CN105236392B - Carbon nano tube/graphene laminated film and preparation method thereof - Google Patents
Carbon nano tube/graphene laminated film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of carbon nano tube/graphene laminated film and preparation method thereof.The carbon nano tube/graphene laminated film is formed by graphene sheet layer accumulation, between graphene sheet layer growth have a CNT, connect the adjacent graphene sheet layer of levels or left and right.Preparation method includes the solution A for preparing graphitiferous alkenes material；Prepare pbz polymer carbon source and the solution B of transition metal catalyst precursor body；Solution A and solution B are mixed, obtain mixed solution；Mixed solution is filtered, dries, obtains doped graphite alkenes substance film；By doped graphite alkenes substance film in reducing gas and inert gas heat temperature raising, obtain carbon nano tube/graphene laminated film.Direction and thickness direction all have high thermal conductivity in the face of the carbon nano tube/graphene laminated film of the present invention, can be applied in cooling system, solve the heat dissipation problem in high heat flux field.
Description
Technical field
The invention belongs to field of composite material preparation, and in particular to a kind of carbon nano tube/graphene laminated film and its system
Preparation Method.
Background technology
With the development of industrial technology, the field such as microelectronics, LED and high energy weapon proposes higher to the thermal conductivity of material
It is required that the mainly thermal diffusion material of demand high heat conduction.Specifically, the component on electronic circuit board is increasingly intensive so that
Electronic chip heat flow density increases, and heat is difficult to conduct rapidly, chip temperature rise, causes product failure, therefore electronics
The thermal management of product turns into the important topic of product design.In addition, emerging LED industry is also faced with chip cooling problem,
The rising of its chip temperature will substantially reduce LED life-span, and the rising of temperature will also reduce LED luminous efficiency, therefore
LED radiating temperature control techniques are as one of LED core technology.It is same as the high energy weaponry of representative using high power laser weapon
There is also local heat flux density's height cause to radiate difficulty the problem of, and also there is an urgent need to the environment of a relative low temperature for its component
Ability reliability service, this is also that cooling system needs to solve the problems, such as.
Graphene has excellent heat conductivility, and thermal conductivity is up to 5300W/mK in its face at room temperature, is thermal conductivity highest
Material.Existing graphene film heat sink material is to be assembled into membrane structure, microcosmic knot by certain way by graphene film
Structure is tightly packed graphene sheet layer.Mainly pass through Van der Waals force phase between graphene sheet layer in existing graphene heat conduction film
Interaction, piece interlayer heat transfer efficiency is low, can not meet high heat conduction demand.Axial resistivity direction has high thermal conductivity,
The thermal conductivity of CNT at room temperature vertically can be of about 3000W/mK~3500W/mK.
The carbon nano tube/graphene composite reported at present is mainly prepared by liquid phase mechanical mixing, such as application number
For 201310693751.1 Chinese patent literature《A kind of graphene-carbon nano tube composite material film and preparation method thereof》
（The new photoelectric material Co., Ltd application of Zhangjiagang Kant）.The Chinese patent literature of Application No. 201410157857.4《It is a kind of
The preparation method of carbon nano tube/graphene composite》（Southwest Petrol University applies）Disclosed method be by CNT with
Graphene oxide simple physical mixes, then redox graphene, then become the mixing material of CNT and graphene, this
CNT is randomly dispersed within graphene sheet layer in the composite of sample, does not play connection graphene sheet layer effect, does not have
There is the high thermal conductivity for playing axial resistivity.Therefore, prepare and carbon nano-tube oriented be arranged in graphenic surface, UNICOM's graphite
The three-dimensional network composite of alkene piece turns into research emphasis.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided direction and thickness direction in a kind of face
There is carbon nano tube/graphene laminated film of high thermal conductivity and preparation method thereof, apply it in cooling system, solve
The heat dissipation problem in high heat flux field.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of carbon nano tube/graphene laminated film, the carbon nano tube/graphene laminated film is by graphene sheet layer
Accumulation forms, and being grown between the graphene sheet layer has CNT, axially connects levels for the CNT of vertical direction
Graphene sheet layer, it is axially the adjacent graphene sheet layer in the CNT connection left and right of horizontal direction.
In above-mentioned carbon nano tube/graphene laminated film, it is preferred that the CNT includes single-walled carbon nanotube
And/or multi-walled carbon nanotube.
In above-mentioned carbon nano tube/graphene laminated film, it is preferred that the carbon nano tube/graphene laminated film
Thickness is 3 μm~40 μm.
In above-mentioned carbon nano tube/graphene laminated film, it is preferred that the carbon nano tube/graphene laminated film
Direction in face（That is horizontal direction）Thermal conductivity is 500W/mK~1200W/mK, and thickness direction thermal conductivity is 0.1W/mK~20W/
mK。
The technical concept total as one, the present invention also provide a kind of above-mentioned carbon nano tube/graphene laminated film
Preparation method, comprise the following steps：
（1）Graphite alkenes material is added in polar solvent, stirs and assisting ultrasonic is disperseed, obtain solution A；
（2）Macromolecule carbon source and transition metal catalyst precursor body are dissolved in polar solvent, stir simultaneously assisting ultrasonic
It is scattered, obtain solution B；
（3）The solution A of above-mentioned gained and solution B are mixed, stirs and assisting ultrasonic is disperseed, until it is well mixed, obtain
Mixed solution；
（4）By step（3）Obtained mixed solution is filtered, and dries filter membrane after filtering, then by the filter cake on filter membrane
Take off, obtain doped graphite alkenes substance film；
（5）By step（4）Obtained doped graphite alkenes substance film is placed in stove, in reducing gas and inert gas
In, 150 DEG C~300 DEG C are first heated to, is incubated 20min~60min, then 600 DEG C~1200 DEG C are warming up to, it is incubated 30min
~120min, obtain carbon nano tube/graphene laminated film.
In above-mentioned preparation method, it is preferred that the step（2）In, the macromolecule carbon source and transition-metal catalyst
The mass values of presoma are 1~20: 1.
In above-mentioned preparation method, it is preferred that in the solution A concentration of graphite alkenes material be 0.1mg/ml~
10mg/ml, the concentration of macromolecule carbon source is 0.25mg/ml~2.5mg/ml in the solution B, and the solution A mixes with solution B
When volume ratio be 1: 1~5.
In above-mentioned preparation method, it is preferred that the step（1）In, the graphite alkenes material include graphene and/or
Modified graphene, the modified graphene include graphene oxide；The polar solvent includes water, ethanol, acetone, N, N- diformazans
One or more in base formamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO).
In above-mentioned preparation method, it is preferred that the step（2）In, the macromolecule carbon source includes polymethylacrylic acid
One or more in methyl esters, polyethylene, polyvinyl alcohol, sucrose, urea；The transition metal catalyst precursor body has for iron
Machine compound, the organic compound of cobalt, nickel organic compound in one or more, the organic compound of the iron includes two
One or more in luxuriant iron, ferric acetate, ferric nitrate, iron chloride, iron pentacarbonyl, the organic compound of the cobalt include acetic acid
One or more in cobalt, cobalt nitrate, cobalt oxalate, cobalt chloride, the organic compound of the nickel include nickel acetate, nickel nitrate, chlorine
Change the one or more in nickel, nickel oxalate；The polar solvent includes water, ethanol, acetone, N,N-dimethylformamide, N- first
One or more in base pyrrolidones, dimethyl sulfoxide (DMSO).
In above-mentioned preparation method, it is preferred that the step（5）In, the volume flow of the reducing gas and inert gas
It is 0.1~0.8: 1 to measure ratio, and the reducing gas is hydrogen, and the inert gas is nitrogen or argon gas；The step（5）In,
The speed of the heating is 5 DEG C/min~10 DEG C/min.
Compared with prior art, the advantage of the invention is that：
1st, carbon nano tube/graphene laminated film of the invention can self-sustained, can be used alone, in the THIN COMPOSITE
It is carbon nano-tube oriented to be arranged between graphene sheet layer in film, effective UNICOM graphene sheet layer, drastically increase composite wood
The heat conductivility of material.
2nd, the present invention is prepared in the method for carbon nano tube/graphene laminated film, by high-temperature process graphite alkenes material,
Obtained graphene crystal structure is complete, and defect is few.The present invention is led in graphene film interlayer doped catalyst presoma and carbon source
Hot conditions activated catalyst is crossed, successfully the CNT in graphene Intercalation reaction, UNICOM horizontal direction and vertical side
To graphene sheet layer, effectively improve the thermal conductivity and mechanical property of graphene film all directions.
3rd, in preparation method of the invention, by 150 DEG C~300 DEG C of low temperature（It is preferred that 200 DEG C or so）Processing a period of time,
Activated catalyst, avoid carbon source from decomposing and be lost in, then high-temperature process, the now own activation of catalyst being capable of sufficiently catalytic CNT
Growth.
4th, because carbon nano tube/graphene laminated film of the present invention has above feature and advantage, it is allow to be used as two
Heat sink material is tieed up, can also be directly bonded between electronic component and fin, as thermal interfacial material, improves radiating effect
Rate.The carbon nano tube/graphene laminated film of the present invention effectively contacts as thermal diffusion material with heating element, and generate heat first device
Part surface forms hot concentrated area because running produces amount of heat, and hot concentrated area heat can be along carbon nanometer
Pipe/graphene composite film surface is quickly spread, while is quickly spread along carbon nano tube/graphene laminated film normal direction, finally
It is delivered to fin.The heat sink material of the present invention, which can be used for heating element, includes microelectronic component, integrated circuit, crystal
Pipe, chip（Such as power chip, radio frequency chip）, LED light source, processor, wiring board, radome, battery and superlaser it is military
Device device temperature higher part position or heating module etc., the equipment containing above-mentioned heating element include notebook computer, intelligent hand
Machine, computer, digital camera, projecting apparatus, TV, electronic instrument, LED light device or high power laser light weapon etc..
Brief description of the drawings
Fig. 1 is the microstructure schematic diagram of carbon nano tube/graphene laminated film prepared by the embodiment of the present invention 1.
Fig. 2 is the process principle figure that doping graphene oxide film is prepared in the embodiment of the present invention 1.
Fig. 3 is the stereoscan photograph of the carbon nano tube/graphene laminated film in the embodiment of the present invention 1.
Fig. 4 is the optical photograph of the carbon nano tube/graphene laminated film in the embodiment of the present invention 1.
Fig. 5 is the transmission electron microscope photo of the carbon nano tube/graphene laminated film in the embodiment of the present invention 1.
Marginal data：
1st, graphene sheet layer；2nd, CNT.
Embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
Limit the scope of the invention.
Material and instrument employed in following examples are commercially available.
Embodiment 1
A kind of carbon nano tube/graphene laminated film of the invention, as shown in figure 1, the carbon nano tube/graphene THIN COMPOSITE
Film is to be accumulated to form by graphene sheet layer 1, and being grown between graphene sheet layer 1 has CNT 2, is axially received for the carbon of vertical direction
Mitron 2 connects levels graphene sheet layer 1, and axially the CNT 2 for horizontal direction connects the adjacent graphene sheet layer in left and right
1。
In the present embodiment, CNT 2 is multi-walled carbon nanotube.
In the present embodiment, the thickness of carbon nano tube/graphene laminated film is 5 μm.
In the present embodiment, direction thermal conductivity is 900W/mK in the face of carbon nano tube/graphene laminated film, thickness direction
Thermal conductivity is 5.9W/mK.
A kind of preparation method of the carbon nano tube/graphene laminated film of above-mentioned the present embodiment, comprises the following steps：
（1）Prepare graphene oxide solution：Take graphene oxide 20mg to be placed in 50ml beaker, added into beaker
40ml DMF solvent, the bath of mechanical agitation assisting ultrasonic are scattered 30 minutes（Generally in 5~60 minutes scopes
It is interior）, obtain finely dispersed graphene oxide solution（Solution A）.
（2）Scattered carbon source and catalyst precursor：Take 100mg PMMA（Polymethyl methacrylate）With 100mg nickel acetates
It is added in 40ml DMF solvent, the bath of mechanical agitation assisting ultrasonic is scattered 30 minutes, is uniformly dispersed
Solution B.
（3）Prepare mixed solution：By above-mentioned steps（1）Obtained solution A is added drop-wise to step（2）In obtained solution B, side
Side stirring is added dropwise, after being added dropwise, the bath of mechanical agitation assisting ultrasonic is scattered 30 minutes（Generally in the range of 30~60 minutes）, obtain
To finely dispersed mixed solution.
（4）Adulterate the preparation of graphene oxide film（Solution filters self assembly）：Take step（3）Obtained mixed solution falls
Enter in sand core funnel, be filtered by vacuum；Selected filter membrane is Kynoar, and a diameter of 5 centimetres of filter membrane, aperture is 0.45 micron.Cross
After filter, filter membrane and filtrate are placed in baking oven and dried 10 minutes, drying temperature is 40 DEG C, then by filter cake from dried
Filter membrane on peel off, obtain adulterate graphene oxide film, process principle figure is referring to Fig. 2.
（5）Adulterate graphene oxide film heat treatment and catalytic growth CNT：By step（4）Obtained doping oxidation
Graphene film is placed in tubular quartz stove, is heated in hydrogen and argon gas, argon flow amount 500sccm, and hydrogen flowing quantity is
400sccm.230 DEG C first are heated to 5 DEG C/min programming rate, 30min is incubated, continues to add with 5 DEG C/min programming rate
Heat is incubated 120min, that is, obtains carbon nano tube/graphene laminated film, as shown in Fig. 3, Fig. 4, Fig. 5, Fig. 3 is carbon to 800 DEG C
Nanotube/graphene composite film side stereoscan photograph, it can be seen that graphene layer structure.Fig. 4 is CNT/stone
Black alkene laminated film optical photograph, film are in black, a diameter of 4cm.Fig. 5 is the transmission of carbon nano tube/graphene laminated film
Electromicroscopic photograph, it is seen that grow more wall short carbon nanometer tubes between graphene layer, CNT UNICOM adjoining graphite alkene piece.
By detection, the carbon nano tube/graphene laminated film that above-mentioned the present embodiment is prepared, direction thermal conductivity in face
For 900W/mK, thickness direction thermal conductivity is 5.9W/mK, and the thickness of laminated film is 5 μm.
Embodiment 2
The carbon nano tube/graphene laminated film of the present embodiment is substantially the same manner as Example 1, differs only in：This implementation
Direction thermal conductivity is 910W/mK in the face of the carbon nano tube/graphene laminated film of example, and thickness direction thermal conductivity is 3.8W/mK.
The thickness of the laminated film of the present embodiment is 5 μm.
The preparation method of the carbon nano tube/graphene laminated film of the present embodiment is substantially the same manner as Example 1, and difference only exists
In：Step（2）Middle PMMA and nickel acetate quality are 10mg.
Described above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example.All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications under the premise without departing from the principles of the invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of carbon nano tube/graphene laminated film, comprises the following steps：
（1）Graphite alkenes material is added in polar solvent, stirs and assisting ultrasonic is disperseed, obtain solution A；
（2）Macromolecule carbon source and transition metal catalyst precursor body are dissolved in polar solvent, stirs and assisting ultrasonic is disperseed,
Obtain solution B；The transition metal catalyst precursor body is one kind in the compound, the compound of cobalt, the compound of nickel of iron
Or it is a variety of, the compound of the iron includes the one or more in ferrocene, ferric acetate, ferric nitrate, iron chloride, iron pentacarbonyl,
The compound of the cobalt includes the one or more in cobalt acetate, cobalt nitrate, cobalt oxalate, cobalt chloride, the compound bag of the nickel
Include the one or more in nickel acetate, nickel nitrate, nickel chloride, nickel oxalate；
（3）The solution A of above-mentioned gained and solution B are mixed, stirs and assisting ultrasonic is disperseed, until it is well mixed, mixed
Solution；
（4）By step（3）Obtained mixed solution is filtered, and dries filter membrane after filtering, then the filter cake on filter membrane is taken off,
Obtain doped graphite alkenes substance film；
（5）By step（4）Obtained doped graphite alkenes substance film is placed in stove, in reducing gas and inert gas, first
150 DEG C~300 DEG C are heated to, is incubated 20min~60min, then is warming up to 600 DEG C~1200 DEG C, insulation 30min~
120min, obtain carbon nano tube/graphene laminated film；
The carbon nano tube/graphene laminated film is formed by graphene sheet layer accumulation, is grown between the graphene sheet layer
There is CNT, axially the CNT for vertical direction connects levels graphene sheet layer, is axially received for the carbon of horizontal direction
The adjacent graphene sheet layer in mitron connection left and right.
2. preparation method according to claim 1, it is characterised in that the step（2）In, the macromolecule carbon source and mistake
The mass values for crossing metal catalyst precursor are 1~20: 1.
3. preparation method according to claim 1, it is characterised in that the concentration of graphite alkenes material is in the solution A
0.1mg/ml~10mg/ml, the concentration of macromolecule carbon source is 0.25mg/ml~2.5mg/ml in the solution B, the solution A
Volume ratio when being mixed with solution B is 1: 1~5.
4. according to preparation method according to any one of claims 1 to 3, it is characterised in that the step（1）In, the stone
Black alkenes material includes graphene and/or modified graphene, and the modified graphene includes graphene oxide；The polar solvent
Including the one or more in water, ethanol, acetone, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO).
5. according to preparation method according to any one of claims 1 to 3, it is characterised in that the step（2）In, the height
Molecule carbon source includes the one or more in polymethyl methacrylate, polyethylene, polyvinyl alcohol, sucrose, urea；The polarity
Solvent includes water, ethanol, acetone, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, one kind in dimethyl sulfoxide (DMSO) or more
Kind.
6. according to preparation method according to any one of claims 1 to 3, it is characterised in that the step（5）In, it is described to go back
The volume flow ratio of raw-gas and inert gas is 0.1~0.8: 1, and the reducing gas is hydrogen, and the inert gas is
Nitrogen or argon gas；The step（5）In, the speed of the heating is 5 DEG C/min~10 DEG C/min.
7. according to preparation method according to any one of claims 1 to 3, it is characterised in that the CNT includes single wall
CNT and/or multi-walled carbon nanotube.
8. according to preparation method according to any one of claims 1 to 3, it is characterised in that the carbon nano tube/graphene is answered
The thickness for closing film is 3 μm~40 μm.
9. according to preparation method according to any one of claims 1 to 3, it is characterised in that the carbon nano tube/graphene is answered
It is 500W/mK~1200W/mK to close direction thermal conductivity in the face of film, and thickness direction thermal conductivity is 0.1W/mK~20W/mK.
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| CN113213452B (en) * | 2021-06-11 | 2023-03-21 | 天津大学 | Three-dimensional ordered macroporous carbon material composed of carbon nanotubes and preparation method thereof |
| CN114394585B (en) * | 2021-12-31 | 2023-08-04 | 深圳市深瑞墨烯科技有限公司 | Composite film, preparation method thereof and electronic equipment |
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| CN114975979B (en) * | 2022-07-06 | 2024-01-26 | 广东墨睿科技有限公司 | C/G/CNT-S negative electrode material, preparation method and application |
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