CN106904595B - 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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- CN106904595B CN106904595B CN201710165880.1A CN201710165880A CN106904595B CN 106904595 B CN106904595 B CN 106904595B CN 201710165880 A CN201710165880 A CN 201710165880A CN 106904595 B CN106904595 B CN 106904595B
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Abstract
The invention discloses a kind of preparation methods of the hollow carbon nanomaterial of nitrating; it include: that different amounts of photoacoustic spectroscopy is taken to be laid in porcelain boat bottom; then the photoacoustic spectroscopy for being laid in porcelain boat bottom and ZnO nano material are placed in tube furnace; the two is set to keep certain distance; under inertia or reducing atmosphere protection, heating TATB makes it obtain the hollow carbon nanomaterial of nitrating after the reaction such as distillation, pyrolysis, carbonization.Carbon source needed for the present invention replaces tradition preparation with the high small organic molecule TATB of nitrogen content, only needs a kind of substance that can settle the hollow carbon nanomaterial of obtained nitrating at one go, and without additionally introducing nitrogen source, template is without using acid corrosion.
Description
Technical field
The invention belongs to the preparation technical fields of nano material, are related to a kind of preparation method of hollow carbon nanomaterial, tool
Body is related to a kind of preparation method of hollow carbon nanomaterial of nitrating.
Background technique
Recent years, nitrating carbon nanomaterial have 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, high conductivity and good chemical stability
The advantages that, while the introducing of nitrogen-atoms is so that the electric conductivity and chemical activity of hollow carbon material become controllable.
Prepare at present the hollow carbon nanomaterial of nitrating (hollow carbon balls of such as nitrating, nitrating hollow carbon nano-particle, mix
The hollow carbon nanotube of nitrogen, carbon paste capsule of nitrating etc.) method mainly include soft template method and hard template method.Soft template method is main
It refers to generating nitrating carbon precursor by self assembly of organic molecules to prepare.Soft template used in this method can pass through
Direct carbonization removal has certain advantage in terms of controlling pattern, but when the diameter of the hollow carbon material of nitrating is less than 100nm
When its pattern and size be difficult to control.This is because the core template of very little is easy to reunite, thus influence prepare product size and
Pattern.Hard template method generally refers to polymerize by solution surface or the carbon precursor of nitrating is coated on thing by CVD method
First in designed hard template, by carbonization, etching template preparation.Comparatively, hard template method is advantageously than soft template method.
Firstly, the hollow nitrating carbon material of hard template method preparation is uniform, good dispersion.Secondly, this method can be by selecting different moulds
Plate and regulation experiment condition control NHC size, inner space and the structure of shell.But currently used hard template method is still
It comes with some shortcomings.For preparation method, for solution polymerization process, need strict control reaction condition or surface modification 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 is only in advance polystyrene (PS) template sulfonation
Processing uniform could be coated on PS ball.For CVD method, low output.In addition to this, hard template method is also needed using HCl or HF
Removing template is gone to make complex steps, time-consuming, pollution environment.These disadvantages described above significantly limit the hollow carbon material of nitrating
Extensive use.
Summary of the invention
The purpose of the invention is to overcome above-mentioned the deficiencies in the prior art, providing one kind has nitrogen content height,
Morphology controllable, the preparation method of the hollow carbon nanomaterial of nitrating without subsequent the advantages that 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 template is sacrificed certainly, with three ammonia
Base trinitrobenzen (TATB) is used as sole carbon source and nitrogen source, is prepared, is specifically comprised the following steps: using chemical vapour deposition technique
It takes TATB to be laid in porcelain boat bottom, the TATB for being laid in porcelain boat bottom and ZnO nano material is then placed in tubular type
In furnace, make the two holding certain distance, under inertia or reducing atmosphere protection, heating TATB makes it by distilling, being pyrolyzed, 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: mass ratio > 10 of the TATB and ZnO nano material template.Generally in experiment, choosing
Select TATB quality can for 0.05~1g, but according to experiment or implementation condition, can with the dosage of appropriate adjustment TATB,
Effect is 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 be 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 and TATB keep certain distance to refer to ZnO nano material
Material template, which is placed in right above TATB, is no more than 5cm, or is placed in and is no more than 15cm along the protection gas airflow direction downstream distance TATB.
Further scheme is: the heating TATB refers to heating rate<10 DEG C/min, and 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 the hollow carbon nanomaterial of aforementioned nitrating
The hollow carbon nanomaterial of obtained nitrating.
The hollow carbon nanomaterial of nitrating has the property that pattern is unified, and nitrogen content is high, the type of nitrogen (pyridine nitrogen,
Pyrroles's nitrogen, graphite nitrogen) it can be adjusted by control reaction temperature.Temperature is different, and the ratio of three kinds of obtained nitrogen is just different.
Compared with the prior art, the present invention has the following beneficial effects: the small organic molecule that the present invention is high with nitrogen content
Carbon source needed for TATB replaces tradition preparation, only needs a kind of substance that can settle the hollow carbon nanomaterial of obtained nitrating, nothing at one go
Nitrogen source need to be additionally introduced.It is low-boiling Zn since ZnO is decomposed the H radical reduction generated by TATB, during the reaction
Volatilization, therefore template is without using acid corrosion.
Due to the hollow carbon nanomaterial of nitrating prepared by the present invention can growth in situ on electrode material, therefore show excellent
Chemical property, such as high high rate performance, excellent cyclical stability and big face capacitance.
Detailed description of the invention
Fig. 1 is the Flied emission scanning for the ZnO nano-rod array being grown in foam nickel base made from the embodiment of the present invention 1
Electromicroscopic photograph.
Fig. 2 is the field for the nitrating hollow carbon nanometer stick array being grown in foam nickel base made from the embodiment of the present invention 1
Emit stereoscan photograph.
Fig. 3 is the transmission electron microscope photo of nitrating hollow carbon nanometer stick array made from the embodiment of the present invention 1.
Fig. 4 is the XPS spectrum figure of the N1s of nitrating hollow carbon nanometer stick array made from the embodiment of the present invention 1.
Fig. 5 is the low power field hair for the nitrating hollow carbon nanometer stick array being grown in carbon cloth substrate made from embodiment 2
Penetrate stereoscan photograph.
Fig. 6 is the high power field hair for the nitrating hollow carbon nanometer stick array being grown in carbon cloth substrate made from embodiment 2
Penetrate stereoscan photograph.
Fig. 7 is the field emission scanning electron microscope photo of the hollow carbon nano rod of nitrating powdered made from the embodiment of the present invention 5.
Specific embodiment
Below with reference to the embodiment of the present invention and attached drawing, the invention will be further elaborated.
Embodiment 1
A kind of preparation method of the hollow carbon nanomaterial of nitrating, comprising:
(1) foam nickel base is successively placed in acetone, ethyl alcohol and distilled water and is cleaned.Then it is immersed in 5mmol
L-1Zinc nitrate ethanol solution in 10min repeated 3~5 times in 100 DEG C of rapid draings after taking-up.Finally in air by substrate
350 DEG C of holding 30min are heated to, zinc nitrate is decomposed and ZnO seed layer is made；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquor is slow
Instill wherein, it is to be mixed uniformly after the substrate obtained in step (1) with ZnO seed layer is vertically put into reaction kettle.Most
Reaction kettle is placed in baking oven afterwards, reacts 6h at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.20g photoacoustic spectroscopy (TATB) is taken to be laid in porcelain boat bottom, then by step (2) preparation with
The foam nickel base of ZnO nano-rod array is placed in above TATB at 2.5cm, and the two is placed at nitrogen and hydrogen mixed gas guarantor
It protects in pipe type furnace.The nitrating hollow carbon being grown in foam nickel base is made after being raised to 750 DEG C of heat preservation 1h with 3 DEG C/min speed
Nanometer stick array.
Embodiment 2
A kind of preparation method of the hollow carbon nanomaterial of nitrating, comprising:
(1) carbon cloth substrate is successively placed in acetone, ethyl alcohol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min repeated 3~5 times in 100 DEG C of rapid draings after taking-up.Finally substrate is added in air
Heat decomposes zinc nitrate and ZnO seed layer is made to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquor is slow
Instill wherein, it is to be mixed uniformly after the substrate obtained in step (1) with ZnO seed layer is vertically put into reaction kettle.Most
Reaction kettle is placed in baking oven afterwards, reacts 6h at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.25g photoacoustic spectroscopy (TATB) is taken to be laid in porcelain boat bottom, then by step (2) preparation with
The carbon cloth substrate of ZnO nano-rod array is placed in above TATB at 2.5cm, and the two is placed at nitrogen and hydrogen mixed gas protection
Under tube furnace in.The obtained nitrating hollow carbon being grown in carbon cloth substrate is received after being raised to 750 DEG C of heat preservation 1h with 3 DEG C/min speed
Rice stick array.
Embodiment 3
A kind of preparation method of the hollow carbon nanomaterial of nitrating, comprising:
(1) carbon cloth substrate is successively placed in acetone, ethyl alcohol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min repeated 3~5 times in 100 DEG C of rapid draings after taking-up.Finally substrate is added in air
Heat decomposes zinc nitrate and ZnO seed layer is made to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquor is slow
Instill wherein, it is to be mixed uniformly after the carbon cloth substrate obtained in step (1) with ZnO seed layer is vertically put into reaction kettle
In.Finally reaction kettle is placed in baking oven, reacts 6h at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) it takes 0.25g photoacoustic spectroscopy (TATB) to be laid in porcelain boat bottom, then prepares itself and step (2)
Carbon cloth substrate with ZnO nano-rod array be placed in tube furnace (ZnO be placed in along protection the downstream gas airflow direction distance TATB
At 10cm).Under nitrogen and hydrogen mixed gas protection, 750 DEG C are raised to 3 DEG C/min speed, is made after heat preservation 1h and is 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, comprising:
(1) carbon cloth substrate is successively placed in acetone, ethyl alcohol and distilled water and is cleaned.Then it is immersed in 5mmolL-1
Zinc nitrate ethanol solution in 10min repeated 3~5 times in 100 DEG C of rapid draings after taking-up.Finally substrate is added in air
Heat decomposes zinc nitrate and ZnO seed layer is made to 350 DEG C of holding 30min；
(2) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquor is slow
Instill wherein, it is to be mixed uniformly after the carbon cloth substrate obtained in step (1) with ZnO seed layer is vertically put into reaction kettle
In.Finally reaction kettle is placed in baking oven, reacts 6h at 90 DEG C, washing is dried to obtain ZnO nano-rod array template after having reacted；
(3) 0.25g photoacoustic spectroscopy (TATB) is taken to be laid in porcelain boat bottom, then by step (2) preparation with
The carbon cloth substrate of ZnO nano-rod array is placed in above TATB at 2.5cm.And the two is placed at nitrogen and hydrogen mixed gas protection
Under tube furnace in.The nitrating hollow carbon being grown in carbon cloth substrate is made after being raised to 1000 DEG C of heat preservation 1h with 3 DEG C/min speed
Nanometer stick array.
Embodiment 5
A kind of preparation method of the hollow carbon nanomaterial of nitrating, comprising:
(1) 30mmolL is prepared in ptfe autoclave-1Zinc nitrate aqueous solution 80mL, 3mL concentrated ammonia liquor is slow
Instill wherein, it is to be mixed uniformly after reaction kettle is placed in baking oven, react 6h at 90 DEG C, react after wash be dried to obtain powder
Shape ZnO nanorod；
(2) it takes 0.25g photoacoustic spectroscopy (TATB) to be laid in porcelain boat bottom, then prepares porcelain boat and step (1)
Powdered ZnO nanorod be placed in tube furnace (ZnO be placed in along protection gas airflow direction distance TATB downstream 5cm at).?
Under nitrogen and hydrogen mixed gas protection, 1000 DEG C are raised to 5 DEG C/min speed, powdered nitrating hollow carbon is made after keeping the temperature 1h
Nanometer rods.
The present invention will be further described below with reference to the drawings.As shown in Fig. 1, it can be seen that made from embodiment 1
Hexagonal prisms pattern is presented in the ZnO nano-rod array template being grown in foam nickel base；From attached drawing 2 as can be seen that embodiment 1 is made
Standby obtained nitrating hollow carbon nanometer stick array substantially maintains the pattern of ZnO template；From attached 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 attached drawing 4 as can be seen that nitrating hollow carbon nanometer
Stick array is containing there are three types of nitrogen, respectively pyridine nitrogen, pyrroles's nitrogen, graphite nitrogen.
From attached drawing 5 as can be seen that the nitrating hollow carbon nanometer stick array that embodiment 2 is prepared uniformly is grown in carbon fiber
In dimension；From attached drawing 6 as can be seen that nitrating carbon nano rod array is hollow structure.
From attached drawing 7 as can be seen that nitrating carbon nano rod powdered made from the embodiment of the present invention 5 is hollow structure.
Further, it is used for the hollow carbon nanomaterial of nitrating that the embodiment of the present invention 1 is prepared to make electrode material.
The electrode material of preparation (2000mV/s) under high sweep speed, scan round curve still can be kept close to rectangle, explanation
High high rate performance；After circulation 20000 times, capacitance has only dropped 6.8%, illustrates excellent cyclical stability；In scanning speed
For 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 preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (7)
1. a kind of preparation method of the hollow carbon nanomaterial of nitrating, it is characterised in that using ZnO nano material as sacrifice template certainly,
It using TATB as sole carbon source and nitrogen source, is prepared, is specifically comprised the following steps: using chemical vapour deposition technique
It takes TATB to be laid in porcelain boat bottom, then the TATB for being laid in porcelain boat bottom and ZnO nano material is placed in tube furnace,
The two is set to keep certain distance, in the case where inertia or reducing atmosphere are protected, heating TATB makes it by distilling, pyrolysis, is carbonized instead
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
Mass ratio > 10 of ZnO nano material template.
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 and TATB keep certain distance to refer to that ZnO nano material template is placed in no more than 5cm right above TATB, or are placed in
It is no more than 15cm along the protection gas airflow direction downstream distance TATB.
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 keep reaction temperature time 1h after reaching reaction temperature.
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| CN110721723B (en) * | 2019-10-29 | 2022-05-03 | 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 |
| CN112509823B (en) * | 2020-12-22 | 2022-02-15 | 上海第二工业大学 | Hollow carbon microsphere supercapacitor electrode material and solvent-free preparation method thereof |
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