CN106995214A - Graphene/carbon nano-tube nano laminated composite thin film and preparation method thereof - Google Patents
Graphene/carbon nano-tube nano laminated composite thin film and preparation method thereof Download PDFInfo
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- CN106995214A CN106995214A CN201710265193.7A CN201710265193A CN106995214A CN 106995214 A CN106995214 A CN 106995214A CN 201710265193 A CN201710265193 A CN 201710265193A CN 106995214 A CN106995214 A CN 106995214A
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Abstract
The invention provides a kind of graphene/carbon nano-tube nano laminated composite thin film and preparation method thereof.The graphene/carbon nano-tube nano laminated composite thin film is made up of the graphene extra-thin film formed in water surface and the CNT ultrathin membrane pulled out from carbon nano pipe array, graphene extra-thin film and CNT ultrathin membrane are alternately stacked to form nano-stack structure, and weight percentage of the graphene extra-thin film in nano laminated composite thin film is 0 100%.Graphene dispersing solution is expelled to water surface formation graphene extra-thin film, CNT ultrathin membrane is pulled out from carbon nano pipe array, the repeated multiple times transfer of graphene extra-thin film and CNT ultrathin membrane is stacked, graphene/carbon nano-tube nano laminated composite thin film is formed.The graphene/carbon nano-tube nano laminated composite thin film can be used for be electromagnetically shielded, ultracapacitor, lithium battery, solar cell, radiating, composite enhancing etc. field.
Description
Technical field
The present invention relates to nanometer material science and technical field, more particularly to graphene and carbon nano tube compound material neck
Domain.
Background technology
CNT and graphene have typical peacekeeping Two-dimensional Carbon nanostructured, and since the advent of the world is caused widely
Concern.1991, CNT was unexpected by electron microscope expert doctor Iijima of Japanese NEC Corporation's basic research laboratories
It was found that.CNT is that with special construction, (radial dimension is nanometer scale to one kind, and axial dimension is micron dimension even millimeter
Magnitude) one-dimensional tubular nanometer material, several layers to tens of layers of coaxial pipe is mainly made up of the carbon atom of hexagonal arrangement,
Fixed distance is kept between layers, and about 0.34 nanometer, diameter is generally 2-50 nanometers.CNT has in the axial direction
High strength, high conductivity, high-termal conductivity and excellent chemical property.Graphene is big by Manchester, England in 2004
Learn physicist An Deliehaimu and Constantine Nuo Woxiao loves are successfully prepared first.Graphene is that a kind of two dimension is brilliant
Body, it is the carbon simple substance neatly arranged by hexagonal lattice structure by carbon atom, and Stability Analysis of Structures has height in in-plane
Mechanical strength, high conductivity, highly thermally conductive property and excellent chemical property.
Graphene/carbon nanotube composite material causes extensive research interest, integrated graphene and CNT it is several
What advantage, produces cooperative effect, shows the mechanical strength more excellent than any one homogenous material, thermal conductivity, electric conductivity
With electrochemical energy storage performance, have good in terms of composite enhancing, radiating, electromagnetic shielding, ultracapacitor, energy-storage battery
Good application prospect.The Graphene/carbon nanotube composite material reported for work at present is broadly divided into three classes, and the first kind is with graphene
Powder or carbon nanotube powder are raw material, and the two is dispersed in certain solvent together, then by spin coating, spray, take out
The method film forming such as filter, electro-deposition, resulting Graphene/carbon nanotube composite material has the disadvantages that：1) graphene and carbon
Nanotube disperses uneven, 2) graphene and CNT random distribution, without orientation texture.Equations of The Second Kind is with graphene powder
Or carbon nanotube powder is raw material, by surface chemical modification so that opposite electric on graphene and carbon nano tube surface band
Lotus, and be dispersed in water, by the method film forming of electrostatic drive LBL self-assembly, resulting graphene/carbon nano-tube is combined
Material has the disadvantages that：The surface chemical modification heavy damage structure of graphene and CNT, reduction laminated film
Properties.3rd class method is in-situ chemical vapor deposition method, and graphene and CNT are successively grown in substrate, is formed
The patent of graphene/carbon nanotube composite film, such as Tsing-Hua University and Hongfujin Precise Industry (Shenzhen) Co., Ltd.
CN105174204A, CN103359717A, CN102796991A, CN102794945A and CN102724620A are make use of
Learn vapour deposition process and successively grow graphene and CNT in substrate, but the graphene/carbon nano-tube THIN COMPOSITE of gained
Film has the disadvantages that：1) CNT is perpendicular to membrane plane directional spreding, it is difficult to along membrane plane directional spreding, 2) technology
Complexity, cost is high, it is difficult to industrialize.
The content of the invention
It is compound it is an object of the invention to provide a kind of graphene/carbon nano-tube nano-stack for above-mentioned technical problem
Film, described graphene/carbon nano-tube nano laminated composite thin film be included in water surface formation graphene extra-thin film and from
The high-orientation carbon nanotube ultrathin membrane that carbon nano pipe array is pulled out, graphene extra-thin film is in graphene/carbon nano-tube nano-stack
Weight fraction in laminated film is graphene extra-thin film and CNT ultrathin membrane formation nanoscale lamination knot less than 100%
Structure.
Another object of the present invention is to propose a kind of side for preparing graphene/carbon nano-tube nano laminated composite thin film
Method, step includes：
1) CNT ultrathin membrane is pulled out from carbon nano pipe array, by the ultra-thin membrane stack formation carbon nanometer of y layers of CNT
Tube layer CNTy；
2) graphene dispersing solution is expelled to water surface one layer graphene ultrathin membrane of formation；
3) the y layer CNTs ultrathin membrane of step 1 is imported in water and exported so that the graphene of water surface in step 2
Ultra-thin film transfer covers carbon nano-tube film surface, repeats x times, ultra-thin to y layers of CNT to shift x layer graphenes ultrathin membrane
On film, a graphene/carbon nano-tube bilayer (G is formedx/CNTy)1；
4) in graphene/carbon nano-tube bilayer (Gx/CNTy)1Upper covering carbon nanotube layer CNTy, then shift x schungites
Alkene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (Gx/CNTy)2, the like, move in circles n times, obtain graphite
Alkene/carbon nanotube laminated composite thin film (Gx/CNTy)n。
Step 5 can also further be included) by above-mentioned graphene/carbon nano-tube nano laminated composite thin film (Gx/CNTy)n
It is heat-treated under an inert gas, obtains graphene/carbon nano-tube nano laminated composite thin film.
The concentration of graphene dispersing solution is that the solvent in 0.001-2mg/ml, dispersion liquid is organic solvent miscible with water,
Including 1-METHYLPYRROLIDONE, N, N-dimethylformamide, DMAC N,N' dimethyl acetamide, NVP, methanol, second
One or several kinds in alcohol, isopropanol, acetone, dimethyl sulfoxide (DMSO)；
The thickness of graphene extra-thin film is in 0.34 nanometer to 100 nanometer ranges；
The thickness of CNT ultrathin membrane is in 2 nanometers to 100 nanometer ranges；
Y values are more than or equal to 1, x values and are more than or equal to 1, n values more than or equal to 1.
Above-mentioned steps 5) in heat treatment temperature in room temperature to 3000 degrees Celsius.Heat treatment can further improve leading for composite membrane
Electrical and thermal conductivity, heat treatment temperature is higher, and performance can be better, and treatment temperature does not have effect when being less than room temperature, and treatment temperature is high
Technically it is difficult in 3000 degrees Celsius.So heat treatment temperature in room temperature to 3000 degrees Celsius.
Graphene/carbon nano-tube nano laminated composite thin film pliability that this method is obtained is good, mechanical strength is high, thermal conductivity
It is high, the advantages of electrical conductivity is high.The graphene/carbon nano-tube nano laminated composite thin film of the acquisition radiating, electromagnetic shielding, it is super
The fields such as capacitor, lithium battery, solar cell have extensive actual application value.
Embodiment
Clear, complete description will be carried out to the technical scheme in the embodiment of the present invention below.Obviously, described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Embodiment 1
(1) it is 3 centimetres of transparent CNT ultrathin membranes to pull out width from carbon nano pipe array, is covered cleaning
On sheet glass, sheet glass is immersed and taken out after drenching in ethanol, is dried naturally.
(2) 1mg/ml graphenes/1-METHYLPYRROLIDONE dispersion liquid is slowly expelled in the culture dish being filled with water, forms saturating
Bright graphene extra-thin film.
(3) carried out dragging for film in culture dish with the sheet glass in step 1, i.e., graphene extra-thin film is transferred to CNT
On ultrathin membrane, dry naturally, form a graphene/carbon nano-tube bilayer (G1/CNT1)1。
(4) in graphene/carbon nano-tube bilayer (G1/CNT1)1One layer of CNT ultrathin membrane of upper covering, then shifts one
Layer graphene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (G1/CNT1)2, the like, move in circles n times, obtain
Graphene/carbon nano-tube nano laminated composite thin film (G1/CNT1)n。
(5) by the graphene/carbon nano-tube nano laminated composite thin film (G of step 41/CNT1)nIn 2850 DEG C of argon gas protections
Lower heat treatment 2 hours, obtains the highly conductive graphene/carbon nano-tube nano laminated composite thin film of flexible high heat conduction.
Embodiment 2
(1) it is 5 centimetres of transparent CNT ultrathin membranes to pull out width from carbon nano pipe array, on clean sheet glass
One layer of CNT ultrathin membrane is covered, sheet glass is immersed and taken out after drenching in DMF, is dried naturally.
(2) 0.2mg/ml graphenes/alcohol dispersion liquid is slowly expelled in the culture dish being filled with water, forms transparent graphite
Alkene ultrathin membrane.
(3) carried out dragging for film in culture dish with the sheet glass in step 1, i.e., form one layer on CNT ultrathin membrane surface
Uniform graphene extra-thin film, dries naturally, then repeats to drag for film drying twice, i.e., in one layer of CNT ultrathin membrane surface heap
Folded three layer graphene ultrathin membranes, form a graphene/carbon nano-tube bilayer (G3/CNT1)1。
(4) in graphene/carbon nano-tube bilayer (G3/CNT1)1One layer of CNT ultrathin membrane of upper covering, then shifts three
Layer graphene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (G3/CNT1)2, the like, move in circles n times, obtain
Graphene/carbon nano-tube nano laminated composite thin film (G3/CNT1)n。
(5) by the graphene/carbon nano-tube nano laminated composite thin film (G of step 43/CNT1)nIn 3000 DEG C of argon gas protections
Lower heat treatment 24 hours, obtains the highly conductive graphene/carbon nano-tube nano laminated composite thin film of flexible high heat conduction.
Embodiment 3
(1) it is 7 centimetres of transparent CNT ultrathin membranes to pull out width from carbon nano pipe array, covers 3 layers of CNT
Ultrathin membrane on clean sheet glass, will sheet glass immerse drench in ethanol after take out, dry naturally.
(2) 0.5mg/ml graphenes/1-METHYLPYRROLIDONE dispersion liquid is slowly expelled in the culture dish being filled with water, formed
Transparent graphene extra-thin film.
(3) carried out dragging for film in culture dish with the sheet glass in step 1, i.e., it is uniform in one layer of carbon nano tube surface formation
Graphene film, dries naturally, forms a graphene/carbon nano-tube bilayer (G1/CNT3)1。
(4) in graphene/carbon nano-tube bilayer (G1/CNT3)13 layers of CNT ultrathin membrane of upper covering, then shift one layer
Graphene extra-thin film, forms two graphene/carbon nano-tube bilayer (G1/CNT3)2, the like, move in circles n times, obtain stone
Black alkene/carbon nanotube laminated composite thin film (G1/CNT3)n。
(5) by the graphene/carbon nano-tube nano laminated composite thin film (G of step 41/CNT3)nIn 2000 DEG C of nitrogen protections
Lower heat treatment 10 hours, obtains the highly conductive graphene/carbon nano-tube nano laminated composite thin film of flexible high heat conduction.
Embodiment 4
(1) it is 5 centimetres of transparent CNT ultrathin membranes to pull out width from carbon nano pipe array, on clean sheet glass
One layer of CNT ultrathin membrane is covered, sheet glass is immersed and taken out after drenching in DMF, is dried naturally.
(2) 0.8mg/ml graphenes/alcohol dispersion liquid is slowly expelled in the culture dish being filled with water, forms transparent graphite
Alkene ultrathin membrane.
(3) carried out dragging for film in culture dish with the sheet glass in step 1, i.e., it is uniform in one layer of carbon nano tube surface formation
Graphene film, dries naturally, then repeats to drag for film drying twice, i.e., stacks three layers of stone on one layer of CNT ultrathin membrane surface
Black alkene ultrathin membrane, forms a graphene/carbon nano-tube bilayer (G3/CNT1)1。
(4) in graphene/carbon nano-tube bilayer (G3/CNT1)1One layer of CNT ultrathin membrane of upper covering, then shifts three
Layer graphene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (G3/CNT1)2, the like, move in circles n times, obtain
Graphene/carbon nano-tube nano laminated composite thin film (G3/CNT1)n。
(5) by the graphene/carbon nano-tube nano laminated composite thin film (G of step 43/CNT1)nIn 1000 DEG C of argon gas protections
Lower heat treatment 2 hours, obtains the highly conductive graphene/carbon nano-tube nano laminated composite thin film of flexible high heat conduction.
Embodiment 5
(1) it is 5 centimetres of transparent CNT ultrathin membranes to pull out width from carbon nano pipe array, on clean sheet glass
Three layers of CNT ultrathin membrane are covered, sheet glass is immersed and taken out after drenching in DMF, is dried naturally.
(2) 0.8mg/ml graphenes/alcohol dispersion liquid is slowly expelled in the culture dish being filled with water, forms transparent graphite
Alkene ultrathin membrane.
(3) carried out dragging for film in culture dish with the sheet glass in step 1, i.e., it is uniform in one layer of carbon nano tube surface formation
Graphene film, dries naturally, then repeats to drag for film drying twice, i.e., stacks three layers of stone on one layer of CNT ultrathin membrane surface
Black alkene ultrathin membrane, forms a graphene/carbon nano-tube bilayer (G3/CNT3)1。
(4) in graphene/carbon nano-tube bilayer (G3/CNT3)1Three layers of CNT ultrathin membrane of upper covering, then shift three
Layer graphene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (G3/CNT3)2, the like, move in circles n times, obtain
The flexible highly conductive graphene/carbon nano-tube nano laminated composite thin film (G of high heat conduction3/CNT3)n。
Claims (10)
1. a kind of graphene/carbon nano-tube nano laminated composite thin film, it is characterised in that：Included in the graphene of water surface formation
Ultrathin membrane and the CNT ultrathin membrane pulled out from carbon nano pipe array, graphene extra-thin film is in graphene/carbon nano-tube nanometer
Weight fraction in laminated composite thin film is that graphene extra-thin film and CNT ultrathin membrane are alternately stacked to be formed less than 100%
Nano-stack structure.
2. graphene/carbon nano-tube nano laminated composite thin film according to claim 1, it is characterised in that graphene is ultra-thin
The thickness of film is in 0.34 nanometer to 100 nanometer ranges.
3. graphene/carbon nano-tube nano laminated composite thin film according to claim 1, it is characterised in that CNT surpasses
The thickness of film is in 2 nanometers to 100 nanometer ranges.
4. a kind of method for preparing the graphene/carbon nano-tube nano laminated composite thin film described in claim any one of 1-3, institute
The method stated comprises the following steps：
1) the CNT ultrathin membrane of orientation is pulled out from carbon nano pipe array, y layers of CNT ultrathin membrane are stacked；
2) graphene dispersing solution is expelled to water surface one layer graphene ultrathin membrane of formation；
3) the y layer CNTs ultrathin membrane of step 1 is imported in water and exported so that the graphene of water surface is ultra-thin in step 2
Film transfer covers carbon nano-tube film surface, repeats x times, to shift x layer graphenes ultrathin membrane to y layers of CNT ultrathin membrane
On, form a graphene/carbon nano-tube bilayer (Gx/CNTy)1；
4) in the graphene/carbon nano-tube bilayer (G of step 3x/CNTy)1Upper y layers of CNT ultrathin membrane of covering, then shift x
Layer graphene ultrathin membrane, forms two graphene/carbon nano-tube bilayer (Gx/CNTy)2, the like, move in circles n times, obtain
Graphene/carbon nano-tube nano laminated composite thin film (Gx/CNTy)n。
5. method according to claim 4, it is characterised in that also comprising step 5) above-mentioned graphene/carbon nano-tube is received
Rice laminated composite thin film (Gx/CNTy)nIt is heat-treated under an inert gas, obtains graphene/carbon nano-tube nano-stack THIN COMPOSITE
Film.
6. method according to claim 4, it is characterised in that the concentration of described graphene dispersing solution is 0.001-2mg/
Solvent in ml, dispersion liquid is organic solvent miscible with water, including 1-METHYLPYRROLIDONE, DMF, N, N-
It is a kind of or several in dimethyl acetamide, NVP, methanol, ethanol, isopropanol, acetone, dimethyl sulfoxide (DMSO)
Kind；Described graphene extra-thin film is formed in water surface, and its thickness is in 0.34-100 nanometer thickness；Described CNT ultrathin membrane
Pulled out from carbon nano pipe array, its thickness is at 2-100 nanometers.
7. method according to claim 4, it is characterised in that y values are more than or equal to 1, x values and are more than or equal to 1, n values
More than or equal to 1.
8. method according to claim 5, it is characterised in that heat treatment temperature is in room temperature to 3000 degrees Celsius.
9. method according to claim 4, it is characterised in that the graphene/carbon nano-tube nano laminated composite thin film
With graphene extra-thin film and CNT ultrathin membrane alternating stacked configuration.
10. the use of graphene/carbon nano-tube nano laminated composite thin film prepared by the method described in claim any one of 4-9
On the way, for radiating, being electromagnetically shielded, ultracapacitor, lithium battery or area of solar cell.
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| CN107732116A (en) * | 2017-11-20 | 2018-02-23 | 南通百正电子新材料股份有限公司 | A kind of nickelous selenide film of graphene carbon nanotube two for lithium battery and preparation method thereof |
| CN110257022A (en) * | 2019-07-18 | 2019-09-20 | 深圳前海量子翼纳米碳科技有限公司 | A kind of electromagnetic shielding thermal conductive silicon rubber mat of insulation and preparation method thereof |
| CN110483005A (en) * | 2019-09-18 | 2019-11-22 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Graphene-carbon nano tube Film laminated film and the preparation method and application thereof |
| CN110602934A (en) * | 2019-08-13 | 2019-12-20 | 深圳烯湾科技有限公司 | Electromagnetic shielding heat dissipation film and preparation method and application thereof |
| CN111470490A (en) * | 2020-04-15 | 2020-07-31 | 南京大学 | Oriented carbon nanotube/graphene composite heat-conducting film, preparation method thereof and semiconductor device |
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| CN111470490A (en) * | 2020-04-15 | 2020-07-31 | 南京大学 | Oriented carbon nanotube/graphene composite heat-conducting film, preparation method thereof and semiconductor device |
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Application publication date: 20170801 |
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| RJ01 | Rejection of invention patent application after publication |