CN106032271A - Preparation method of carbon nanotube powder with low resistivity - Google Patents
Preparation method of carbon nanotube powder with low resistivity Download PDFInfo
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- CN106032271A CN106032271A CN201510105613.6A CN201510105613A CN106032271A CN 106032271 A CN106032271 A CN 106032271A CN 201510105613 A CN201510105613 A CN 201510105613A CN 106032271 A CN106032271 A CN 106032271A
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Abstract
The invention provides a preparation method of carbon nanotube powder with a low resistivity. The preparation method comprises the following steps: subjecting primary carbon nanotubes to a high temperature oxidation treatment in atmosphere, taking out fully oxidized carbon nanotubes, adding carbon nanotubes into an acid solution to carry out acid washing and soaking, after the requirements are met, washing the carbon nanotubes until carbon nanotubes become neutral, drying, saving carbon nanotubes for later use; doping halogen elements on the surface of dried powder, washing the powder to neutral, and drying the powder to obtain target product. The provided method can reduce the resistivity of primary carbon nanotubes with a high resistivity so as to improve the conductivity of the carbon nanotubes. The carbon nanotube powder can be used as the raw material of various composite materials.
Description
Technical field
The present invention relates to carbon nanotube dust technical field, be specifically related to the preparation method of a kind of low-resistivity carbon nanotube dust.
Background technology
CNT has the excellent properties such as excellent mechanics, optics, electricity, high temperature resistant, corrosion-resistant, light weight, and this makes
It can add phase as the preferable nanometer of one.The electrical property of its novelty has made CNT application in nanoelectronics
Increasingly receiving publicity, the effect of the electric conductivity of raising matrix is reported the most in a large number by CNT as conductive filler, but
It is substantially all on the basis of attention not being placed on the bulk conductivity promoting carbon nanometer tube material, simply focuses on carbon and receive
On combination interface between mitron and matrix, although but electric conductivity promotes do not given play to the electricity that CNT is excellent completely
Performance.
Such as describe in the patent of invention of Publication No. CN 101552052A can easily and high efficiency manufacture by low
The manufacture method of the conducting film that the CNT of resistivity is formed.Dissolve perfluor sulfuric acid polymer as dispersant in solvent
Solution dispersing Nano carbon tubes, use and be dispersed with the solution of this CNT and utilize vacuum filtration process to be formed to be formed by CNT,
And the conducting film formed by CNT is manufactured by being dried this film.This method is also only limited to a CNT and is containing
The solvent of dispersant disperses so that it is can uniformly overlap in film forming procedure and improve its conductivity, not to CNT
Carry out the process promoting electric conductivity in advance but use original CNT, if the resistance of CNT body can be entered
Row reduction processes can will promote the electric conductivity of conducting film further.
A kind of CNT with low-resistivity, high-modulus or high heat conductance is described in Publication No. CN 103827364A
Fiber and the method preparing this fiber by use fiber spinning dope spinning.The spinning solution comprising CNT is fed
In spinning head, spinning solution is extruded by least one spinneret orifice in spinning head and is spun into carbon nano-tube fibre to be formed, will spin
Carbon nano-tube fibre is become to solidify to form the carbon nano-tube fibre of solidification in setting medium.This patent uses CNT spinning
Stock solution carries out wet spinning, and the CNT in CNT spinning solution is not the most through any process technique, and it is prepared
The carbon nano-tube fibre low-resistivity become also is only the resistivity of the body relying on CNT, is not involved with CNT
Powder body carries out reducing the process of its bulk resistivity.
Summary of the invention
The technical problem to be solved is the deficiency for above-mentioned existence, it is provided that a kind of carbon by original high resistivity is received
The bulk resistivity of mitron reduces, thus promotes the electric conductivity of its body, it is possible to as preparing the raw material of various composite,
Particularly can promote the preparation method of the low-resistivity carbon nanotube dust of conductivity of composite material energy.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of low-resistivity carbon nanotube dust, it is characterised in that include following steps:
The oxidation processing technique of CNT:
Use original CNT, put in Muffle furnace or other high-temperature services and carry out high temperature oxidation process, remove
The amorphous carbon on its surface and some easy vaporization at high temperature or the material of decomposition, and make some defective locations of original carbon nanotubes surface
Regrow Guan Bi, obtains powder body A；
The pickling soaking technology of CNT:
CNT through high temperature oxidation process is mixed according to proportioning and acid solution, takes out after applying stirring, washed to
After neutrality, obtain can be used for the powder body B of subsequent technique；
Carbon nano tube-doped technique:
By powder body B with the material of halogen can be doped mix, this type of material include halogen (fluorine, chlorine,
Bromine, iodine) simple substance or the compounding substances of the most several element, after to take high temperature or strong illumination to process in closing container anti-
Taking out after should, washing is ground to neutral drying, prepares the carbon nanotube dust of low-resistivity.
In such scheme, in the oxidation processing technique of described CNT, high-temperature oxydation temperature is 100-800 DEG C, high temperature
Oxidization time is 5-300min.
In such scheme, in the pickling soaking technology of described CNT, acid solution is the one of hydrochloric acid, sulphuric acid and nitric acid
Or several mixed solutions, concentration is 10%-80%, and the time of CNT and acid mixing is 3-240min, and mixing speed is
100-1000rpm。
In such scheme, in described carbon nano tube-doped technique, CNT controls at 1g with the ratio of halogen family material:
0.1ml-1g:5ml.
In such scheme, in described carbon nano tube-doped technique, if doping reaction takes high-temperature process, its reaction temperature is
50-300 DEG C, the response time is 30-720min.
In such scheme, in described carbon nano tube-doped technique, if doping reaction takes strong illumination to process, during its reaction
Between be 30-1440min.
In such scheme, described CNT is appointing in SWCN, multi-walled carbon nano-tubes and double-walled carbon nano-tube
Anticipating one or more combination in any, CNT caliber is 1nm～100nm.
The beneficial effects of the present invention is:
(1) CNT body is carried out process and can effectively promote its bulk conductivity, the resistance of more original CNT
Rate reduces 50%-70%, haves laid a good foundation for the electric conductivity giving full play to CNT excellent, and it can be as carrying
Rise the excellent filler of composite material conductive rate.
(2) CNT processed through this method, owing to changing the characteristic of its body construction, verifies through lot of experiments
After, it has more excellent dispersive property compared to original CNT, thus solves in preparation composite material
A key difficult problem.
Accompanying drawing explanation
Fig. 1 is the method flow diagram of the embodiment of the present invention 1；
Fig. 2 is the SEM photograph of powder body A in the embodiment of the present invention 1；
Fig. 3 is the SEM photograph of powder body B in the embodiment of the present invention 1.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated:
Embodiment 1:
Seeing Fig. 1, this height is led carbon-nanotube-modialuminum aluminum material preparation method and is achieved in that
Step one sees Fig. 2, the oxidation processing technique of CNT:
Using original caliber is 60nm multi-walled carbon nano-tubes, puts in Muffle furnace or other high-temperature services,
Oxidation processes 30min under 600 DEG C of high temperature, removes the amorphous carbon on its surface and some easy vaporization at high temperature or the material of decomposition, and makes
Some defective locations of original carbon nanotubes surface regrow Guan Bi, obtain powder body A；
Step 2 sees Fig. 3, the pickling soaking technology of CNT:
Multi-walled carbon nano-tubes through high temperature oxidation process is joined in the concentrated hydrochloric acid that concentration is 36.5% and soak, apply stirring
Take out after 100rpm mixing 10min, washed to neutrality, obtain can be used for the powder body B of subsequent technique；
The carbon nano tube-doped technique of step 3:
Being mixed by powder body B and ICl, mixed proportion is 1g:0.1ml, after process 480min closing in container 200 DEG C
Rear taking-up, washing is ground to neutral drying, is prepared the multi-walled carbon nano-tubes powder body of low-resistivity.
Embodiment 2:
The present embodiment difference from embodiment 1 is, the CNT employed in step one is SWCN, caliber
For 2nm.
Embodiment 3:
The present embodiment difference from embodiment 1 is, step 2 used halogen family material is elemental iodine.
Embodiment 4:
The present embodiment difference from embodiment 1 is, step 3 is processing the composite granule obtained, strong illumination through high light
Shi Changwei 720min.
Embodiment 5:
The present embodiment difference from embodiment 1 is, in step 3, powder body B and ICl mixed proportion are 1g:1ml.
Each embodiment processes CNT and original carbon nanotubes resistance value contrast test data
The Application Example being only the present invention described above, can not limit the interest field of the present invention with this, therefore certainly
The equivalence change made according to scope of the present invention patent, still belongs to protection scope of the present invention.
Claims (7)
1. the preparation method of a low-resistivity carbon nanotube dust, it is characterised in that include following steps:
The oxidation processing technique of CNT:
Use original CNT, put in Muffle furnace or other high-temperature services and carry out high temperature oxidation process, remove
The amorphous carbon on its surface and some easy vaporization at high temperature or the material of decomposition, and make some defective locations of original carbon nanotubes surface
Regrow Guan Bi, obtains powder body A；
The pickling soaking technology of CNT:
CNT through high temperature oxidation process is mixed according to acid solution, takes out after applying stirring, washed to neutral
After, obtain can be used for the powder body B of subsequent technique；
Carbon nano tube-doped technique:
By powder body B with the material of halogen can be doped mix, this type of material include halogen (fluorine, chlorine,
Bromine, iodine) simple substance or the compounding substances of the most several element, after to take high temperature or strong illumination to process in closing container anti-
Taking out after should, washing is ground to neutral drying, prepares the carbon nanotube dust of low-resistivity.
2. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
In the oxidation processing technique of pipe, high-temperature oxydation temperature is 100-800 DEG C, and the high-temperature oxydation time is 5-300min.
3. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
In the pickling soaking technology of pipe, acid solution is one or several mixed solution of hydrochloric acid, sulphuric acid and nitric acid, and concentration is
10%-80%, the time of CNT and acid mixing is 3-240min, and mixing speed is 100-1000rpm.
4. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
In pipe doping process, CNT controls at 1g:0.1ml-1g:5ml with the ratio of halogen family material.
5. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
In pipe doping process, if doping reaction takes high-temperature process, its reaction temperature is 50-300 DEG C, and the response time is 30-720min.
6. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
In pipe doping process, if doping reaction takes strong illumination to process, its response time is 30-1440min.
7. the preparation method of low-resistivity carbon nanotube dust as claimed in claim 1, it is characterised in that described carbon nanometer
Pipe is any one in SWCN, multi-walled carbon nano-tubes and double-walled carbon nano-tube or two or more combination in any, carbon
Nanotube caliber is 1nm～100nm.
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| CN201510105613.6A CN106032271A (en) | 2015-03-11 | 2015-03-11 | Preparation method of carbon nanotube powder with low resistivity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766664A (en) * | 2018-05-15 | 2018-11-06 | 王召惠 | A kind of preparation method of Modified Activated Carbon element base electrode paste |
| CN110817846A (en) * | 2018-08-10 | 2020-02-21 | 南京大学 | Low-cost large-scale modification technology for improving conductivity and specific surface area of carbon nanotube film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020127171A1 (en) * | 2001-02-12 | 2002-09-12 | William Marsh Rice University | Process for purifying single-wall carbon nanotubes and compositions thereof |
| CN101164874A (en) * | 2007-09-26 | 2008-04-23 | 合肥工业大学 | Method for purifying multi-wall carbon nano pipe |
-
2015
- 2015-03-11 CN CN201510105613.6A patent/CN106032271A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020127171A1 (en) * | 2001-02-12 | 2002-09-12 | William Marsh Rice University | Process for purifying single-wall carbon nanotubes and compositions thereof |
| CN101164874A (en) * | 2007-09-26 | 2008-04-23 | 合肥工业大学 | Method for purifying multi-wall carbon nano pipe |
Non-Patent Citations (2)
| Title |
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| 唐国强等: "溴吸附对碳纳米管导电性能的提高", 《化学学报》 * |
| 赵成大: "《固体量子化学-材料化学的理论基础》", 31 August 2003, 高等教育出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766664A (en) * | 2018-05-15 | 2018-11-06 | 王召惠 | A kind of preparation method of Modified Activated Carbon element base electrode paste |
| CN110817846A (en) * | 2018-08-10 | 2020-02-21 | 南京大学 | Low-cost large-scale modification technology for improving conductivity and specific surface area of carbon nanotube film |
| CN110817846B (en) * | 2018-08-10 | 2022-08-12 | 南京大学 | Low-cost large-scale modification technology for improving conductivity and specific surface area of carbon nanotube film |
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