CN106904595A - A kind of preparation method of the hollow carbon nanomaterial of nitrating - Google Patents
A kind of preparation method of the hollow carbon nanomaterial of nitrating Download PDFInfo
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- CN106904595A CN106904595A CN201710165880.1A CN201710165880A CN106904595A CN 106904595 A CN106904595 A CN 106904595A CN 201710165880 A CN201710165880 A CN 201710165880A CN 106904595 A CN106904595 A CN 106904595A
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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Abstract
The invention discloses a kind of preparation method of the hollow carbon nanomaterial of nitrating, including：Take different amounts of photoacoustic spectroscopy and be laid in porcelain boat bottom; then the photoacoustic spectroscopy and ZnO nano material that porcelain boat bottom will be laid in are placed in tube furnace; both are made to keep certain distance; under inertia or reducing atmosphere protection, heating TATB makes it by obtaining the hollow carbon nanomaterial of nitrating after the reactions such as distillation, pyrolysis, carbonization.The present invention prepares required carbon source with nitrogen content organic molecule TATB substitution tradition high, only needs a kind of material just can settle the hollow carbon nanomaterial of prepared nitrating at one go, and without additionally introducing nitrogen source, template need not use acid corrosion.
Description
Technical field
The invention belongs to the preparing technical field of nano material, it is related to a kind of preparation method of hollow carbon nanomaterial, has
Body is related to a kind of preparation method of the hollow carbon nanomaterial of nitrating.
Background technology
Recent years, nitrating carbon nanomaterial has caused the concern of domestic and international many scientific research persons.Wherein hollow nitrating
Carbon nanomaterial (NHC) is especially prominent.NHC not only has big specific surface area, electrical conductivity and good chemical stability high
The advantages of, while the introducing of nitrogen-atoms causes that the electric conductivity and chemism of hollow carbon material become controllable.
At present prepare the hollow carbon nanomaterial of nitrating (such as the hollow carbon balls of nitrating, the hollow carbon nano-particle of nitrating, mix
The hollow CNT of nitrogen, carbon paste capsule of nitrating etc.) method mainly include soft template method and hard template method.Soft template method is main
Refer to generating nitrating carbon precursor by self assembly of organic molecules preparing.Soft template used in the method can pass through
Direct carbonization is removed, and has certain advantage in terms of pattern is controlled, but when the diameter of the hollow carbon material of nitrating is less than 100nm
When its pattern and size be difficult control.Because the core template of very little be easy to reunite so that influence prepare product size and
Pattern.Hard template method is generally referred to be polymerized by solution surface or the carbon precursor of nitrating is coated on into thing by CVD
In the hard template for first designing, by carbonization, prepared by etching template.Comparatively, hard template method is than soft template method advantageously.
First, the hollow nitrating carbon material that prepared by hard template method is homogeneous, good dispersion.Secondly, the method can be by selecting different moulds
Plate controls NHC sizes, inner space and the structure of shell with regulation and control experiment condition.But, currently used hard template method is still
Come with some shortcomings.From for preparation method, for solution polymerization process, it is necessary to strictly control reaction condition or surface modification are hard
Template can just make presoma (aniline, formaldehyde resin, dopamine etc.) be evenly coated at template surface.If dopamine is only in PH=
SiO can be just evenly coated under 8.5 reaction condition2In template.Polyaniline only has in advance polystyrene (PS) template sulfonation
Treatment homogeneous could be coated on PS balls.For CVD, yield poorly.In addition, hard template method also needs to use HCl or HF
Removing template is removed so that complex steps, take, pollute environment.The above these shortcoming significantly limit the hollow carbon material of nitrating
Extensive use.
The content of the invention
The invention aims to overcome above-mentioned the deficiencies in the prior art, there is provided one kind has nitrogen content high,
Morphology controllable, the preparation method of the hollow carbon nanomaterial of nitrating the advantages of without subsequently removing removing template.
Technical scheme is as follows：
A kind of preparation method of the hollow carbon nanomaterial of nitrating, is using ZnO nano material as from template is sacrificed, with three ammonia
Base trinitrobenzen (TATB) is prepared as sole carbon source and nitrogen source using chemical vapour deposition technique, specifically includes following steps：
Take TATB and be laid in porcelain boat bottom, the TATB and ZnO nano material that will then be laid in porcelain boat bottom are placed in tubular type
In stove, both are made to keep certain distance, under inertia or reducing atmosphere protection, heating TATB makes it by distillation, pyrolysis, carbon
The hollow carbon nanomaterial of nitrating is obtained after changing reaction.
Further scheme is：The pattern of the hollow carbon nanomaterial of nitrating is determined by ZnO nano material template.
Further scheme is：The mass ratio of the TATB and ZnO nano material template>10.Typically in experiment, choosing
The quality for selecting TATB can be 0.05~1g, but according to experiment or implementation condition, can suitably adjust the consumption of TATB, its
Effect can be expected.
Further scheme is：The pattern of the ZnO nano material template can be nano wire, nanotube, nanosphere,
The various patterns such as nanobelt.ZnO nano material template can be carried in substrate, or is existed with powder morphology.
Further scheme is：The substrate is nickel foam, carbon fiber or carbon cloth.
Further scheme is：The ZnO nano material template keeps certain distance to refer to ZnO nano material with TATB
Material template is placed in no more than 5cm directly over TATB, or is placed in along protection gas airflow direction apart from TATB downstreams no more than 15cm.
Further scheme is：The heating TATB refers to heating rate<10 DEG C/min, reaction temperature>500 DEG C, reach
Reaction temperature time 1h is kept after reaction temperature.
Another object of the present invention is claimed according to the preparation of the preparation method of foregoing nitrating hollow carbon nanomaterial
The hollow carbon nanomaterial of nitrating for obtaining.
The hollow carbon nanomaterial of nitrating has the property that：Pattern is unified, and nitrogen content is high, the species of nitrogen (pyridine nitrogen,
Pyrroles's nitrogen, graphite nitrogen) can be adjusted by controlling reaction temperature.Temperature is different, and the three kinds of ratios of nitrogen for obtaining are just different.
The present invention compared with prior art, has the advantages that：The present invention is with nitrogen content organic molecule high
TATB substitution tradition prepares required carbon source, only needs a kind of material just can settle the hollow carbon nanomaterial of prepared nitrating, nothing at one go
Nitrogen source need to be additionally introduced.It is lower boiling Zn because ZnO is decomposed the H radical reductions for producing by TATB, it is during the course of the reaction
Volatilization, therefore template need not use acid corrosion.
The hollow carbon nanomaterial of nitrating prepared due to the present invention can growth in situ on electrode material, therefore show excellent
Chemical property, such as high rate performance high, excellent cyclical stability, and big face capacitance.
Brief description of the drawings
Fig. 1 is the obtained Flied emission scanning for being grown in the ZnO nano-rod array in foam nickel base of the embodiment of the present invention 1
Electromicroscopic photograph.
Fig. 2 is the obtained field for being grown in the nitrating hollow carbon nanometer stick array in foam nickel base of the embodiment of the present invention 1
Transmitting stereoscan photograph.
Fig. 3 is the transmission electron microscope photo of nitrating hollow carbon nanometer stick array obtained in the embodiment of the present invention 1.
Fig. 4 is the XPS spectrum figure of the N1s of nitrating hollow carbon nanometer stick array obtained in the embodiment of the present invention 1.
Fig. 5 is with the obtained low power for being grown in the nitrating hollow carbon nanometer stick array in the carbon cloth substrate hair of embodiment 2
Penetrate stereoscan photograph.
Fig. 6 is with the obtained high power for being grown in the nitrating hollow carbon nanometer stick array in the carbon cloth substrate hair of embodiment 2
Penetrate stereoscan photograph.
Fig. 7 is the field emission scanning electron microscope photo of the hollow carbon nano rod of nitrating powdered obtained in the embodiment of the present invention 5.
Specific embodiment
With reference to embodiments of the invention and accompanying drawing, the invention will be further elaborated.
Embodiment 1
A kind of preparation method of the hollow carbon nanomaterial of nitrating, including：
(1) foam nickel base is successively placed in acetone, ethanol and distilled water and is cleaned.Then it is immersed in 5mmol
L-1Zinc nitrate ethanol solution in 10min, in 100 DEG C of rapid draings after taking-up, repeat 3~5 times.Finally substrate by atmosphere
350 DEG C of holding 30min are heated to, zinc nitrate are decomposed and ZnO Seed Layers is obtained；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquors is slow
Instill wherein, it is to be mixed it is uniform after the substrate that obtained length in step (1) has ZnO Seed Layers is vertically put into reactor.Most
Reactor is placed in baking oven afterwards, 6h is reacted at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.20g photoacoustic spectroscopies (TATB) are taken and is laid in porcelain boat bottom, then have length prepared by step (2)
The foam nickel base of ZnO nano-rod array is placed at the 2.5cm of TATB tops, and both are placed at into nitrogen and hydrogen mixed gas guarantor
In shield pipe type stove.The nitrating hollow carbon being grown in foam nickel base is obtained after being raised to 750 DEG C of insulation 1h with 3 DEG C/min speed
Nanometer stick array.
Embodiment 2
A kind of preparation method of the hollow carbon nanomaterial of nitrating, including：
(1) carbon cloth substrate is successively placed in acetone, ethanol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min, in 100 DEG C of rapid draings after taking-up, repeat 3~5 times.Finally substrate is added in atmosphere
Heat decomposes zinc nitrate and ZnO Seed Layers is obtained to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquors is slow
Instill wherein, it is to be mixed it is uniform after the substrate that obtained length in step (1) has ZnO Seed Layers is vertically put into reactor.Most
Reactor is placed in baking oven afterwards, 6h is reacted at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.25g photoacoustic spectroscopies (TATB) are taken and is laid in porcelain boat bottom, then have length prepared by step (2)
The carbon cloth substrate of ZnO nano-rod array is placed at the 2.5cm of TATB tops, and both are placed at into nitrogen and hydrogen mixed gas protection
Under tube furnace in.The prepared nitrating hollow carbon being grown in carbon cloth substrate is received after being raised to 750 DEG C of insulation 1h with 3 DEG C/min speed
Rice rod array.
Embodiment 3
A kind of preparation method of the hollow carbon nanomaterial of nitrating, including：
(1) carbon cloth substrate is successively placed in acetone, ethanol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min, in 100 DEG C of rapid draings after taking-up, repeat 3~5 times.Finally substrate is added in atmosphere
Heat decomposes zinc nitrate and ZnO Seed Layers is obtained to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquors is slow
Instill wherein, it is to be mixed it is uniform after the carbon cloth substrate that obtained length in step (1) has ZnO Seed Layers is vertically put into reactor
In.Finally reactor is placed in baking oven, 6h is reacted at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.25g photoacoustic spectroscopies (TATB) are taken and is laid in porcelain boat bottom, then prepare itself and step (2)
Length have ZnO nano-rod array carbon cloth substrate be placed in tube furnace (ZnO be placed in along protection gas airflow direction apart from TATB downstreams
At 10cm).Under nitrogen and hydrogen mixed gas protection, 750 DEG C are raised to 3 DEG C/min speed, are obtained after insulation 1h and are grown in carbon
Nitrating hollow carbon nanometer stick array in cloth substrate.
Embodiment 4
A kind of preparation method of the hollow carbon nanomaterial of nitrating, including：
(1) carbon cloth substrate is successively placed in acetone, ethanol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min, in 100 DEG C of rapid draings after taking-up, repeat 3~5 times.Finally substrate is added in atmosphere
Heat decomposes zinc nitrate and ZnO Seed Layers is obtained to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquors is slow
Instill wherein, it is to be mixed it is uniform after the carbon cloth substrate that obtained length in step (1) has ZnO Seed Layers is vertically put into reactor
In.Finally reactor is placed in baking oven, 6h is reacted at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.25g photoacoustic spectroscopies (TATB) are taken and is laid in porcelain boat bottom, then have length prepared by step (2)
The carbon cloth substrate of ZnO nano-rod array is placed at the 2.5cm of TATB tops.And both are placed at nitrogen and hydrogen mixed gas protection
Under tube furnace in.The nitrating hollow carbon being grown in carbon cloth substrate is obtained after being raised to 1000 DEG C of insulation 1h with 3 DEG C/min speed
Nanometer stick array.
Embodiment 5
A kind of preparation method of the hollow carbon nanomaterial of nitrating, including：
(1) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquors is slow
Instill wherein, it is to be mixed it is uniform after reactor is placed in baking oven, react 6h at 90 DEG C, washed after react and be dried to obtain powder
Shape ZnO nanorod；
(2) 0.25g photoacoustic spectroscopies (TATB) are taken and is laid in porcelain boat bottom, then prepare porcelain boat and step (1)
Powdered ZnO nanorod be placed in tube furnace (ZnO be placed in along protection gas airflow direction at the 5cm of TATB downstreams).
Under nitrogen and hydrogen mixed gas protection, 1000 DEG C are raised to 5 DEG C/min speed, powdered nitrating hollow carbon is obtained after insulation 1h
Nanometer rods.
The present invention is further illustrated below in conjunction with the accompanying drawings.As shown in Figure 1, it can be seen that obtained in embodiment 1
The ZnO nano-rod array template being grown in foam nickel base is presented hexagon looks；From accompanying drawing 2 as can be seen that embodiment 1 is made
The standby nitrating hollow carbon nanometer stick array for obtaining substantially maintains the pattern of ZnO templates；From accompanying drawing 3 as can be seen that embodiment 1
The nitrating carbon nano rod array of preparation is hollow structure, and wall thickness is about 20nm；From accompanying drawing 4 as can be seen that nitrating hollow carbon nanometer
Rod array contains three kinds of nitrogen, respectively pyridine nitrogen, pyrroles's nitrogen, graphite nitrogen.
From accompanying drawing 5 as can be seen that the nitrating hollow carbon nanometer stick array that embodiment 2 is prepared uniformly is grown in carbon fibre
In dimension；From accompanying drawing 6 as can be seen that nitrating carbon nano rod array is hollow structure.
From accompanying drawing 7 as can be seen that nitrating carbon nano rod powdered obtained in the embodiment of the present invention 5 is hollow structure.
Further, the hollow carbon nanomaterial of nitrating for the embodiment of the present invention 1 being prepared is used to make electrode material.
The electrode material of preparation (2000mV/s) under sweep speed high, scan round curve still can remain close to rectangle, explanation
High rate performance high；After circulation 20000 times, capacitance has only dropped 6.8%, illustrates excellent cyclical stability；In sweep speed
It is 5mV/s, face capacitance is up to 54.2mF/cm2。
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferably implementation method, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and implementation methods, and these modifications and implementation method will fall in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. the preparation method of the hollow carbon nanomaterial of a kind of nitrating, it is characterised in that using ZnO nano material as from sacrificing template,
Using TATB as sole carbon source and nitrogen source, prepared using chemical vapour deposition technique, specifically include following steps：
Take TATB and be laid in porcelain boat bottom, the TATB and ZnO nano material that will then be laid in porcelain boat bottom are placed in tube furnace,
Both are made to keep certain distance, under inertia or reducing atmosphere protection, heating TATB makes it anti-by distillation, pyrolysis, carbonization
Should after obtain the hollow carbon nanomaterial of nitrating.
2. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 1, it is characterised in that nitrating hollow carbon is received
The pattern of rice material is determined by ZnO nano material template.
3. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 1, it is characterised in that：The TATB and
The mass ratio of ZnO nano material template>10.
4. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 1, it is characterised in that：The ZnO nano
Material load exists in substrate, or with powder morphology.
5. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 4, it is characterised in that：The substrate is bubble
Foam nickel, carbon fiber or carbon cloth.
6. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 1, it is characterised in that：The ZnO nano
Material pattern keeps certain distance to refer to ZnO nano material template and is placed in TATB surfaces no more than 5cm with TATB, or is placed in
Along protection gas airflow direction 15cm is no more than apart from TATB downstreams.
7. the preparation method of the hollow carbon nanomaterial of nitrating according to claim 1, it is characterised in that：The heating TATB
Refer to heating rate<10 DEG C/min, reaction temperature>500 DEG C, kept for reaction temperature time 1h after reaching reaction temperature.
8. the preparation method of the hollow carbon nanomaterial of nitrating described in any one of claim 1~7 claim is prepared
The hollow carbon nanomaterial of nitrating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109267326A (en) * | 2018-07-20 | 2019-01-25 | 华中科技大学 | Multi-element doping carbon nano pipe array modifying carbon fibers and the preparation method and application thereof |
| CN110721723A (en) * | 2019-10-29 | 2020-01-24 | 中国工程物理研究院化工材料研究所 | Interpenetrating network structure conductive carbon-based alloy material and preparation method thereof |
| CN112509823A (en) * | 2020-12-22 | 2021-03-16 | 上海第二工业大学 | Hollow carbon microsphere supercapacitor electrode material and solvent-free preparation method thereof |
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