CN108752713A - One kind aligning graphene superelevation thermal conductivity composite material and preparation method - Google Patents
One kind aligning graphene superelevation thermal conductivity composite material and preparation method Download PDFInfo
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- CN108752713A CN108752713A CN201810662719.XA CN201810662719A CN108752713A CN 108752713 A CN108752713 A CN 108752713A CN 201810662719 A CN201810662719 A CN 201810662719A CN 108752713 A CN108752713 A CN 108752713A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
Abstract
The invention discloses one kind aligning graphene superelevation thermal conductivity composite material and preparation method, the composite material is combined by the graphene nanometer sheet of non-oxide reduction, macromolecule matrix, dispersant and couplant, and so that graphene nanometer sheet is arranged in macromolecule matrix inner orientation by applying gradient magnetic.The present invention makes full use of high thermal conductivity characteristic in graphene face, is aligned by the effect realization of graphene landau diamagnetism, and under the premise of same additive amount, the composite material heat conductivility of gained is far above other doping and other common graphite alkene mixing materials.
Description
Technical field
The present invention relates to the technical fields of Heat Conduction Material, are related specifically to one kind and aligning graphene superelevation thermal conductivity
Composite material and preparation method.
Background technology
Heat conduction problem is always electronics industry and the topic that Material Field is urgently paid close attention to, currently used heat conduction material
Material is mostly the metal materials such as copper, aluminium, some composite heat conducting materials such as heat-conducting plastic etc. is due to its easy plasticity, weight in recent years
Gently, the advantages that at low cost and high-insulativity, is attempted applied in the Related product of the fields such as LED and heat dissipation of lithium battery.At present
With disclosed heat-conducting plastic related patents mostly using metal oxide ceramic body, carbon fiber and graphite as dopant, by
Small (bulk thermal conductivities such as oxide ceramic are less than 100W/ (mK)) in its thermal conductivity, doping is limited, and (carbon fiber and graphite are mixed
Miscellaneous amount is excessively high to be caused to improve its electric conductivity) etc. factors cause the heat-conducting plastic thermal conductivity being finally combined less than 10W/
(m·K)。
Graphene is as a kind of two dimensional crystal being made of hexagonal cell shape lattice structure with sp2 hybridized orbits carbon atom
Film, only there are one carbon atom thickness, because it is domestic and international with excellent physics and chemical property and potential have also been applied
The hot spot of research.Wherein thermal conductivity theoretical prediction reaches 6000W/ (mK) in the face of graphene, is the 10- of common Heat Conduction Material
20 times of (room temperature thermal conductivities:Copper 393.6W/ (mK);Aluminium 238.6W/ (mK)).Therefore graphene composite high-molecular Heat Conduction Material
High heat conductivility may be implemented.If patent 20141022171.9 discloses a kind of insulating and heat-conducting plastics and preparation method thereof,
It is added in plastics preparation process using by modified graphene, the graphene composite plastic of the gained made has good thermal conductivity
Energy.But it is with a large amount of defect and incomplete since the graphene used in the above method is redox graphene powder
The functional groups such as-CO ,-OH and the-COOH of reduction, these defects and functional group can significantly influence the lattice quality of graphene, drop
Phonon transmission speed increases phon scattering probability in bottom surface, to significantly influence the thermal conductivity of graphene.Therefore, such
Thermal conductivity is less than 1000W/ (mK) in Graphene powder dignity prepared by method, is much smaller than its theoretical value.Therefore institute is compound obtains
The thermal conductivity of the plastics arrived also only has 10-20W/ (mK).
Raising prepares the thermal conductivity of graphene in order to solve the above problem, and patent 201410673428.2 discloses a kind of graphite
Compound thermal conductivity plastics of alkene and preparation method thereof, above-mentioned patent prepare high-quality measurer using single isotope 13C by nickel catalysis
Have a grapheme material of high-termal conductivity, then with macromolecule body, couplant and dispersant is compound prepares with certain thermal conductance
Graphene composite heat-conducting plastics.On the one hand using graphene prepared by chemical vapour deposition technique to have, low output is of high cost to ask
Topic, the more important problem of another aspect, for graphene as a kind of planar material, high heat conductance is only thermal conductivity in face
Rate, and minimum less than 10W/ (mK) perpendicular to graphene face direction thermal conductivity, thus the graphene nanometer sheet of random distribution by
In the minimum reason of non-basal plane orientation thermal conductivity so that overall thermal conductivity mutually can inhibit and offset, and cause prepared by this method
Graphene composite plastic can not make full use of the highly thermally conductive characteristic of graphene so that its heat conductivity is by substantially
Degree limitation.So that utilizing the preparation-obtained graphene composite heat-conducting plastics thermal conductivity of method disclosed in patent 201410673428.2
Rate is less than 20W/ (mK).
Invention content
It is an object of the invention to overcome the shortcomings of the prior art, provide that a kind of diamagnetic to align graphene compound
High thermal conductivity material, has and its excellent heat conductivility.
In order to achieve the goal above, the technical scheme is that:
One kind aligning graphene superelevation thermal conductivity composite material, which is received by the graphene of non-oxide reduction
Rice piece, macromolecule matrix, dispersant and couplant are combined;The wherein described graphene nanometer sheet is in the composite material
Mass fraction is 1~10%, and is arranged by the macromolecule matrix inner orientation that acts on of gradient magnetic.
Optionally, the number of plies of the graphene nanometer sheet is 1~10 layer, and thickness is 0.4nm~4nm.
Optionally, the macromolecule matrix is at least one of PE, PC, PP, ABS, nylon.
Optionally, the dispersant is at least one of N-Methyl pyrrolidone, DMA, in the composite material
Mass fraction is 10~20%.
Optionally, the couplant is polyvinylpyrrolidone, the mass fraction in the composite material be 0.5%~
5%.
The preparation method of above-mentioned composite material includes the following steps:
(1) highly oriented pyrolytic graphite is scattered in dispersant, non-oxide reduction is prepared using direct liquid phase stripping method
The dispersion liquid of graphene nanometer sheet;
(2) dispersion liquid of graphene nanometer sheet and macromolecule matrix and uniform coupling agent are mixed to form graphene-plastics
Mixture;
(3) it injects the mixture into mold or plasticity equipment and applies gradient magnetic so that graphene nanometer sheet orientation row
Row form after solidification and align graphene superelevation thermal conductivity composite material.
Optionally, the gradient magnetic is tapering gradient magnetic field.
Optionally, the intensity of the gradient magnetic is 0.3-3 teslas.
Beneficial effects of the present invention are:
(1) graphene nanometer sheet is placed under gradient magnetic, due to the effect of graphene landau diamagnetism, graphene nano
Sector-meeting is converted by a rotating torque, and from upper state to lower state, until graphene nanometer sheet is oriented parallel to gradient magnetic
Field gradient direction reaches minimum energy state, tends towards stability at this time, to realize aligning inside macromolecule matrix, fills
Divide using high thermal conductivity characteristic in graphene face, under the premise of same additive amount, the composite material heat conductivility of gained is far above
Other doping and other common graphite alkene mixing materials.
(2) the non-oxide reduced graphene of high quality zero defect is prepared by directly removing highly oriented pyrolytic graphite, protects
The fabulous heat conductivility of above-mentioned graphene is demonstrate,proved so that thermal conductivity is up to 4800W/ (m in graphene face prepared by the above method
K), the composite material of gained has superelevation thermal conductivity.
(3) preparation method is simple, and controllability is strong.
Description of the drawings
Fig. 1 is the process flow chart of preparation method of the present invention.
Fig. 2 is the scanning electron microscope phenogram of graphene nanometer sheet of the present invention.
Fig. 3 is the Raman characterization figure of graphene nanometer sheet of the present invention.
Fig. 4 is the principle schematic of preparation method of the present invention;
Fig. 5 is magnetic field gradient and magnetic field intensity spatial distribution map;
Fig. 6 is the pictorial diagram for the graphene-PE plastic hybrids that the embodiment of the present invention obtains.
Specific implementation mode
The present invention is further explained below in conjunction with the drawings and specific embodiments.
With reference to figure 1, the preparation method of the highly directional arrangement graphene superelevation thermal conductivity composite material of the present invention, being will be highly directional
Pyrolytic graphite is scattered in dispersant, and the graphene nanometer sheet of non-oxide reduction is prepared using direct liquid phase stripping method;By graphite
The dispersion liquid of alkene nanometer sheet is mixed to form graphene-plastic hybrid with macromolecule matrix and uniform coupling agent;Mixture is noted
Enter in mold or plasticity equipment and apply gradient magnetic so that graphene nanometer sheet aligns, and is formed and is aligned after solidification
Graphene superelevation thermal conductivity composite material.By mass percentage, its ratio be:Graphene nanometer sheet 1~10%, dispersant 10~
20%, couplant 0.5%~5%, remaining is macromolecule matrix.Optionally, the number of plies of graphene nanometer sheet is 1~10 layer, thick
Degree is 0.4nm~4nm, and Fig. 2 is the scanning electron microscope (SEM) photograph of graphene nanometer sheet obtained, and Fig. 3 is the Raman table of graphene nanometer sheet
Sign figure;Macromolecule matrix is at least one of PE, PC, PP, ABS, nylon;Dispersant is in N-Methyl pyrrolidone, DMA
It is at least one;Couplant is polyvinylpyrrolidone.
With reference to figure 4, since graphene nanometer sheet has landau diamagnetism, by diamagnetic force effect under gradient magnetic control
Turning to lower state by upper state, finally stabilization is parallel to magnetic field gradient directions, to be arranged in macromolecule matrix inner orientation.Its
Middle gradient magnetic is tapering gradient magnetic field, and intensity is 0.3-3 teslas.With reference to figure 5, for the tapering gradient of the varying strength of citing
The magnetic field intensity spatial distribution in magnetic field.
Embodiment 1
High quality highly oriented pyrolytic graphite is scattered in N-Methyl pyrrolidone, is prepared using direct liquid phase stripping method non-
Redox high-quality graphene nanometer sheet;The dispersion liquid of graphene nanometer sheet and PE and polyvinylpyrrolidone are uniformly mixed
Conjunction forms graphene-plastic hybrid;Inject the mixture into mold or plasticity equipment and apply gradient magnetic (1.5 it is special this
Draw) so that graphene nanometer sheet aligns, solidification.The mass fraction of the graphene nanometer sheet is 2.5%, N- methyl pyrroles
Pyrrolidone mass fraction is 15%, and polyvinylpyrrolidone mass fraction is 3%.
Embodiment as a comparison, composition is constant, and highly oriented pyrolytic graphite is scattered in N-Methyl pyrrolidone, using straight
Connect the graphene nanometer sheet that liquid phase stripping method prepares non-oxide reduction;By the dispersion liquid of graphene nanometer sheet and macromolecule matrix and
Polyvinylpyrrolidone is uniformly mixed to form graphene-plastic hybrid;It injects the mixture into mold or plasticity equipment, Gu
Change, obtains non-directional arrangement graphene composite material.
Embodiment 2
The mass fraction of graphene nanometer sheet is 5%, remaining is the same as embodiment 1.Same setting comparative example.
Embodiment 3
The mass fraction of graphene nanometer sheet is 7.5%, remaining is the same as embodiment 1.Same setting comparative example.
The pictorial diagram for the graphene-PE plastic hybrids that Fig. 6 obtains for Examples 1 to 3 and the comparison with no graphene, can
See that the increase with graphene content, color are gradually deepened.
By the non-directional row for aligning graphene superelevation thermal conductivity composite material and comparative example of Examples 1 to 3
Row graphene composite material carries out thermal conductivity test respectively, and test result see the table below:
It can be seen that using highly directional arrangement graphene composite material than common graphite alkene composite material with superior
Heat conductivility, and heat conductivility increases with the increase of graphene content.
One kind that above-described embodiment only is used for further illustrating the present invention aligns graphene superelevation thermal conductivity composite wood
Material and preparation method thereof, but the invention is not limited in embodiments, it is every according to the technical essence of the invention to above example
Made by any simple modification, equivalent change and modification, each fall in the protection domain of technical solution of the present invention.
Claims (8)
1. one kind aligning graphene superelevation thermal conductivity composite material, it is characterised in that:It is received by the graphene of non-oxide reduction
Rice piece, macromolecule matrix, dispersant and couplant are combined;The wherein described graphene nanometer sheet is in the composite material
Mass fraction is 1~10%, and is arranged by the macromolecule matrix inner orientation that acts on of gradient magnetic.
2. composite material according to claim 1, it is characterised in that:The number of plies of the graphene nanometer sheet is 1~10 layer,
Thickness is 0.4nm~4nm.
3. composite material according to claim 1, it is characterised in that:The macromolecule matrix is PE, PC, PP, ABS, Buddhist nun
At least one of dragon.
4. composite material according to claim 1, it is characterised in that:The dispersant is in N-Methyl pyrrolidone, DMA
At least one, mass fraction in the composite material is 10~20%.
5. composite material according to claim 1, it is characterised in that:The couplant is polyvinylpyrrolidone, in institute
It is 0.5%~5% to state the mass fraction in composite material.
6. the preparation method of any one of Claims 1 to 5 composite material, it is characterised in that include the following steps:
(1) highly oriented pyrolytic graphite is scattered in dispersant, the graphite of non-oxide reduction is prepared using direct liquid phase stripping method
The dispersion liquid of alkene nanometer sheet;
(2) dispersion liquid of graphene nanometer sheet graphene-plastics are mixed to form with macromolecule matrix and uniform coupling agent to mix
Object;
(3) it injecting the mixture into mold or plasticity equipment and applies gradient magnetic so that graphene nanometer sheet aligns, Gu
It is formed after change and aligns graphene superelevation thermal conductivity composite material.
7. preparation method according to claim 6, it is characterised in that:The gradient magnetic is tapering gradient magnetic field.
8. the preparation method described according to claim 6 or 7, it is characterised in that:The intensity of the gradient magnetic be 0.3-3 it is special this
It draws.
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CN109439988A (en) * | 2018-12-29 | 2019-03-08 | 厦门十维科技有限公司 | The preparation method for aligning graphene acieral of superelevation thermal conductivity |
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