CN104211051A - Graphene composite material and preparation method thereof - Google Patents

Graphene composite material and preparation method thereof Download PDF

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Publication number
CN104211051A
CN104211051A CN201410421728.1A CN201410421728A CN104211051A CN 104211051 A CN104211051 A CN 104211051A CN 201410421728 A CN201410421728 A CN 201410421728A CN 104211051 A CN104211051 A CN 104211051A
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composite material
graphene composite
graphene
graphite
nano
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Inventor
李琦
李召平
康飞宇
杜鸿达
孙占威
蔡庆荣
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SUPERC TECHNOLOGY Ltd
Shenzhen Graduate School Tsinghua University
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SUPERC TECHNOLOGY Ltd
Shenzhen Graduate School Tsinghua University
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Priority to CN201410421728.1A priority Critical patent/CN104211051A/en
Publication of CN104211051A publication Critical patent/CN104211051A/en
Priority to PCT/CN2015/078660 priority patent/WO2016029715A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/21—After-treatment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to the technical field of materials, and in particular relates to a graphene composite material and a preparation method thereof. The graphene composite material comprises 50-100wt% of graphene and 0.001-50wt% of other nano materials, wherein the other nano materials comprise carbon nanotubes and/or nano carbon fibers. The graphene composite material provided by the invention is not only high in purity, but also excellent in thermal and electric conductivity and mechanical property, can be widely used in the fields of heat radiation, electric conduction, radiation prevention and the like in industries such as 3C, flat-panel displays, LEDs, battery modules, automobiles, medical instruments, aerospace and aviation, metallurgy and nuclear reaction.

Description

A kind of graphene composite material and preparation method thereof
Technical field
The present invention relates to material technology field, be specifically related to a kind of high-performance (high heat conduction, high conduction, high strength) graphene composite material and preparation method thereof.
Background technology
Along with the raising of operating power, equipment volume is more and more less, and it is important all the more that equipment cooling seems.The material of current heat conduction field application can be divided into the metals such as gold and silver, copper, aluminum oxide, nitride and the carbonaceous materials such as the oxide compounds such as magnesium oxide, BN.Wherein in carbonaceous material family, there is thermal conductivity up to the diamond thin of 2400W/m.K, the carbon nano fiber of vapor phase growth (VGCF:2000W/m.K), carbon nanotube (CNT:3000～6600W/m.K) and the current known Graphene up to 5300W/m.K.Carbonaceous material has proportion little (1.9～2.2g/cc), and thermal expansion is little, the advantage that thermal conductivity is high.
At present, utilize carbonaceous material thermal paper to mainly contain two kinds of technology: a kind of is that expanded graphite is pressed into the paper that thickness does not wait from 50 microns to 0.3 millimeter, and thermal conductivity is at 300～500W/m.K, and resistivity is only 10 -4Ω cm left and right; Another kind is rostone ink sheet (pyrolytic graphite sheet, PGS), conventionally with PI (polyimide) film, after 1000～1400 ℃ of cracking, become carbon film, 2700～3000 ℃ of greyings make, thermal conductivity reaches 700～1950W/m.K, and specific conductivity is at 10000～20000S/cm.The latter is higher compared with the former snappiness.
The graphite paper that the expanded graphite of take is prepared as raw material, thermal conductivity is not high, poor mechanical property; Although and with PGS relative expansion graphite paper thermal conductivity and the mechanics that the carbide greying of PI and other materials obtains, all improve a lot, its raw-material productive rate only has 30wt%, therefore with high costs.
Summary of the invention
In order to address the above problem, the object of the invention is to, a kind of graphene composite material is provided, this matrix material not only has the mechanical properties such as high heat conduction, the high electro-chemical properties conducting electricity and high strength, and productive rate is high, with low cost.
Two of object of the present invention is to provide the preparation method of described graphene composite material.
The present invention is achieved through the following technical solutions:
A graphene composite material, comprises Graphene 50～100wt% and other nano materials 0.001～50wt%, and described nano material is carbon nanotube (CNT) and/or carbon nano fiber (VGCF).
Preferably, the surface of described graphene composite material has stacked and/or THE FOLD FEATURES.
Preferably, the grain-size of described graphene composite material is 10 μ m～500 μ m; At least >=10 μ m, preferably >=50 μ m, more preferably >=100 μ m, most preferably >=500 μ m.
Preferably, the density of described graphene composite material is 1.60g/cc～2.20g/cc.At least >=1.60g/cc, preferably >=1.80g/cc, more preferably >=2.00g/cc, most preferably >=2.20g/cc.
Preferably, described graphene composite material tensile strength is 20MPa～100MPa; At least >=20MPa, preferably >=30MPa, more preferably >=50MPa, most preferably >=100MPa.
Preferably, described graphene composite material thermal conductivity is 1000W/m.K～3000W/m.K.At least >=1000W/m.K, preferably >=1500W/m.K, more preferably >=2000W/m.K, most preferably >=3000W/m.K.
Preferably, described graphene composite material specific conductivity is 10000S/cm～1000000S/cm; Specific conductivity at least >=10,000S/cm, preferably >=50,000S/cm, more preferably >=100,000S/cm, most preferably >=1000000S/cm.
Preferably, described graphene composite material purity (graphitized carbon content) >=99.90wt%.
Preferably, described Graphene is the multi-layer graphene of the number of plies number of plies≤100 layer (≤34nm), preferably≤few layer graphene of 10 layers (≤3.4nm), few layer graphene of more preferably≤5 layers (≤1.7nm), most preferably individual layer, the double-layer graphite alkene of 1～2 layer (≤0.68nm);
Preferably, one or more mixtures in few wall pipe of the multi-walled pipes that described carbon nanotube is 10～100nm, 3～10nm, 3～5nm twin wall emitter lateral, 0.3～3nm single-walled pipe.
Preferably, described carbon nano fiber refers to the carbon fiber of the vapor phase growth of 100～150nm.
The method of preparing described graphene composite material, comprises and is prepared as follows step:
A. prepare the few layer of high density graphite slurry, concrete preparation referenced patent number is 201210546111.3 document;
B. get above-mentioned slurry and join general paper machine, in described ratio, add nano material, dilution suction filtration obtains the certain wet Graphene Composite Paper of thickness; But be not limited to the technology such as traditional copy paper, coating, printing, die casting.
C. get after above-mentioned wet Graphene Composite Paper oven dry, compacting under 25～35MPa pressure, obtains graphite composite film;
D. above-mentioned graphite composite film is placed in to High Temperature Furnaces Heating Apparatus and carries out recrystallize processing, finally obtain described graphene composite material.
Wherein, the temperature in described High Temperature Furnaces Heating Apparatus is 1000 ℃～5000 ℃, and pressure is 0.001～10MPa; Recrystallize is to carry out under the atmosphere of vacuum, rare gas element or oxygen absorbent protection.Temperature of reaction is at least selected 1500 ℃, preferred >=2000 ℃, more preferably >=2500 ℃, most preferably >=3000 ℃; Reaction pressure is 0.001MPa, preferably >=0.1MPa, more preferably >=1MPa, most preferably >=10MPa at least.Under the optional vacuum of reaction atmosphere, any rare gas element (nitrogen, argon gas etc.) or any oxygen absorbent protection of the environment.
This preparation method includes but not limited to occur under given conditions the nanometer recrystallize of Graphene and crystal is grown up or local graphiteization reaction.。
Any shapes such as high-performance graphene composite material can film, paper, rod, piece, pipe and any size exist.
The present invention includes Graphene 50～100wt%, carbon nanotube 0.001～50wt% or carbon nano fiber 0.001～50wt%; The present invention is from the graphene composite material that the Graphene of volume production prepares, thermal conductivity, and thermal diffusivity, specific conductivity and toughness, have very large lifting (its specific conductivity at least >=10,000S/cm; Thermal conductivity >=1,000W/m.K; Tensile strength at least; Density at least >=1.60g/cc; Grain-size at least >=10 μ m; ), and be easy to processing.
Graphene is two-dimensional sheet carbon nanomaterial, is the basic comprising unit of graphite and carbon nanotube, and the physicals that it is excellent, has allowed Graphene become the active material in this century.Single-layer graphene resistivity is up to 10 -6Ω cm (similar with Single Walled Carbon Nanotube and silver); Thermal conductivity reaches 5300W/mK (similar with Single Walled Carbon Nanotube, higher than diamond); Intensity can reach 1000GPa (similar with multiple-wall carbon nanotube, be 200 times of steel); Electronic mobility is up to 200000cm 2/ V.s (similar with Single Walled Carbon Nanotube, than fast 100 times of silicon); Have 97.7% transparency (being better than CNT (carbon nano-tube) and ITO) and up to 2630m simultaneously 2/ g specific surface area (being the twice of Single Walled Carbon Nanotube).
Utilize the feature of high heat conductance, high conductivity and the good mechanical property of Graphene, carbon nanotube or carbon nano fiber, Graphene, carbon nanotube or carbon nano fiber self-assembly can be reset to heat radiation and the conducting element that obtains various practicalities.
Compared with prior art, the present invention is based on the graphene composite material that the high-performance of Graphene makes and there is following advantages:
1), property indices is all higher than PGS technology;
2), can, under thick film (>100 μ m), obtain high thermal conductivity;
3), high-level efficiency and high yield;
4), recrystallization temperature (or greying) is low, and the time is short.
There is heat radiation, conduction, the radioprotective field of industry such as can being widely used in 3C, flat-panel monitor, LED, battery modules, automobile, medicine equipment, space flight and aviation, metallurgy, nuclear reaction in any shapes such as high-performance graphene composite material of the present invention can film, paper, rod, piece, pipe.
Accompanying drawing explanation
Fig. 1 is the cross section scanning electron microscope image of graphene composite material of the present invention,
Fig. 2 is the surface scan sem image of graphene composite material of the present invention.
concrete embodiment
Below in conjunction with embodiment, the present invention is described in further detail, to help those skilled in the art, understands the present invention.
Embodiment 1
A graphene composite material, comprises few layer of graphite 90wt% and carbon nanotube (CNT) 10wt%.Preparation method:
A. prepare the few layer of high density graphite slurry, concrete preparation referenced patent number is 201210546111.3 document;
B. get above-mentioned slurry and join general paper machine, in the ratio of Graphene/CNT=90/10, add CNT, suitably dilution and suction filtration obtain the certain wet Graphene Composite Paper of thickness;
C. get after above-mentioned l Water Paper oven dry compacting under 25MPa pressure;
D. above-mentioned graphite composite film is placed in respectively to 1500 ℃ of High Temperature Furnaces Heating Apparatuss, 2200 ℃, 3000 ℃, carries out recrystallize processing; Obtain described graphene composite material.
Detect: with four-point method measuring diaphragm resistivity and laser method, measure thermal conductivity.Obtaining lowest resistivity is 0.8 * 10 -5ohm.cm, thermal conductivity are that 2100W/m.K, intensity are 50MPa.
Embodiment 2
A graphene composite material, comprises few layer of graphite 90wt% and VGCF 10wt%.
Preparation method:
A. the few layer of high density graphite slurry, prepares referenced patent 201210546111.3;
B. get above-mentioned slurry and join general paper machine, in the ratio of Graphene/VGCF=90/10, add VGCF, suitably dilution and suction filtration obtain the certain wet Graphene Composite Paper of thickness;
C. get after above-mentioned l Water Paper oven dry compacting under 35MPa pressure;
D. above-mentioned graphite composite film is placed in respectively to 1500 ℃ of High Temperature Furnaces Heating Apparatuss, 2200 ℃, 3000 ℃, carries out recrystallize processing; Obtain described graphene composite material.
Detect: with four-point method measuring diaphragm resistivity and laser method, measure thermal conductivity.Obtaining lowest resistivity is 2 * 10 -5ohm.cm, thermal conductivity are that 1900W/m.K, intensity are 45MPa.
Embodiment 3
A graphene composite material, comprises few layer of graphite 99wt% and CNT 1wt%.
Preparation method:
A. high density is lacked the preparation referenced patent 201210546111.3 of layer graphite slurry;
B. get above-mentioned slurry and join general paper machine, in the ratio of Graphene/CNT=99/1, add CNT, suitably dilution and suction filtration obtain the certain wet Graphene Composite Paper of thickness;
C. get after above-mentioned l Water Paper oven dry compacting under 25MPa pressure;
E. above-mentioned graphite composite film is placed in respectively to 1500 ℃ of High Temperature Furnaces Heating Apparatuss, 2200 ℃, 3000 ℃, carries out recrystallize processing; Obtain described graphene composite material.
Detect: with four-point method measuring diaphragm resistivity and laser method, measure thermal conductivity.Obtaining lowest resistivity is 0.5 * 10 -5ohm.cm, thermal conductivity are that 2300W/m.K, intensity are 25MPa.
Embodiment 4
A graphene composite material, comprises few layer of graphite 99wt% and VGCF 1wt%.
Preparation method:
A. high density is lacked the preparation referenced patent 201210546111.3 of layer graphite slurry;
B. get above-mentioned slurry and join general paper machine, in the ratio of Graphene/VGCF=99/1, add VGCF, suitably dilution and suction filtration obtain the certain wet Graphene Composite Paper of thickness;
C. get after above-mentioned l Water Paper oven dry compacting under 35MPa pressure;
D. above-mentioned graphite composite film is placed in respectively to 1500 ℃ of High Temperature Furnaces Heating Apparatuss, 2200 ℃, 3000 ℃, carries out recrystallize processing;
Detect: with four-point method measuring diaphragm resistivity and laser method, measure thermal conductivity.Obtaining lowest resistivity is 2
* 10 -5ohm.cm, thermal conductivity are that 2200W/m.K, intensity are 25MPa.
Above-described embodiment, is preferred embodiment of the present invention, is not used for limiting the scope of the present invention, and the equivalence of being done with the feature described in the claims in the present invention and principle therefore all changes or modifies, within all should being included in the claims in the present invention scope.
As can be seen from Figure 1 the large single crystal body that, in graphene composite material of the present invention, nano-graphene forms through recrystallize.
As can be seen from Figure 2, the surface of graphene composite material of the present invention has the characteristic features of gauffer, grain boundary.

Claims (10)

1. a graphene composite material, is characterized in that, comprises Graphene 50～100wt% and other nano materials 0.001～50wt%, and described other materials nano material is carbon nanotube and/or carbon nano fiber.
2. graphene composite material as claimed in claim 1, is characterized in that, the surface of described graphene composite material has stacked and/or THE FOLD FEATURES.
3. graphene composite material as claimed in claim 2, is characterized in that, the grain-size of described graphene composite material is 10 μ m～500 μ m, and density is 1.60g/cc～2.20g/cc.
4. graphene composite material as claimed in claim 3, is characterized in that, described graphene composite material tensile strength is 20MPa～100MPa, and thermal conductivity is 1000W/m.K～3000W/m.K.
5. graphene composite material as claimed in claim 4, is characterized in that, described graphene composite material specific conductivity is 10000S/cm～1000000S/cm, purity >=99.90wt%.
6. graphene composite material as claimed in claim 1, is characterized in that, described Graphene is the number of plies≤100, thickness≤34nm.
7. graphene composite material as claimed in claim 1, is characterized in that, one or more mixtures in few wall pipe of the multi-walled pipes that described carbon nanotube is 10～100nm, 3～10nm, 3～5nm twin wall emitter lateral, 0.3～3nm single-walled pipe.
8. graphene composite material as claimed in claim 1, is characterized in that, described carbon nano fiber refers to the carbon fiber of the vapor phase growth of 100～150nm.
9. the method for preparation graphene composite material as described in any one in claim 1-8, is characterized in that, comprises and is prepared as follows step:
A. prepare high density thin layer graphite slurry;
B. get above-mentioned slurry and join general paper machine, in described ratio, add nano material, dilution suction filtration obtains the certain wet Graphene Composite Paper of thickness;
C. get after above-mentioned wet Graphene Composite Paper oven dry, compacting under 25～35MPa pressure, obtains graphite composite film;
D. above-mentioned graphite composite film is placed in to High Temperature Furnaces Heating Apparatus and carries out recrystallize processing, finally obtain described graphene composite material.
10. described in claim 9, prepare the method for graphene composite material, it is characterized in that, the temperature in described High Temperature Furnaces Heating Apparatus is 1000 ℃～5000 ℃, and pressure is 0.001～10MPa; Recrystallize is to carry out under the atmosphere of vacuum, rare gas element or oxygen absorbent protection.
CN201410421728.1A 2014-08-25 2014-08-25 Graphene composite material and preparation method thereof Pending CN104211051A (en)

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CN104743550A (en) * 2015-03-24 2015-07-01 中国科学院宁波材料技术与工程研究所 Three-dimensional macroscale graphene and preparation method thereof
WO2016029715A1 (en) * 2014-08-25 2016-03-03 鸿纳（东莞）新材料科技有限公司 Graphene composite material and preparation method therefor
CN106348282A (en) * 2016-08-23 2017-01-25 华侨大学 Double helix carbon fiber graphene composite material and preparation method thereof
CN108407425A (en) * 2018-02-11 2018-08-17 东莞市明骏智能科技有限公司 A kind of graphene-carbon nano tube fiber base heat-conducting pad and preparation method thereof
CN108602046A (en) * 2015-12-28 2018-09-28 纳米技术仪器公司 Graphene-Carbon Hybrid Foam
CN109037503A (en) * 2018-10-31 2018-12-18 福建巨电新能源股份有限公司 A kind of polymer Li-ion battery carbon composite membrane
CN109314225A (en) * 2016-06-07 2019-02-05 纳米技术仪器公司 With the alkali metal battery based on integral type 3D graphene-carbon-metal hybrid foam electrode
CN109776103A (en) * 2019-01-17 2019-05-21 郑州中科新兴产业技术研究院 A kind of preparation method of three-dimensional grapheme/carbon nanotube composite heat dissipation material
CN110872193A (en) * 2018-09-04 2020-03-10 天津大学 Preparation method of high-thermal-conductivity graphene/chopped carbon fiber composite material
CN111172804A (en) * 2020-03-03 2020-05-19 福建滤冠新型材料科技有限公司 Graphene carbon nanofiber paper and preparation method thereof

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WO2016029715A1 (en) * 2014-08-25 2016-03-03 鸿纳（东莞）新材料科技有限公司 Graphene composite material and preparation method therefor
CN104743550A (en) * 2015-03-24 2015-07-01 中国科学院宁波材料技术与工程研究所 Three-dimensional macroscale graphene and preparation method thereof
CN108602046A (en) * 2015-12-28 2018-09-28 纳米技术仪器公司 Graphene-Carbon Hybrid Foam
CN108602046B (en) * 2015-12-28 2023-02-17 纳米技术仪器公司 Graphene-carbon hybrid foam
CN109314225B (en) * 2016-06-07 2022-08-12 纳米技术仪器公司 Alkali metal battery with electrodes based on monolithic 3D graphene-carbon-metal hybrid foam
CN109314225A (en) * 2016-06-07 2019-02-05 纳米技术仪器公司 With the alkali metal battery based on integral type 3D graphene-carbon-metal hybrid foam electrode
CN106348282A (en) * 2016-08-23 2017-01-25 华侨大学 Double helix carbon fiber graphene composite material and preparation method thereof
CN108407425A (en) * 2018-02-11 2018-08-17 东莞市明骏智能科技有限公司 A kind of graphene-carbon nano tube fiber base heat-conducting pad and preparation method thereof
CN110872193A (en) * 2018-09-04 2020-03-10 天津大学 Preparation method of high-thermal-conductivity graphene/chopped carbon fiber composite material
CN109037503A (en) * 2018-10-31 2018-12-18 福建巨电新能源股份有限公司 A kind of polymer Li-ion battery carbon composite membrane
CN109776103B (en) * 2019-01-17 2021-07-09 郑州中科新兴产业技术研究院 Preparation method of three-dimensional graphene/carbon nanotube composite heat dissipation material
CN109776103A (en) * 2019-01-17 2019-05-21 郑州中科新兴产业技术研究院 A kind of preparation method of three-dimensional grapheme/carbon nanotube composite heat dissipation material
CN111172804A (en) * 2020-03-03 2020-05-19 福建滤冠新型材料科技有限公司 Graphene carbon nanofiber paper and preparation method thereof

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