire 3 and conducting wire 4 and DC power supply to disconnect, parallel coil 5 generates
Perpendicular to the magnetic field of 7 long side of tempered glass and broadside composition in-plane, so that the graphene edge controlled in organic solution is vertical
It arranges in the direction of above-mentioned plane；Heat is by being transmitted in graphene face at this time, and by the convection current of organic solvent and
Heat transfer is transmitted, and thermal conductivity is larger；
Conducting wire 3 is connected DC power supply, parallel coil 6 with conducting wire 4 by the connection of break line 1 and conducting wire 2 and DC power supply
Generate be parallel to 7 long side of tempered glass and broadside composition in-plane magnetic field so that in organic solvent graphene arrangement side
To above-mentioned plane is parallel to, the graphene arragement direction in organic solvent is parallel to above-mentioned plane, and heat at this time, which only passes through, to be had
Solvent progress is thermally conductive, and graphene promotes thermally conductive event resolves, and thermal conductivity is smaller；
By conducting wire 1, conducting wire 2, conducting wire 3 and conducting wire 4 all with DC power supply disconnect, at this time in organic solvent graphene row
Column direction restores chaotic arrangement under the warm-up movement effect of organic solvent molecule, and heat at this time passes through free convection and heat
It is transmitted.
Embodiment 5
It is described further by taking uncured graphene composite material prepared by embodiment 2 as an example below.
The size of conducting-heat elements is 200mm*200mm*15mm, 5 the number of turns of vertical coil, 4 circle, each 6 the number of turns of parallel coil.
7 thickness 3mm of tempered glass.
Current strength 200A, horizontal induced magnetic field intensity 0.16T, vertical induced magnetic field intensity 0.16T.
Thermal conductivity test is carried out to above-mentioned heat-transfer device, conducting wire 1 connects DC power supply with conducting wire 2, and graphene is perpendicular to steel
When changing glass planar, thermal conductivity is 65.8W/ (mK)；The connection of break line 1 and conducting wire 2 and DC power supply, by conducting wire 3
DC power supply is connected with conducting wire 4, when graphene is parallel to tempered glass plane, thermal conductivity is 5.8W/ (mK)；By conducting wire 1,
Conducting wire 2, conducting wire 3 and conducting wire 4 all with DC power supply disconnect, graphene in organic solvent non-directional arrange when, 18.8W/
(m·K)。
Comparative example 1
When material is the not polyvinylpyrrolidone of containing graphene in heat-transfer device sealing tempered glass 7, with the material
For compare explanation.
The size of conducting-heat elements is 200mm*200mm*15mm, 4 circle of vertical coil the number of turns, each 6 circle of parallel coil the number of turns.
Tempered glass thickness 3mm.
Current strength 200A, horizontal induced magnetic field intensity 0.16T, vertical induced magnetic field intensity 0.16T.
Heating conduction test is carried out to above-mentioned heat-transfer device, thermal conductivity is 5.2W/ (mK).
Test result shows when graphene-doped into organic solvent, and the change of heating conduction whether depends on graphene
Arragement direction in organic solvent.When tempered glass of the graphene perpendicular to two sides, heating conduction is best；Work as graphene
When being parallel to the tempered glass of two sides, graphene does not almost influence the heating conduction of organic solvent；When graphene confusion is arranged
When cloth, the heating conduction of organic solvent can be improved to a certain extent.Therefore, thermal conductivity prepared by the present invention is adjustable uncured
Graphene composite material and heat-transfer device can satisfy industrial demand.
Certainly, above content is only presently preferred embodiments of the present invention, be should not be construed as limiting to implementation of the invention
Example range.The present invention is also not limited to the example above, and those skilled in the art are in essential scope of the invention
Interior made all the changes and improvements etc., should all belong in patent covering scope of the invention.
Claims (9)
1. a kind of adjustable uncured graphene composite material of thermal conductivity, which is characterized in that the composite material includes that graphene is received
The mass ratio of rice piece, dispersing agent and organic solvent, the graphene nanometer sheet and dispersing agent is 0.05~0.2:1, and graphene is received
The mass volume ratio of rice piece and organic solvent is 1~2mg/mL；
The organic solvent is N-Methyl pyrrolidone；The dispersing agent is polyvinylpyrrolidone.
2. the adjustable uncured graphene composite material of thermal conductivity according to claim 1, which is characterized in that the graphite
Alkene nanometer sheet is the stratiform accumulation body of non-oxidized graphite alkene.
3. the preparation method of the adjustable uncured graphene composite material of thermal conductivity according to claim 2, feature exist
In, comprising the following steps:
(1) it disperses highly oriented pyrolytic graphite in dispersing agent, the graphene of non-oxide reduction is prepared using high-shear emulsion machine
The mass ratio of nanometer sheet dispersion liquid, highly oriented pyrolytic graphite and dispersing agent is 1:100；
(2) graphene nanometer sheet dispersion liquid made from step (1) is mixed with organic solvent, stirring makes it be uniformly mixed into thermal conductivity
The adjustable uncured graphene composite material of rate.
4. the preparation method of the adjustable uncured graphene composite material of thermal conductivity according to claim 3, feature exist
In high-shear emulsion machine removes graphene nanometer sheet in the step (1), comprising the following steps:
It is handled graphite flakes 12 hours, 10000rpm/min by FLUKO FA25-25G high shear mixing head, wherein graphite squama
Piece and N-Methyl pyrrolidone mix；Whole system is put into mixture of ice and water to prevent from overheating during shear-mixed.
It is stood overnight after the completion of shearing, takes supernatant to be centrifuged 1 hour under 7000rpm revolving speed, supernatant is taken to obtain non-oxide reduction
Graphene nanometer sheet dispersion liquid.
5. the preparation method of the adjustable uncured graphene composite material of thermal conductivity according to claim 3, feature exist
In it is 100~200mg/mL that highly oriented pyrolytic graphite, which is scattered in the concentration in N-Methyl pyrrolidone, in the step (1).
6. a kind of adjustable uncured graphene composite material of thermal conductivity based on the preparation of any one of claim 3-5 the method
Application, which is characterized in that the composite material be used to prepare by magnetic field regulate and control heat-transfer device.
7. application according to claim 6, which is characterized in that the heat-transfer device includes conducting-heat elements and induction coil；
The conducting-heat elements are rectangular parallelepiped structure, including sealing tempered glass (7), and are sealed in the internal sky of tempered glass (7)
The adjustable uncured graphene composite material (8) of the thermal conductivity of chamber, the composite material (8) are completely filled with sealing tempered glass
(7) internal cavities；
The induction coil includes being wound in two parallel coils of conducting-heat elements upper and lower part respectively along conducting-heat elements long side
(6), parallel coil (6) intersects at conducting-heat elements broadside；And intersect with parallel coil (6), it is wound in tempered glass side
One vertical coil (5)；The both ends of each coil are respectively arranged with wire connecting power anode and cathode.
8. application according to claim 7, which is characterized in that the number of turns of the vertical coil (5) is 5~50 circles.
9. application according to claim 8, which is characterized in that the number of turns and parallel coil of each parallel coil (6)
(6) vertical conducting-heat elements edge length is directly proportional, and ratio is 50~100mm/ circle.
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| CN112608721A (en) * | 2020-12-14 | 2021-04-06 | 碳元科技股份有限公司 | 3D graphite composite heat conduction material, preparation method, composite slurry and smart phone |
| CN116023817A (en) * | 2022-12-28 | 2023-04-28 | 湖州市吴兴区核源金属新材研究院 | Method for improving heat dissipation of electrophoretic paint coating |
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Application publication date: 20190510 |