CN109369185A - A kind of preparation method of nitrogen-doped graphene complex carbon material - Google Patents
A kind of preparation method of nitrogen-doped graphene complex carbon material Download PDFInfo
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- CN109369185A CN109369185A CN201811124816.XA CN201811124816A CN109369185A CN 109369185 A CN109369185 A CN 109369185A CN 201811124816 A CN201811124816 A CN 201811124816A CN 109369185 A CN109369185 A CN 109369185A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The present invention relates to a kind of preparation method of nitrogen-doped graphene complex carbon material, this method includes the following steps: with nitrogen source material to grind graphene oxide by a certain percentage, and corresponding solvent is added, carries out ultrasonic disperse processing to it；Then electric spinning polymer is added, magnetic agitation is carried out at 40-80 DEG C, prepares nitrogen-doped graphene compound precursor liquid solution；Afterwards by electrostatic spinning apparatus, spinning operation is carried out to it；Finally, spun tunica fibrosa is placed in tube furnace, be first warming up to 200-300 DEG C, pre-oxidized, after be warming up to 400-1900 DEG C while being passed through protection gas and calcined, finally obtain nitrogen-doped graphene complex carbon material.The present invention has the advantages that the nitrogen-doped graphene complex carbon material nitrogen content with higher that the present invention prepares, while there is composite fibre web frame and preferable electric conductivity.
Description
Technical field
The present invention relates to a kind of synthetic material, in particular to a kind of preparation method of nitrogen-doped graphene complex carbon material.
Background technique
Graphene can generate Hall effect and abnormal half-integer quantum suddenly due to carrier mobility with higher
Therefore you have excellent electric property at effect.Meanwhile the lattice structure of graphene is highly stable, electronics moves in orbit
Suffered interference is very small, has outstanding electric conductivity.But graphene there are chemical stabilities it is higher, not hydrophilic and its
The interaction of his medium is weak, is easy to produce aggregation, is not easy the problems such as being dispersed into nanoscale twins, is unfavorable for the abundant of its performance
Show.Therefore, the excessively modified method of research multi-pass, introduces functional group, changes the surface nature of graphene, keep graphene better
Using.Wherein nitrogen-atoms and carbon atom have closer size, can relatively easily be embedded into graphene lattice and realize
Doping.
Currently, for realize nitrogen-doped graphene preparation method be broadly divided into directly generate type nitrogen-doped graphene and
Post-processing type nitrogen-doped graphene.The type nitrogen-doped graphene of directly generating mainly includes chemical vapour deposition technique, solvent heat seal
At method and arc discharge synthesis method.Post-processing type nitrogen-doped graphene is broadly divided into heat treatment nitrogen doped graphene, plasma
Body handles nitrogen-doped graphene and photochemical treatment nitrogen-doped graphene.Above method, which not can guarantee nitrogen-doped graphene, to be had
The batch production of effect ground, and arc process etc. is due to needing biggish Hydrogen Vapor Pressure and discharge current, risk higher.And N doping stone
Black alkene catalytic activity with higher and electrochemical stability, have very big potentiality in terms of being used as electro-catalyst carrier.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation process is simple, and the nitrogen-doped graphene of process control
The preparation method of complex carbon material.
In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of system of nitrogen-doped graphene complex carbon material
Preparation Method, innovative point are: the preparation method includes the following steps:
Step S1: graphite oxide and nitrogen source material are subjected to ground and mixed by the mass ratio of 1:3-1:6, corresponding solvent is added and carries out
Ultrasonic disperse, the graphite oxide is graphite through made from peroxidating, the nitrogen source material is nitrogen compound-material, described super
Sound jitter time is 30-50min；
Step S2: being added electrostatic spinning polymer, and magnetic agitation is carried out at 40 DEG C -80 DEG C and is configured to precursor solution, described
The magnetic agitation time is 1-3h；
Step S3: above-mentioned precursor solution is carried out spinning and stands formation by electrostatic spinning technique to consolidate uniform fiber
Film；
Step S4: above-mentioned tunica fibrosa is kept the temperature with the heating rate of 2-6 DEG C/min to 200-300 DEG C, soaking time is
1-3h carries out pre-oxidation treatment；
Step S5: by the tunica fibrosa after above-mentioned pre-oxidation, 400- is warming up to the heating rate of 2-8 DEG C/min under a shielding gas
It 1900 DEG C, is kept the temperature, soaking time 2-4h obtains nitrogen-doped graphene complex carbon material.
Further, the nitrogen source material in the step S1 is melamine, urea, cyanamide, cdicynanmide, biuret, three
The mixture of one or more of chlorethamin, pyridine, pyrroles, acetoxime.
Further, the solvent in the step S1 is dimethylformamide, deionized water, chloroform, tetrahydrofuran, first and second
One of ketone, camphorsulfonic acid.
Further, the electrostatic spinning polymer in the step S2 is polyacrylonitrile, polystyrene, polyaniline/polyoxy
One of mixture of ethylene, polyaniline/polystyrene mixture.
Further, electrostatic spinning procedure parameter is arranged in the step S3: receiving distance is 10-20cm, applies voltage
For 12-35kV, fltting speed 0.001-0.01mm/s, temperature is 30-50 DEG C.
Further, the protection gas in the step S5 is one of helium, argon gas, and gas flow is 100-
300sccm。
The present invention has the advantages that
(1) preparation method of nitrogen-doped graphene complex carbon material provided by the invention utilizes electrostatic spinning combination high temperature sintering
Method prepare nitrogen-doped graphene, entire preparation method simple process, and process control, can effectively prepare have compared with
The nitrogen-doped graphene complex carbon material of good fiber net structure；
(2) nitrogen-doped graphene complex carbon material provided by the invention, having a size of Nano grade, nitrogen content is higher, and conductive
Property is good, energy storage, electro-catalysis, in terms of with good application prospect.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the preparation technology flow chart of nitrogen-doped graphene of the invention.
Fig. 2 is that the SEM of 1 nitrogen-doped graphene of the embodiment of the present invention schemes.
Fig. 3 is 1 nitrogen-doped graphene CV of embodiment of the present invention figure.
Fig. 4 is that the SEM of 2 nitrogen-doped graphene of the embodiment of the present invention schemes.
Fig. 5 is 2 nitrogen-doped graphene CV of embodiment of the present invention figure.
Specific embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
The preparation method of nitrogen-doped graphene complex carbon material of the present invention, as shown in Figure 1, including the following steps:
Step S1: graphite oxide and nitrogen source material are subjected to ground and mixed by the mass ratio of 1:3-1:6, corresponding solvent is added and carries out
Ultrasonic disperse, the graphite oxide is graphite through made from peroxidating, the nitrogen source material is nitrogen compound-material, described super
Sound jitter time is 30-50min；
Step S2: being added electrostatic spinning polymer, and magnetic agitation is carried out at 40 DEG C -80 DEG C and is configured to precursor solution, described
The magnetic agitation time is 1-3h；
Step S3: above-mentioned precursor solution is carried out spinning and stands formation by electrostatic spinning technique to consolidate uniform fiber
Film；
Step S4: above-mentioned tunica fibrosa is kept the temperature with the heating rate of 2-6 DEG C/min to 200-300 DEG C, soaking time is
1-3h carries out pre-oxidation treatment；
Step S5: by the tunica fibrosa after above-mentioned pre-oxidation, 400- is warming up to the heating rate of 2-8 DEG C/min under a shielding gas
It 1900 DEG C, is kept the temperature, soaking time 2-4h obtains nitrogen-doped graphene complex carbon material.
As embodiment, more specifically embodiment are as follows:
Nitrogen source material in step S1 be melamine, urea, cyanamide, cdicynanmide, biuret, trichloro-triethylamine, pyridine, pyrroles,
The mixture of one or more of acetoxime.
Solvent in step S1 is dimethylformamide, in deionized water, chloroform, tetrahydrofuran, methyl ethyl ketone, camphorsulfonic acid
One kind.
Electrostatic spinning polymer in step S2 is polyacrylonitrile, polystyrene, polyaniline/polyoxyethylene mixture, gathers
One of aniline/polystyrene blends.
Electrostatic spinning procedure parameter is arranged in step S3: receiving distance is 10-20cm, and application voltage is 12-35kV, is promoted
Speed is 0.001-0.01mm/s, and temperature is 30-50 DEG C.
Protection gas in step S5 is one of helium, argon gas, and gas flow is 100-300sccm.
Embodiment 1
The preparation method of the present embodiment nitrogen-doped graphene complex carbon material, as shown in Figure 1, including the following steps:
(1) 9g dimethylformamide is added in 0.02g graphite oxide and 0.1g melamine ground and mixed according to mass ratio 1:5,
Ultrasonic disperse 45min obtains grey black suspension.
(2) 0.7g polyacrylonitrile is added in suspension, is placed on magnetic stirring apparatus and continues to stir 2h and guarantee that temperature is
60 DEG C, until all dissolution becomes black sol, obtain spinning precursor solution.
(3) electrostatic spinning apparatus is utilized, the syringe equipped with precursor solution is placed on positive position, keeps and receives
The distance of plate is 17cm, and voltage 18kV, syringe fltting speed is 0.002mm/s, and temperature is 30 DEG C, obtains fiber through spinning
Film.
(4) sheet that the tunica fibrosa spun out is cut to 5cm × 5cm, is placed in tube furnace, with the heating of 4 DEG C/min
Rate is warming up to 250 DEG C, forms yellowish-brown sheet film after keeping the temperature 2h, completes preoxidation process.
(5) tunica fibrosa after pre-oxidation is warming up to 700 DEG C with the heating rate of 4 DEG C/min, keeps the temperature 3h, form black patch
Shape film obtains nitrogen-doped graphene complex carbon material.
Embodiment 2
The preparation method of the present embodiment nitrogen-doped graphene complex carbon material, as shown in Figure 1, including the following steps:
(1) 9g dimethylformamide, ultrasound is added in 0.02g graphite oxide and 0.1g urea ground and mixed according to mass ratio 1:5
Disperse 45min, obtains grey black suspension.
(2) 0.7g polyacrylonitrile is added in suspension, is placed on magnetic stirring apparatus and continues to stir 2h and guarantee that temperature is
60 DEG C, until all dissolution becomes black sol, obtain spinning precursor solution.
(3) electrostatic spinning apparatus is utilized, the syringe equipped with precursor solution is placed on positive position, keeps and receives
The distance of plate is 17cm, and voltage 20kV, syringe fltting speed is 0.004mm/s, and temperature is 30 DEG C, by spinning for 7h
To tunica fibrosa.
(4) sheet that the tunica fibrosa spun out is cut to 5cm × 5cm, is placed in tube furnace, with the heating of 4 DEG C/min
Rate is warming up to 250 DEG C, forms yellowish-brown sheet film after keeping the temperature 2h, completes preoxidation process.
(5) tunica fibrosa after pre-oxidation is warming up to 700 DEG C with the heating rate of 4 DEG C/min, keeps the temperature 3h, form black patch
Shape film obtains nitrogen-doped graphene complex carbon material.
By the preparation method of above-described embodiment 1 and embodiment 2, the nitrogen-doped graphene complex carbon material being prepared is through sweeping
Electronic Speculum observation is retouched, SEM figure such as Fig. 2 and Fig. 4 respectively is obtained, wherein the tunica fibrosa string diameter being prepared through embodiment 1 is distributed in
Between 300-400nm, there is apparent fibrous reticular structure, and fiber is evenly distributed；The tunica fibrosa being prepared through embodiment 2
String diameter is distributed between 200-300nm, and is in reticular structure.Tunica fibrosa element composition, table specific as follows are obtained through energy spectrum analysis
It is shown:
To the tunica fibrosa prepared through Examples 1 and 2, be tested for the property using cyclic voltammetry, test result respectively such as Fig. 3 and
5.Tunica fibrosa prepared by embodiment 1, oxidation peak is about between -0.25-0V, and reduction peak is between 1-1.5, maximum current density
For 3.6mA/cm2；Tunica fibrosa prepared by embodiment 2, oxidation peak is about between -0.5-0V, and reduction peak is between 1-1.5, most
High current density is 13.7mA/cm2。
Comprehensive Experiment analysis result can be seen that the preparation side of nitrogen-doped graphene complex carbon material provided by the invention
Method prepares nitrogen-doped graphene using the method for electrostatic spinning combination high temperature sintering, entire preparation method simple process, and
Process control can prepare the nitrogen-doped graphene complex carbon material for the composite fibre web frame that is evenly distributed；The present invention provides
Nitrogen-doped graphene complex carbon material, having a size of Nano grade, nitrogen content is higher, and good conductivity, urges in energy storage, electricity
Change, sensor etc. are with good application prospect.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (6)
1. a kind of preparation method of nitrogen-doped graphene complex carbon material, it is characterised in that: the preparation method includes following step
It is rapid:
Step S1: graphite oxide and nitrogen source material are subjected to ground and mixed by the mass ratio of 1:3-1:6, corresponding solvent is added and carries out
Ultrasonic disperse, the graphite oxide is graphite through made from peroxidating, the nitrogen source material is nitrogen compound-material, described super
Sound jitter time is 30-50min；
Step S2: being added electrostatic spinning polymer, and magnetic agitation is carried out at 40 DEG C -80 DEG C and is configured to precursor solution, described
The magnetic agitation time is 1-3h；
Step S3: above-mentioned precursor solution is carried out spinning and stands formation by electrostatic spinning technique to consolidate uniform fiber
Film；
Step S4: above-mentioned tunica fibrosa is kept the temperature with the heating rate of 2-6 DEG C/min to 200-300 DEG C, soaking time is
1-3h carries out pre-oxidation treatment；
Step S5: by the tunica fibrosa after above-mentioned pre-oxidation, 400- is warming up to the heating rate of 2-8 DEG C/min under a shielding gas
It 1900 DEG C, is kept the temperature, soaking time 2-4h obtains nitrogen-doped graphene complex carbon material.
2. the preparation method of nitrogen-doped graphene complex carbon material according to claim 1, it is characterised in that: the step
Nitrogen source material in S1 be melamine, urea, cyanamide, cdicynanmide, biuret, trichloro-triethylamine, pyridine, pyrroles, in acetoxime
One or more kinds of mixtures.
3. the preparation method of nitrogen-doped graphene complex carbon material according to claim 1, it is characterised in that: the step
Solvent in S1 is one of dimethylformamide, deionized water, chloroform, tetrahydrofuran, methyl ethyl ketone, camphorsulfonic acid.
4. the preparation method of nitrogen-doped graphene complex carbon material according to claim 1, it is characterised in that: the step
Electrostatic spinning polymer in S2 is polyacrylonitrile, polystyrene, polyaniline/polyoxyethylene mixture, polyaniline/polystyrene
One of mixture.
5. the preparation method of nitrogen-doped graphene complex carbon material according to claim 1, it is characterised in that: the step
Electrostatic spinning procedure parameter is arranged in S3: receiving distance is 10-20cm, and application voltage is 12-35kV, fltting speed 0.001-
0.01mm/s, temperature are 30-50 DEG C.
6. the preparation method of nitrogen-doped graphene complex carbon material according to claim 1, it is characterised in that: the step
Protection gas in S5 is one of helium, argon gas, and gas flow is 100-300sccm.
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| CN112751013A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Nitrogen-doped TiO2/GRA composite material |
| CN113735597A (en) * | 2021-08-23 | 2021-12-03 | 西北工业大学 | Preparation method of polymer conversion ceramic-based wave-absorbing material loaded with nitrogen-doped graphene in situ |
| CN115851271A (en) * | 2023-02-18 | 2023-03-28 | 北京化工大学 | Preparation method of nitrogen-doped fluorescent carbon dots |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
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| CN115851271B (en) * | 2023-02-18 | 2023-05-02 | 北京化工大学 | Preparation method of nitrogen-doped fluorescent carbon dots |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
| CN116575144B (en) * | 2023-07-13 | 2023-09-26 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
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