CN109721046A - A kind of preparation method of conductive carbon nanotube - Google Patents
A kind of preparation method of conductive carbon nanotube Download PDFInfo
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- CN109721046A CN109721046A CN201811028240.7A CN201811028240A CN109721046A CN 109721046 A CN109721046 A CN 109721046A CN 201811028240 A CN201811028240 A CN 201811028240A CN 109721046 A CN109721046 A CN 109721046A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 68
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000005336 cracking Methods 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 239000010453 quartz Substances 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000011946 reduction process Methods 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 230000036541 health Effects 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of conductive carbon nanotube, steps are as follows: S1, weighs catalyst and is dissolved in organic carbon source, stand quartz glass plate 20h or more, is pushed into tube furnace reactor；S2, it is passed through N at room temperature2The air in tube furnace reactor is excluded, continues to be passed through N2, heating makes furnace temperature rise to cracking temperature by room temperature, after furnace temperature rises to cracking temperature, starts to be passed through H2, react a few hours, stopping is passed through H2, turn N down2Flow, the reaction made are cooled to 100 DEG C in nitrogen protection atmosphere, and sample is scraped from quartz plate to get desired conductive carbon nanotube.The present invention prepares carbon nanotube by catalyst atmosphere reduction method, using hydrogen as reducing agent, nontoxic, health environment-friendly, and can reduce oxygen-containing functional group in reduction process and remain；Catalyst is added in reduction process, the missing that can be rolled into a ball can be further reduced, so that carbon nanotube contains more conductive group, electric conductivity is excellent, and is suitable for industrialized production carbon nanotube.
Description
Technical field
The present invention relates to conductive new material synthetic method field, especially a kind of preparation method of conductive carbon nanotube.
Background technique
Carbon nanotube (Carbon nanotubes, abbreviation CNTs) is a kind of One-dimensional Quantum material with special construction,
Its radial dimension can reach nanoscale, and axial dimension is micron, and the both ends of pipe are generally all sealed, carbon atomic layer interconnected
Tubular structure made of curling, diameter nanometer are differed from one nanometer to tens, and length longest is up to several centimeters, while huge length
The diameter carbon fiber more fabulous than being expected to it is made to be fabricated to toughness.Since it is with biggish draw ratio, excellent mechanics, electricity, magnetic
, thermodynamic property and broad application prospect, have attracted the sight of numerous studies personnel, these features outstanding make for a long time
Multiple practical applications occasion can be applicable in by obtaining carbon nanotube, wherein be had become using carbon nanotube as conductive material, electrode material
For the research focus in clean energy resource field.
Currently, a large amount of patent and common preparation method of carbon nano-tube reported in the literature mainly have both at home and abroad: arc discharge
Method, chemical vapour deposition technique, laser evaporization method, template method etc..How to prepare the carbon nanotube that purity is higher, fault of construction is few is
How the precondition that further investigation application is carried out to it, obtain that easy controlled operation, production cost are low, raw material availability is high, structure
Few, the with high purity preparation method of defect also needs further to further investigate；The missing of part carbon atom is so that system in production preparation
Carbon nanotube contain more defect, make its electric conductivity reduction, and then limit its to carbon nanotube mass requirement compared with
Application in high field.But its process of existing preparation method is still relatively complicated and time-consuming long, furthermore prepared carbon
The electric conductivity of nanotube is still bad, it is difficult to meet the fields such as the high conductive industry of conductive industry, electrodes conduct industry, light transmittance
Requirement.
Summary of the invention
The defects of in view of the prior art, a kind of preparation method of conductive carbon nanotube is provided.
The present invention is realized by following proposal:
A kind of preparation method of conductive carbon nanotube, the preparation method the following steps are included:
S1, it weighs catalyst and is dissolved in organic carbon source, stand quartz glass plate 20h or more, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in tube furnace reactor is excluded, continues to be passed through N2, heating makes furnace temperature by room temperature liter
Start to be passed through H after furnace temperature rises to cracking temperature to cracking temperature2, react a few hours, stopping is passed through H2, turn N down2Flow,
The reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, and sample is scraped from quartz plate to get desired conductive carbon nanotube
Pipe.
The catalyst is the Fe/Co, Fe/Ni, Fe/Cu, at least one of Ni/Ag of commercialization.
The organic carbon source is at least one of ortho-xylene, paraxylene, toluene.
The reaction starts the H being passed through2Flow be 200-300mL/min, the N being passed through in reaction process2Flow 500-
800mL/min。
The furnace temperature of tube furnace reactor is risen into cracking temperature by room temperature within 15-24h.
The reaction time is 3-5 hours.
The sheet resistance value of the conductive carbon nanotube is no more than 100m Ω/.
The invention has the benefit that
A kind of preparation method of conductive carbon nanotube of the present invention prepares carbon nanotube by catalyst atmosphere reduction method, uses
Hydrogen can reduce oxygen-containing functional group in reduction process and remain as reducing agent, nontoxic, health environment-friendly；It is added in reduction process
Catalyst can be further reduced the missing that can be rolled into a ball, so that carbon nanotube contains more conductive group, electric conductivity is excellent；This
It invents that the preparation method is fast and convenient, the production cost of carbon nanotube can be greatly reduced and improves production efficiency, be suitable for
Industrialized production carbon nanotube.
Detailed description of the invention
Fig. 1 is the transmission electron microscope of carbon nanotube prepared by a kind of preparation method of conductive carbon nanotube of the application
Figure；
Fig. 2 is the transmission electron microscope figure of carbon nanotube prepared by a kind of preparation method of conductive carbon nanotube of the application
The figure of amplification.
Specific embodiment
The preferred embodiment of the invention is further illustrated below:
A kind of preparation method of conductive carbon nanotube, the preparation method the following steps are included:
S1, it weighs catalyst and is dissolved in organic carbon source, stand quartz glass plate 20h or more, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in tube furnace reactor is excluded, continues to be passed through N2, heating makes furnace temperature by room temperature liter
Start to be passed through H after furnace temperature rises to cracking temperature to cracking temperature2, react a few hours, stopping is passed through H2, turn N down2Flow,
The reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, and sample is scraped from quartz plate to get desired conductive carbon nanotube
Pipe.
The catalyst is the Fe/Co, Fe/Ni, Fe/Cu, at least one of Ni/Ag of commercialization.
The organic carbon source is at least one of ortho-xylene, paraxylene, toluene.The reaction starts the H being passed through2
Flow be 200-300mL/min, the N being passed through in reaction process2Flow 500-800mL/min.By tubular type within 15-24h
The furnace temperature of furnace reactor rises to cracking temperature by room temperature.The reaction time is 3-5 hours.The sheet resistance of the conductive carbon nanotube
Value is no more than 100m Ω/.
Wherein, in practical applications, the catalyst, organic carbon source mass ratio are as follows: (1-2): (20-50).
The present invention passes through catalyst atmosphere reduction method and controls carbon source to be contained system and realizes with catalyst proportion, reducing atmosphere
The preparation of carbon nanotube.The dispersibility of the preparation process carbon nanotube in water is preferably, it is easy to accomplish the modification to carbon nanotube
And functionalization；The presence of catalyst appropriate also further reduces the missing of carbon atom in reduction process in preparation process, into
One step improves the electric conductivity of carbon nanotube.Preparation method of the present invention is fast and convenient, can greatly reduce carbon nanotube
Production cost and raising production efficiency, are suitable for industrialized production carbon nanotube.
The application is further elaborated below with reference to specific embodiment.
Embodiment 1
A kind of Conductive carbon nanotubes, preparation process are as follows:
S1,2g Fe/Co and 25g ortho-xylene is mixed, stands quartz glass plate 20h, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 200mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 2
A kind of Conductive carbon nanotubes, preparation process are as follows:
S1,1.5g Fe/Ni and 28g ortho-xylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 200mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 3
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.5g Fe/Ni and 28g paraxylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 4
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.8g Fe/Cu and 30g paraxylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 5
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.5g Fe/Ni and 28g toluene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 6
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.9g Ni/Ag and 28g toluene is mixed, stands quartz glass plate 30h, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 7
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.8g Ni/Ag and 30g paraxylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 8
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.8g Fe/Co and 30g paraxylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 200mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 9
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.8g Fe/Cu and 30g paraxylene is mixed, stands quartz glass plate 25h, be pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 15h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
Embodiment 10
A kind of Conductive carbon nanotubes, preparation method process are as follows:
S1,1.8g Fe/Cu and 30g neck dimethylbenzene are mixed, stands quartz glass plate 25h, is pushed into tube furnace reactor
In；
S2, it is passed through N at room temperature2The air in reaction system is excluded, 500mL/min N is passed through2.Make furnace temperature by room in 20h
Temperature rise is to cracking temperature, in starting the H for being passed through 300mL/min flow after furnace temperature rises to cracking temperature2, 5h is reacted, is stopped
Only it is passed through H2, turn nitrogen flow down, the reaction made is cooled to 100 DEG C in nitrogen protection atmosphere, sample is taken out, by it from quartz
Piece scrapes to get desired sample.
A kind of Conductive carbon nanotubes that the present invention prepares embodiment 1 have carried out transmission electron microscope detection, implement
The transmission electron microscope figure of carbon nanotube prepared by example 1 such as Fig. 1, shown in the high power projection electron microscope of the position Fig. 2 amplification.By scheming
1 and figure it is found that a length of size of carbon nanotube that is prepared of embodiment 1 is 1.0-1.2 microns, caliber 30-40nm.
A kind of electric conductivity of Conductive carbon nanotubes of embodiment 1-10 is surveyed with reference to national standard GB/T1410-2006
Examination, measures its sheet resistance value, measurement result is shown in Table 1.
1 carbon nano-tube conductive energy test result of table
| Detection project | Sheet resistance (m Ω/) |
| Embodiment 1 | 80.2 |
| Embodiment 2 | 85.6 |
| Embodiment 3 | 98.3 |
| Embodiment 4 | 88.6 |
| Embodiment 5 | 85.4 |
| Embodiment 6 | 85.0 |
| Embodiment 7 | 90.6 |
| Embodiment 8 | 85.9 |
| Embodiment 9 | 89.8 |
| Embodiment 10 | 95.6 |
From embodiment 1-10 it is found that Conductive carbon nanotubes excellent electric conductivity, sheet resistance prepared by the present invention are below
100mΩ/□.The present invention prepares carbon nanotube by catalyst atmosphere reduction method, using hydrogen as reducing agent, nontoxic, health
Environmental protection, and oxygen-containing functional group in reduction process can be reduced and remained；Catalyst is added in reduction process, can be further reduced can roll into a ball
Missing, so that carbon nanotube contains more conductive group, electric conductivity is excellent；Preparation method of the present invention is fast and convenient,
The production cost of carbon nanotube can be greatly reduced and improve production efficiency, be suitable for industrialized production carbon nanotube.
Although having done more detailed elaboration to technical solution of the present invention and having enumerated, it should be understood that for ability
For field technique personnel, modifications to the embodiments described above may be made or uses equivalent alternative solution, this is to those skilled in the art
It is it is clear that these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the present invention for member
Claimed range.
Claims (7)
1. a kind of preparation method of conductive carbon nanotube, which is characterized in that the preparation method the following steps are included:
S1, it weighs catalyst and is dissolved in organic carbon source, stand quartz glass plate 20h or more, be pushed into tube furnace reactor；
S2, it is passed through N at room temperature2The air in tube furnace reactor is excluded, continues to be passed through N2, heating, which rises to furnace temperature by room temperature, splits
Solution temperature starts to be passed through H after furnace temperature rises to cracking temperature2, react a few hours, stopping is passed through H2, turn N down2Flow makes
Reaction is cooled to 100 DEG C in nitrogen protection atmosphere, and sample is scraped from quartz plate to get desired conductive carbon nanotube.
2. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: the catalyst is quotient
The Fe/Co of product, Fe/Ni, Fe/Cu, at least one of Ni/Ag.
3. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: the organic carbon source is
At least one of ortho-xylene, paraxylene, toluene.
4. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: the reaction starts to lead to
The H entered2Flow be 200-300mL/min, the N being passed through in reaction process2Flow 500-800mL/min.
5. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: will within 15-24h
The furnace temperature of tube furnace reactor rises to cracking temperature by room temperature.
6. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: the reaction time is
3-5 hours.
7. a kind of preparation method of conductive carbon nanotube according to claim 1, it is characterised in that: the conductive carbon nanotube
The sheet resistance value of pipe is no more than 100m Ω/.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110482548A (en) * | 2019-09-04 | 2019-11-22 | 中国科学院山西煤炭化学研究所 | A method of removing super capacitor active carbon oxygen-containing functional group |
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Application publication date: 20190507 Assignee: Jiangsu Jiangan Precision Mould Co.,Ltd. Assignor: Jiangsu electronic information Vocational College Contract record no.: X2023980052417 Denomination of invention: A preparation method for conductive carbon nanotubes Granted publication date: 20230606 License type: Common License Record date: 20231218 |