CN108059150A - Doped carbon nanometer pipe and preparation method thereof - Google Patents
Doped carbon nanometer pipe and preparation method thereof Download PDFInfo
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- CN108059150A CN108059150A CN201711454326.1A CN201711454326A CN108059150A CN 108059150 A CN108059150 A CN 108059150A CN 201711454326 A CN201711454326 A CN 201711454326A CN 108059150 A CN108059150 A CN 108059150A
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- nickel
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- melamine
- nanometer pipe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to field of nanometer material technology, and in particular to a kind of doped carbon nanometer pipe and preparation method thereof.Doped carbon nanometer pipe is by melamine and nickel source with molar ratio 1:13 ratio is mixed with to obtain.A kind of new doped carbon nanometer pipe is provided, using the melamine of low cost as carbon source, nanotube of good performance can be prepared.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of doped carbon nanometer pipe and preparation method thereof.
Background technology
Carbon nanotubes is because its unique mechanics, electronics and chemical characteristic, in physics, chemistry, information technology, environment section
The fields such as, material science, energy technology, life and medical science have broad application prospects.Carbon nanotubes is mixed
It is miscellaneous, i.e., with the carbon atom of other elements substitution carbon nanotubes tube wall, form a kind of process of composite carbon nanometer tube, thus it is possible to vary carbon
The crystal structure and electronic structure of nanotube, so as to change the physics of carbon nanotubes, chemical property.Carbon nanotubes after doping is past
Toward having unusual morphological feature, the acquisition of the carbon nanotubes of doping is expected to further tighten and improve this performance.
The content of the invention
It is an object of the invention to provide a kind of doped carbon nanometer pipe, the present invention provides a kind of new doped carbon nanometer pipe,
Nanotube of good performance can be prepared using the melamine of low cost as carbon source in it.
Another object of the present invention is to provide a kind of preparation method of doped carbon nanometer pipe, method is simple, operation letter
Easily, it is of low cost, easily realize industrialization.
The present invention is solved its technical problem and is realized using following technical scheme：
The present invention proposes a kind of doped carbon nanometer pipe, by melamine and nickel source with molar ratio 1:The ratio of 1-3 is mixed
Conjunction is prepared, and is preferably 1：2-3.
The present invention proposes a kind of preparation method of doped carbon nanometer pipe, by after melamine and nickel source ball milling in 800-1200
It is calcined in the environment of DEG C.
The advantageous effect of doped carbon nanometer pipe of the present invention and preparation method thereof is：The doped carbon nanometer pipe of the present invention, profit
It is carbon source with melamine, the carbon nanometer of doping nitrogen-atoms and the hexatomic ring with rock-steady structure is automatically derived in calcination process
Pipe is then that nickel source reaction further obtains the carbon nanotubes of doping nickel, can further promote the performance of carbon nanotubes.And
The cost of material for preparing the carbon nanotubes is low, operating method is simple answers, is easily achieved industrialization.
Description of the drawings
It in order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of scope, for those of ordinary skill in the art, without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the electron-microscope scanning figure of the doped carbon nanometer pipe of embodiment 1.
Specific embodiment
It, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
In the description of the present invention, it is necessary to which explanation, term " first ", " second " etc. are only used for distinguishing description, without
It is understood that indicate or imply relative importance.
Doped carbon nanometer pipe of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of doped carbon nanometer pipe provided in an embodiment of the present invention, by melamine and nickel source with molar ratio 1:1-3
Ratio be mixed with to obtain, be preferably 1：2-3.The doped carbon nanometer pipe is using melamine as carbon source, then with nickel to preparing
Obtained carbon nanotubes is modified, and then promotes the performance of carbon nanotubes.Melamine is hexagonal array in itself, and is led to
Calcining is crossed so that the double bond in raw material is broken so that the carbon nanotubes being prepared is doped with nitrogen-atoms automatically, then changes carbon
The electronic structure of nanotube expands the performance of carbon nanotubes, simultaneously so that it can have sp simultaneously2And sp3Mixed hybridization shape
State then forms carbon nanotubes, and obtained carbon nanotubes is further modified by nickel, promotes the property of carbon nanotubes
Energy.
It is the nickel because the carbon nano tube structure prepared with melamine is relatively stablized that melamine and nickel source, which use aforementioned proportion,
Source is not easy to adulterate, and by increasing the ratio of nickel source, it can ensure there is sufficient amount of nickel to be doped into carbon nanotubes, then protect
Demonstrate,prove the performance for the doped carbon nanometer pipe being prepared.
Further, nickel source is nickel compound, is preferably nickel chloride, more preferably Nickel dichloride hexahydrate.In the feelings of heating
Under condition, Nickel dichloride hexahydrate can be doped in carbon nanotubes, then can smoothly change the performance of carbon nanotubes.
The present invention also provides a kind of preparation methods of doped carbon nanometer pipe, comprise the following steps：
S1, ball milling；
Melamine and nickel source are proportionally carried out to be mixed to get mixture, then by mixture be put into ball mill into
Row ball milling.It is mixed rather than is mixed in mechanical milling process first, be to add raw material in mechanical milling process in order to prevent, cause
Raw material ball milling degree is uneven, and mixes uneven between raw material, and nickel source is then caused good cannot to be adhered to melamine
On.
It is not only the grain size for reducing nickel source and melamine compound to carry out ball milling, even more so that nickel source is in mechanical milling process
It is middle good to be adhered to melamine surface, then so that in thickness calcination process that nickel is good to be doped to carbon nanotubes
It is interior, then ensure the performance for the carbon nanotubes being prepared.
Further, when ball milling is that ball milling 1-2 is small after melamine is mixed with nickel source, the rotating speed of ball milling is 300r/min
~400r/min.Ball milling is carried out using aforesaid operations condition, can ensure that melamine and nickel source are uniformly mixed, and can be so that three
Poly cyanamid and nickel source are in a suitable particle size range.Meanwhile, it is capable to ensure that nickel source can smoothly be adhered to melamine table
Face, when grinding 1-2 is small, mixture becomes powder.
S2, drying；
Melamine and nickel source are adsorbed with to the presoma of nickel source after ball milling by being dried to obtain.
Dry temperature is 60-80 DEG C.
Melamine and nickel source are ground to the smaller powder of grain size in process of lapping, may be contained inside raw material a small amount of
Moisture, then easily bonding is the larger block structure of volume for melamine and nickel source, if directly being calcined, is be easy to cause
The carbon nanotubes to bond together being prepared then reduces the performance of carbon nanotubes.Therefore obtained powder is dried
It is dry so that powder particle is uniform, and the carbon bonding between particle and particle, subsequent calcination is then caused to be prepared will not occur
Nanotube has good performance.
S3, calcining；
It will be calcined after melamine and nickel source ball milling in the environment of 800-1200 DEG C.Melamine can be removed using calcining
Amino and double bond on amine then obtain the carbon nanotubes of N doping, and nickel source is also doped in carbon nanotubes in calcination process,
Carbon nanotubes is modified.
Further, calcining be kept the temperature after temperature is risen to 300-400 DEG C 1-1.5 it is small when after, then temperature risen into 800-
When 1200 DEG C of reaction 1-3 are small.300-400 DEG C is warming up to first, is to remove the crystallization water in Nickel dichloride hexahydrate, is avoided crystallizing
Water influences the generation of follow-up carbon nanotubes, meanwhile, melamine carries out preliminary exposition.Using gradient increased temperature can to presoma into
Row preheating, prevents presoma to be heated at high temperature suddenly and causes to react uneven, then influences the generation of carbon nanotubes.Then
Temperature rises to 800-1200 DEG C, the further molecular scission of melamine, and passing through between melamine molecule at such a temperature
Hybridized orbit forms carbon nanotubes, while the molecular link of nickel chloride is also broken, and then nickel is doped in carbon nanotubes.
Further, calcining heating is heated up with the rate of 5-7 DEG C/min, is heated up using above-mentioned rate, Neng Goubao
Card tubular type in-furnace temperature is gradually slowly promoted, and prevents damage of the heating to raw material and mechanical equipment suddenly.
Further, calcining is calcined under the atmosphere of protective gas, and protective gas is the air in drain, is prevented
Only during high-temperature calcination, the oxygen, carbon dioxide isoreactivity substance and melamine or other substances in air are anti-
It answers, then influences the purity and correlated performance of the carbon nanotubes of production.
Further, protective gas is inert gas, is preferably nitrogen or argon gas.
Further, the flow for being passed through protective gas is 500-700sccm.
It can ensure that there is sufficient protective gas in tube furnace using above-mentioned flow, while the stream for passing through protective gas
It is dynamic, also the gases such as ammonia, chlorine or the hydrogen chloride of calcining melamine and nickel chloride generation are taken out of outside tube furnace, are then protected
It demonstrate,proves tubular type furnace pressure to stablize, and can guarantee that carbon nanotubes can be successfully generated.
Furnace cooling obtains final product after reaction.
A kind of doped carbon nanometer pipe that the embodiment of the present invention also provides is carbon source using melamine, in calcination process
In automatically derive the carbon nanotubes of doping nitrogen-atoms and the hexatomic ring with rock-steady structure, be then nickel source reaction further
To the carbon nanotubes of doping nickel, the performance of carbon nanotubes can be further promoted.And the cost of material for preparing the carbon nanotubes it is low,
Operating method letter is answered, is easily achieved industrialization.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment also provides a kind of doped carbon nanometer pipe, by melamine and nickel source with molar ratio 1:1 ratio
It is mixed with to obtain, wherein, nickel source is Nickel dichloride hexahydrate.The phenogram of the doped carbon nanometer pipe of the present embodiment is referring to Fig. 1's
Electron-microscope scanning figure.
The present embodiment also provides a kind of preparation method of doped carbon nanometer pipe：
S1, ball milling；
1.576g melamines and 3.932g nickel sources are proportionally carried out to be mixed to get mixture, then put mixture
Enter and ball milling is carried out in ball mill.When Ball-milling Time is 1 small, rotational speed of ball-mill 300r/min.
S2, drying；
Melamine and nickel source are adsorbed with to the presoma of nickel source after ball milling by being dried to obtain.Dry temperature is
60℃。
S3, calcining；
Mixture is calcined in the environment of 1000 DEG C, specifically, after temperature is risen to 300 DEG C keep the temperature 1 it is small when after, then will
Temperature rise to 1000 DEG C reaction 2 it is small when, wherein, calcining heating be to be heated up with the rate of 5 DEG C/min, and in calcination process with
The flow of 500sccm is passed through nitrogen.Furnace cooling obtains final product after reaction.
Embodiment 2
The present embodiment also provides a kind of doped carbon nanometer pipe, by melamine and nickel source with molar ratio 1:3 ratio
It is mixed with to obtain, wherein, nickel source is Nickel dichloride hexahydrate.
The present embodiment also provides a kind of preparation method of doped carbon nanometer pipe：
S1, ball milling；
1.824g melamines and 7.864g nickel sources are proportionally carried out to be mixed to get mixture, then put mixture
Enter and ball milling is carried out in ball mill.When Ball-milling Time is 1.5 small, rotational speed of ball-mill 400r/min.
S2, drying；
Melamine and nickel source are adsorbed with to the presoma of nickel source after ball milling by being dried to obtain.Dry temperature is
80℃。
S3, calcining；
Mixture is calcined in the environment of 1200 DEG C, specifically, after temperature is risen to 400 DEG C keep the temperature 1.5 it is small when after, then
By temperature rise to 1200 DEG C of reactions 3 it is small when, wherein, calcining heating is heated up with the rate of 7 DEG C/min, and in calcination process
Nitrogen is passed through with the flow of 700sccm.Furnace cooling obtains final product after reaction.
Embodiment 3
The present embodiment also provides a kind of doped carbon nanometer pipe, by melamine and nickel source with molar ratio 1:2 ratio
It is mixed with to obtain.
The present embodiment also provides a kind of preparation method of doped carbon nanometer pipe：
S1, ball milling；
1.576g melamines and 4.728g nickel sources are proportionally carried out to be mixed to get mixture, then put mixture
Enter and ball milling is carried out in ball mill.When Ball-milling Time is 2 small, rotational speed of ball-mill 350r/min.
S2, drying；
Melamine and nickel source are adsorbed with to the presoma of nickel source after ball milling by being dried to obtain.Dry temperature is
70℃。
S3, calcining；
Mixture is calcined in the environment of 800 DEG C, specifically, after temperature is risen to 350 DEG C keep the temperature 1 it is small when after, then will
Temperature rise to 800 DEG C reaction 1 it is small when, wherein, calcining heating be to be heated up with the rate of 6 DEG C/min, and in calcination process with
The flow of 600sccm is passed through nitrogen.Furnace cooling obtains final product after reaction.
In conclusion the doped carbon nanometer pipe that 1-3 of the embodiment of the present invention is provided, is carbon source using melamine, is forging
Burn during automatically derive doping nitrogen-atoms and with rock-steady structure hexatomic ring carbon nanotubes, be then nickel source react into
One step obtains the carbon nanotubes of doping nickel, can further promote the performance of carbon nanotubes.And prepare the raw material of the carbon nanotubes
It is at low cost, operating method is simple answers, is easily achieved industrialization.
Embodiments described above is part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of doped carbon nanometer pipe, which is characterized in that it is by melamine and nickel source with molar ratio 1:The ratio mixing of 1-3
It is prepared, is preferably 1：2-3.
2. doped carbon nanometer pipe according to claim 1, which is characterized in that the nickel source is nickel compound, is preferably chlorine
Change nickel, more preferably Nickel dichloride hexahydrate.
3. a kind of preparation method of doped carbon nanometer pipe described in claim 1, which is characterized in that by melamine and nickel source ball
It is calcined after mill in the environment of 800-1200 DEG C.
4. preparation method according to claim 3, which is characterized in that the ball milling is by the melamine and the nickel
When ball milling 1-2 is small after the mixing of source, the rotating speed of ball milling is 300r/min~400r/min.
5. preparation method according to claim 3, which is characterized in that calcining is kept the temperature after temperature is risen to 300-400 DEG C
After when 1-1.5 is small, then by temperature rise to 800-1200 DEG C reaction 1-3 it is small when.
6. preparation method according to claim 3, which is characterized in that calcining heating is the rate progress with 5-7 DEG C/min
Heating.
7. according to the preparation method described in claim 3-6 any one, which is characterized in that calcining is the atmosphere in protective gas
Under calcined, be passed through protective gas flow be 500-700sccm.
8. preparation method according to claim 7, which is characterized in that the protective gas is inert gas, is preferably nitrogen
Gas or argon gas.
9. preparation method according to claim 3, which is characterized in that the melamine and the nickel source are passed through into ball milling
The presoma of nickel source is adsorbed with by being dried to obtain afterwards.
10. preparation method according to claim 3, which is characterized in that dry temperature is 60-80 DEG C.
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Cited By (4)
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| CN108821249A (en) * | 2018-06-12 | 2018-11-16 | 桑德集团有限公司 | Carbon-nitrogen material and preparation method thereof and lithium sulfur battery anode material and lithium-sulfur cell comprising it |
| CN109252359A (en) * | 2018-08-23 | 2019-01-22 | 天津大学 | A kind of preparation method of solid carbon source in-situ growing carbon nano tube modified carbon fiber reinforced resin base electro-magnetic screen composite material |
| CN110252339A (en) * | 2019-07-30 | 2019-09-20 | 宜兴国际环保城科技发展有限公司 | A kind of composite catalyst for the processing of the biochemical waste water of difficulty containing antibiotic |
| CN110272036A (en) * | 2019-05-13 | 2019-09-24 | 中山大学 | A kind of preparation method of the multi-walled carbon nanotube of magnetisable material doping and its multi-walled carbon nanotube of preparation |
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| CN109252359A (en) * | 2018-08-23 | 2019-01-22 | 天津大学 | A kind of preparation method of solid carbon source in-situ growing carbon nano tube modified carbon fiber reinforced resin base electro-magnetic screen composite material |
| CN110272036A (en) * | 2019-05-13 | 2019-09-24 | 中山大学 | A kind of preparation method of the multi-walled carbon nanotube of magnetisable material doping and its multi-walled carbon nanotube of preparation |
| CN110252339A (en) * | 2019-07-30 | 2019-09-20 | 宜兴国际环保城科技发展有限公司 | A kind of composite catalyst for the processing of the biochemical waste water of difficulty containing antibiotic |
| CN110252339B (en) * | 2019-07-30 | 2022-04-29 | 福泉环保城发展有限公司 | Composite catalyst for antibiotic-containing difficult-to-biochemical wastewater treatment |
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