CN106219519A - A kind of preparation method of high-graphitized CNT ultra-thin heat-conductivity conducting thin film - Google Patents
A kind of preparation method of high-graphitized CNT ultra-thin heat-conductivity conducting thin film Download PDFInfo
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- CN106219519A CN106219519A CN201610817816.2A CN201610817816A CN106219519A CN 106219519 A CN106219519 A CN 106219519A CN 201610817816 A CN201610817816 A CN 201610817816A CN 106219519 A CN106219519 A CN 106219519A
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
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Abstract
A kind of preparation method of high-graphitized CNT ultra-thin heat-conductivity conducting thin film, including: first prepare carbon nanotube suspension, in substrate, then form carbon nano-tube film, and peel off from substrate；Carbon nano-tube film is modified process, graphitization processing again, finally with roller machine, carbon nano-tube film is rolled.Carbon nano-tube film prepared by the present invention through carbonization, graphitization processing, and after twin rollers rolls, heat conduction, electric conductivity are greatly improved, its mechanical strength and pliability be improved significantly, in lithium ion battery, alternative aluminium foil Copper Foil is as collector, it is also possible to separately as negative material.
Description
Technical field
The invention belongs to technical field of nano material.
Background technology
CNT has significant application value in nanotechnology, heat-conductivity conducting and the field such as material science and technology.Its
Excellent conductivity, conduction of heat and mechanical performance, be widely used space in many fields.Carbon nano-tube film is to be received by carbon
The one that mitron is made is to environment non-hazardous, nontoxic basic material.Due to carbon nano-tube film has flexibility can
The feature of bending, at transparent conductive film, the parts of the high cost modern electronic product such as flexible display, touch screen have extensively
Application.Carbon nano-tube film also has that density is low, light weight, electrical and thermal conductivity are good simultaneously, it is possible to as lithium battery collector,
Electrode overall weight can be reduced, promote the energy density of battery.
At present prepare the method for carbon nano-tube film by carbon nanotube dust the most single, typically use at CNT
Dispersion liquid adds binding agent, is processed by ultrasonic, stirring or high pressure homogenize and make carbon nanotube suspension, then pass through sucking filtration
Or mode molding in substrate of uniformly coating, make carbon nano-tube film finally by separation.This preparation method has bright
Aobvious shortcoming: add a large amount of binding agent and cause film conductivity undesirable, if using carbonization treatment binding agent carbonization to be carried after film forming
Its electric conductivity high, carbon nano-tube film then can lose original mechanical strength so that the use of carbon nano-tube film is restricted,
Using effect is the most undesirable.
The CNT that this experiment uses is one-dimensional linear type nano-carbon material, and its draw ratio and specific surface area are relatively big, with
Shi Buyi stacking is adsorbed, is mutually intertwined, and this makes the dispersion of CNT relatively easily, the system of carbon nano tube dispersion liquid
For being also more prone to.
CNT is as a kind of nano material, for meeting its application on a macroscopic scale, prepares one and has
There is while satisfactory electrical conductivity the carbon nano-tube film of certain mechanical strength, scientific experiment, commercial Application are all had very
Big value.
Summary of the invention
The purpose of the present invention is to propose to the preparation method of a kind of high-graphitized CNT ultra-thin heat-conductivity conducting thin film,
By rolling under the high-temperature heat treatment of carbon nano-tube film and pressure, overcome that carbon nano-tube film relative intensity is relatively low to be unfavorable for
The shortcoming of production operation, is greatly improved the heat conduction of carbon nano-tube film, conduction and mechanical strength, improves making of carbon nano-tube film
Use performance.
The present invention is achieved by the following technical solutions.
The preparation method of a kind of high-graphitized CNT of the present invention ultra-thin heat-conductivity conducting thin film, including such as
Lower step.
(1) preparation of carbon nanotube suspension, by CNT, dispersant, binding agent and N-Methyl pyrrolidone (NMP)
Solution is raw material, through ultrasonic, high speed shear or ball milling, prepares carbon nanotube suspension, and CNT, dispersant and NMP press
The mass ratio of 4-12:1-2:80-99 is configured to dispersion liquid, then is joined by the mass ratio of 90-100:1-5 by dispersion liquid and binding agent
System forms.
(2) carbon nanotube suspension prepared being coated uniformly in substrate, 65 DEG C are dried.Substrate is formed carbon receive
Mitron thin film.
(3) carbon nano-tube film that will be formed in step (2), peels off from substrate.
(4) modification of carbon nano-tube film: the carbon nano-tube film after peeling off in step (3) is placed in vacuum carburization
In stove, it is warming up to 600 DEG C with 10-15 DEG C/min, is incubated 20-120min, then is warming up to 800 DEG C-1400 DEG C with 2-5 DEG C/min,
Temperature retention time is 1-10h, is cooled to room temperature and takes out after terminating.
(5) carbon nano-tube film after carbonization treatment in step (4) is placed in graphitizing furnace, with 5-20 DEG C/min's again
Programming rate is warming up to 2300 DEG C-3000 DEG C, keeps non-oxide noble gas with argon, nitrogen etc. during graphitization processing
Protection, is incubated 2-36h, cools to room temperature with the furnace and takes out.
(6) being rolled by twin rollers by the carbon nano-tube film after graphitization processing in step (5), twin rollers adjusts thickness
For 10-30 μm, density of film is 0.1 ~ 0.6g/cm3, thickness is 10-50 μm.
Substrate described in step of the present invention (2) is flexible plastic film, Copper Foil or aluminium foil.
The carbon nano-tube film of the present invention is obviously improved than front electric conductivity, and thin film makes its intensity, pliability through rolling
It is remarkably reinforced.
Accompanying drawing explanation
Fig. 1 is the photo before carbon nano-tube film of the present invention peels off matrix.
Fig. 2 is the photo after carbon nano-tube film of the present invention peels off matrix.
Detailed description of the invention
The present invention is described further by following example.
CNT used by the embodiment of the present invention is Chinese patent ZL201210067937.1, ZL201210304345.7
Prepared.
Embodiment 1.
(1) prepared by carbon nanotube suspension.By the CNT of graphitization processing, SDBS dispersant, NMP with 5:1:84
Mass ratio weigh and be placed in beaker, seal with sealed membrane, more ultrasonic 1h, then change closing container high speed shear 1h, make composition
Dissipate liquid.Dispersion liquid and PVDF binding agent are prepared with the mass ratio of 95:1.1, shear 2h in closing container high speed, prepare carbon and receive
Mitron suspension.
(2) carbon nanotube suspension being coated uniformly on flexible plastic film, 65 DEG C are dried.
(3) gently carbon nano-tube film is separated with flexible plastic film with tweezers.
(4) carbon nano-tube film is placed in the carbide furnace being filled with argon shield, is warming up to 600 DEG C with 10/min, insulation
60min, then it is warming up to 1200 DEG C with 3 DEG C/min, it is incubated 5h, is cooled to room temperature after terminating and takes out.
(5) carbon nano-tube film after carbonization treatment is placed in graphitizing furnace, is passed through argon as protective gas, with 15
DEG C/programming rate of min is warming up to 2800 DEG C, temperature retention time is 12h, and after graphitization terminates, cooling is taken out.
(6) being processed by twin rollers rolling by the carbon nano-tube film after graphitization processing, density is about 0.215g/cm3
Thickness is 25 μm.
Embodiment 2.
(1) prepared by carbon nanotube suspension.By the CNT of graphitization processing, SDS dispersant, NMP with 6:1.1:
The mass ratio of 90 weighs and is placed in beaker, seals with sealed membrane, more ultrasonic 1h, then changes closing container high speed shear 1h, is fabricated to
Dispersion liquid.Dispersion liquid and SBR binding agent are prepared with the mass ratio of 90:1, in closing ball milling 4h in container, prepare CNT
Suspension.
(2) carbon nanotube suspension being coated uniformly on Copper Foil, 65 DEG C are dried.
(3) gently carbon nano-tube film is separated with Copper Foil with tweezers.
(4) carbon nano-tube film is placed in the carbide furnace being filled with argon shield, is warming up to 600 DEG C with 12/min, insulation
50min, then it is warming up to 1400 DEG C with 4 DEG C/min, it is incubated 6h, is cooled to room temperature after terminating and takes out.
(5) carbon nano-tube film after carbonization treatment is placed in graphitizing furnace, is passed through argon as protective gas, with 10
DEG C/programming rate of min is warming up to 2700 DEG C, temperature retention time is 18h, and after graphitization terminates, cooling is taken out.
(6) being processed by twin rollers rolling by the carbon nano-tube film after graphitization processing, thickness is 20 μm, and density is about
0.325g/cm3。
Claims (2)
1. a preparation method for high-graphitized CNT ultra-thin heat-conductivity conducting thin film, is characterized in that including walking as follows
Rapid:
(1) be raw material by CNT, dispersant, binding agent and N-Methyl pyrrolidone solution, through ultrasonic, high speed shear or
Ball milling, prepares carbon nanotube suspension, and CNT, dispersant and NMP press the mass ratio preparation composition of 4-12:1-2:80-99
Dissipate liquid, then it is formulated to be pressed the mass ratio of 90-100:1-5 by dispersion liquid and binding agent；
(2) carbon nanotube suspension prepared being coated uniformly in substrate, 65 DEG C are dried；Substrate is formed CNT
Thin film；
(3) carbon nano-tube film that will be formed in step (2), peels off from substrate；
(4) carbon nano-tube film after peeling off in step (3) is placed in vacuum carburization stove, is warming up to 600 with 10-15 DEG C/min
DEG C, it being incubated 20-120min, then be warming up to 800 DEG C-1400 DEG C with 2-5 DEG C/min, temperature retention time is 1-10h, is cooled to after terminating
Room temperature is taken out；
(5) carbon nano-tube film after carbonization treatment in step (4) is placed in graphitizing furnace, with the intensification of 5-20 DEG C/min again
Speed is warming up to 2300 DEG C-3000 DEG C, keeps non-oxide noble gas to protect with argon, nitrogen etc. during graphitization processing
Protect, be incubated 2-36h, cool to room temperature with the furnace and take out；
(6) being rolled by twin rollers by the carbon nano-tube film after graphitization processing in step (5), twin rollers adjusts thickness and is
10-30 μm, density of film is 0.1 ~ 0.6g/cm3, thickness is 10-50 μm.
Preparation method the most according to claim 1, is characterized in that the substrate described in step (2) is flexible plastic film, copper
Paper tinsel or aluminium foil.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107046738A (en) * | 2017-04-06 | 2017-08-15 | 昆明纳太科技有限公司 | Resistance heating element and preparation method thereof |
| CN112299395A (en) * | 2020-07-29 | 2021-02-02 | 李春红 | High metallic, hydrophilic, polymer-free Carbon Nanotube (CNT) sheets and uses thereof |
| CN115124030A (en) * | 2022-08-02 | 2022-09-30 | 武汉市碳翁科技有限公司 | Method for preparing flexible self-supporting carbon nanotube film on large scale |
| CN115732702A (en) * | 2022-12-06 | 2023-03-03 | 武汉理工大学 | High-heat-conductivity current collector and high-safety lithium ion battery based on same |
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| US20130220990A1 (en) * | 2007-10-10 | 2013-08-29 | Hon Hai Precision Industry Co., Ltd. | Method for making sheet-shaped heat and light source and method for heating object using the same |
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| US20130220990A1 (en) * | 2007-10-10 | 2013-08-29 | Hon Hai Precision Industry Co., Ltd. | Method for making sheet-shaped heat and light source and method for heating object using the same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107046738A (en) * | 2017-04-06 | 2017-08-15 | 昆明纳太科技有限公司 | Resistance heating element and preparation method thereof |
| CN107046738B (en) * | 2017-04-06 | 2021-01-05 | 昆明纳太科技有限公司 | Resistance heating element and manufacturing method thereof |
| CN112299395A (en) * | 2020-07-29 | 2021-02-02 | 李春红 | High metallic, hydrophilic, polymer-free Carbon Nanotube (CNT) sheets and uses thereof |
| CN115124030A (en) * | 2022-08-02 | 2022-09-30 | 武汉市碳翁科技有限公司 | Method for preparing flexible self-supporting carbon nanotube film on large scale |
| CN115124030B (en) * | 2022-08-02 | 2023-12-22 | 武汉市碳翁科技有限公司 | Method for preparing flexible self-supporting carbon nano tube film on large scale |
| CN115732702A (en) * | 2022-12-06 | 2023-03-03 | 武汉理工大学 | High-heat-conductivity current collector and high-safety lithium ion battery based on same |
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