CN106396680A - Preparation method of flexible ultrathin carbon nanotube paper - Google Patents
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
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- C04B2235/52—Constituents or additives characterised by their shapes
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Abstract
The invention provides a preparation method of flexible ultrathin carbon nanotube paper. The preparation method comprises steps as follows: firstly, carbon nanotubes wetted with ethanol or acetone are added to distilled water and subjected to ultrasonic dispersion; then, pulp fibers are added, a high-speed shearing emulsifying machine is used for sufficient mixing and dispersion, and conductive carbon nanotube paper is prepared with an ordinary papermaking process; the carbon nanotube paper is modified and then subjected to graphitization; finally, the carbon nanotube paper is rolled by a roll crusher. Compared with conventional carbon nanotube paper, the carbon nanotube paper has the advantages that the conductivity is improved remarkably, and the strength and the flexibility are improved apparently through rolling. A product can be cut into required shapes and sizes, or a conductive carbon nanotube paper product with the specific shape and size is directly manufactured.
Description
Technical field
The invention belongs to chemistry and field of functional materials, be related to the pretreatment of CNT, dispersion, charing, graphitization and
The technology such as rolling.
Background technology
CNT has excellent electrical conduction, heat-conductive characteristic, so that CNT is widely used in many fields
Space, particularly outstanding mechanical property and mechanical performance, because CNT is nano material, its excellent physical and chemical performance
It is difficult to macroscopically showing.So in a lot of research, paper being relied on to carry CNT as matrix and to obtain a kind of being combined
The conductive paper with superperformance.
The preparation method of the carbon nano tube conductive paper of report is broadly divided into two kinds at present:The first, by preparing carbon nanometer
Pipe conductive ink is coated on paper, and this method can retain the physical properties such as the form of good paper, intensity, but this conductive paper is
Single-sided conductive, it is hardly formed the conductive network of three-dimensional;Second, will be black by carbon nanotube conducting by the method for papermaking again
Again it is combined into paper, this method can utilize the adsorptivity of paper and easy formability, so that CNT is filled after being combined with paper fiber
Point dispersion, be adsorbed in paper fiber surface, form three-dimensional conductive network, but the carbon nanotube paper that obtains of this method lose original
The intensity of paper and physical property, limit the space of its application.
Charing, graphitization are the conventional means in heat treatment, are applied to make the carbon content rate of material improve in material with carbon element,
Make amorphous carbon farthest be converted into crystalline structure, improve electric conductivity and the thermal conductivity of material.Rolling process can make material
Material internal structure consolidation, defect is less, and uniformity improves, and then improves intensity and the pliability of material.
Content of the invention
The purpose of the present invention is a kind of preparation method of flexible ultra-thin carbon nanotube paper, can simply, quick, efficient make
Standby flexible ultra-thin carbon nanotube paper, and process the performance of modified carbon nano-tube by series of process, thus improving CNT
The serviceability of paper.
The present invention is achieved by the following technical solutions, and concrete steps include as follows.
(1)To add in distilled water in CNT after ethanol or acetone wetting, 1-3h processed using ultrasonic disperse,
Make CNT dispersed in a liquid.
(2)Using high-speed shearing emulsion machine, pre-dispersed CNT and paper pulp fiber are sufficiently mixed, disperse, answered
Close suspension.
(3)Compound suspension deposition is obtained carbon nano tube conductive paper by the method using common papermaking, is placed in vacuum drying
Case, 65 DEG C are dried 1-3h.
(4)The modification of carbon nanotube paper, the carbon nanotube paper after peeling off is placed in vacuum carbonized stove, with 10-15
DEG C/min is warming up to 600 DEG C, 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)By step(4)Carbon nanotube paper after charing process is placed in graphitizing furnace again, with the intensification of 5-20 DEG C/min
Speed is warming up to 2300 DEG C -3000 DEG C, uses argon gas, nitrogen etc. to keep non-oxide inert gas to protect during graphitization processing
Shield, is incubated 2-36h, cools to room temperature with the furnace and takes out.
(6)Carbon nanotube paper after graphitization processing is rolled by twin rollers, twin rollers roll-in thickness is 0.05-1mm,
Density 0.1 ~ 0.4g/cm that after roll-in, carbon nanotube paper is3, thickness is 0.1-1mm.
The carbon nanotube paper of the present invention is obviously improved than front electric conductivity, through rolling, its intensity, pliability is obtained bright
Aobvious improvement.Product of the present invention can be cut into the shapes and sizes of needs, or the carbon being manufactured directly to specific shapes and sizes
Nanotube conductive paper product.
Brief description
Accompanying drawing 1 is the carbon nano tube conductive paper SEM figure of invention.
Accompanying drawing 2 is the carbon nano tube conductive paper photo of the present invention.
Specific embodiment
The present invention will be described further by following examples.
The present embodiment selects crystal whisker-shaped carbon nanotube(ZL201210067937.1、ZL201210304345.7)As conduction
Agent.
Embodiment 1.
1st, 1g CNT is added in 500ml distilled water, add appropriate dispersant, process 1 hour through ultrasonic disperse
Make CNT dispersed in a liquid.
2nd, by above-mentioned carbon nano-tube solution and paper pulp stirring mixing, by high-speed shearing emulsion machine by CNT and paper pulp
Full and uniform dispersion.
3rd, scattered CNT and pulp solution are passed through to copy to filter into paper, vacuum drying is prepared into CNT and leads
Electric paper.
4th, carbon nanotube paper is placed in the carbide furnace being filled with argon gas protection, 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, be cooled to room temperature after terminating and take out.
5th, the carbon nanotube paper after carbonization treatment is placed in graphitizing furnace, is passed through argon gas as protective gas, with 15 DEG C/
The programming rate of min is warming up to 2800 DEG C, and temperature retention time is 12h, and cooling after graphitization terminates is taken out.
6th, the carbon nanotube paper after graphitization processing is passed through twin rollers rolling process, density is about 0.22g/cm3, thickness
For 0.1mm.
Embodiment 2.
1st, 1g CNT is added in 500ml absolute ethyl alcohol, add appropriate dispersant, process 1 through ultrasonic disperse little
When make CNT dispersed in a liquid.
2nd, by above-mentioned carbon nano-tube solution and paper pulp stirring mixing, then with high-speed shearing emulsion machine by CNT and paper pulp
Full and uniform dispersion.
3rd, scattered CNT and pulp solution are passed through to copy to filter into paper, vacuum drying is prepared into CNT and leads
Electric paper.
4th, carbon nanotube paper is placed in the carbide furnace being filled with argon gas protection, 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, be cooled to room temperature after terminating and take out.
5th, the carbon nanotube paper after carbonization treatment is placed in graphitizing furnace, is passed through argon gas as protective gas, with 15 DEG C/
The programming rate of min is warming up to 2900 DEG C, and temperature retention time is 18h, and cooling after graphitization terminates is taken out.
6th, the carbon nanotube paper after graphitization processing is passed through twin rollers rolling process, density is about 0.39g/cm3, thickness
For 0.05mm.
Claims (1)
1. a kind of preparation method of flexible ultra-thin carbon nanotube paper, is characterized in that comprising the steps:
(1)To add in distilled water in the CNT after ethanol or acetone wetting, ultrasonic disperse processes 1-3h, makes carbon nanometer
Pipe is dispersed in a liquid;
(2)Using high-speed shearing emulsion machine, pre-dispersed CNT and paper pulp fiber are sufficiently mixed, disperse, obtain compound outstanding
Turbid liquid;
(3)Compound suspension deposition is obtained carbon nano tube conductive paper by the method using common papermaking, is placed in vacuum drying box, and 65
DEG C 1-3h is dried;
(4)Carbon nanotube paper after peeling off is placed in vacuum carbonized stove, is warming up to 600 DEG C with 10-15 DEG C/min, be incubated 20-
120min, then it 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)By step(4)Carbon nanotube paper after charing process is placed in graphitizing furnace again, with the programming rate of 5-20 DEG C/min
It is warming up to 2300 DEG C -3000 DEG C, use argon gas, nitrogen etc. to keep non-oxide inert gas shielding during graphitization processing, protect
Warm 2-36h, cools to room temperature with the furnace and takes out;
(6)Carbon nanotube paper after graphitization processing is rolled by twin rollers, twin rollers roll-in thickness is 0.05-1mm, roll-in
Density 0.1 ~ 0.4g/cm that carbon nanotube paper is afterwards3, thickness is 0.1-1mm.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106835847A (en) * | 2017-03-13 | 2017-06-13 | 南昌大学 | A kind of preparation method of bio-compatibility carbon nanometer tube/hydroxyapatite extrusion coating paper |
CN107012720A (en) * | 2017-03-13 | 2017-08-04 | 南昌大学 | A kind of conductive non-woven fabrics preparation method of bio-compatible |
CN108385450A (en) * | 2018-01-23 | 2018-08-10 | 柔电(武汉)科技有限公司 | A kind of carbon nanotube paper and preparation method thereof |
CN109167093A (en) * | 2018-09-03 | 2019-01-08 | 江西克莱威纳米碳材料有限公司 | A kind of hydroxylating whisker carbon nanotube paper and preparation method thereof and a kind of lithium-sulfur cell |
CN109256564A (en) * | 2018-09-10 | 2019-01-22 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-graphite composite material, lithium sulfur battery anode material and lithium-sulfur cell |
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CN105047940A (en) * | 2015-06-16 | 2015-11-11 | 南昌大学 | Preparation method of carbon nanotube film |
CN105514434A (en) * | 2016-01-19 | 2016-04-20 | 南昌大学 | Preparation method of whisker-shaped carbon nano tube film |
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CN102561109A (en) * | 2011-12-20 | 2012-07-11 | 南昌大学 | Method for preparing carbon nano tube conductive paper |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106835847A (en) * | 2017-03-13 | 2017-06-13 | 南昌大学 | A kind of preparation method of bio-compatibility carbon nanometer tube/hydroxyapatite extrusion coating paper |
CN107012720A (en) * | 2017-03-13 | 2017-08-04 | 南昌大学 | A kind of conductive non-woven fabrics preparation method of bio-compatible |
CN108385450A (en) * | 2018-01-23 | 2018-08-10 | 柔电(武汉)科技有限公司 | A kind of carbon nanotube paper and preparation method thereof |
CN109167093A (en) * | 2018-09-03 | 2019-01-08 | 江西克莱威纳米碳材料有限公司 | A kind of hydroxylating whisker carbon nanotube paper and preparation method thereof and a kind of lithium-sulfur cell |
CN109256564A (en) * | 2018-09-10 | 2019-01-22 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-graphite composite material, lithium sulfur battery anode material and lithium-sulfur cell |
CN109256564B (en) * | 2018-09-10 | 2021-07-09 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-graphite composite material, lithium-sulfur battery positive electrode material and lithium-sulfur battery |
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