CN104108703A - Preparation method for nitrogen-doped graphene - Google Patents
Preparation method for nitrogen-doped graphene Download PDFInfo
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- CN104108703A CN104108703A CN201410314717.3A CN201410314717A CN104108703A CN 104108703 A CN104108703 A CN 104108703A CN 201410314717 A CN201410314717 A CN 201410314717A CN 104108703 A CN104108703 A CN 104108703A
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Abstract
The invention discloses a preparation method for nitrogen-doped graphene, which belongs to the technical field of carbon materials. The preparation method comprises the following steps: dispersing hard template montmorillonite in water to form a suspension and adjusting a pH value to 1 to 5; dissolving nitrogen-containing organic micromolecules which are used as a carbon source in the suspension and adding a polymerization initiator to induce polymerization of the carbon source; subjecting a polymerization product to filtering and washing and drying and calcining a filter cake; and removing the hard template by using hydrofluoric acid and carrying out repeated washing by using deionized water so as to obtain the nitrogen-doped graphene. According to the invention, the cheap nitrogen-containing organic micromolecules are used as the carbon source, the parallel structural and the nanometer spatial confinement effect of the hard template are employed, so the nitrogen-doped graphene with few defects and high quality is formed in carbonization of organic matters; and the method has the advantages of simple operation, safety, no toxicity, short reaction time and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene, be specifically related to a kind of nitrating graphene preparation method for ultracapacitor, belong to carbon material technical field.
Background technology
Ultracapacitor claims again electrochemical capacitor, have that capacity is large, power density is high, environmentally safe, have extended cycle life, the advantage such as use temperature wide ranges, have many potential using values in fields such as mobile electronic product, production of renewable energy resources, space system, haulage system.For further improving the energy density of ultracapacitor, people are at continuous research carbon back double layer capacitor material, wish to obtain the carbon material that all has excellent properties aspect these three of specific surface area, specific conductivity and porositys.
Graphene is a kind of individual layer sheet structure novel carbon material being made up of carbon atom, there is large theoretical specific surface area, excellent electron conduction and thermal conductivity, high mechanical strength, meeting the ultracapacitor of high-energy-density and high power density to the requirement of electrode materials, is desirable electrode material for super capacitor.By the doping of nitrogen, not only can change the electronic structure of Graphene, improve electroconductibility and the stability of Graphene, can also in the carbon grid of Graphene, introduce nitrogen atom structure, increase the electrochemical activity site on Graphene surface.The preparation method of nitrating Graphene has chemical Vapor deposition process, ammonia source pyrolysis method, nitrogen plasma discharge method, solvent-thermal method and nitrogenous precursor transformation approach etc. at present, but these methods are had relatively high expectations and complicated operation to Preparation equipment, be difficult to be promoted, and the Graphene making is often reunited seriously, available ratio surperficial little, nitrogen content is lower, the nitrogen-atoms electrochemical activity mixing is also lower, is unfavorable for that it applies as electrode material for super capacitor.
Summary of the invention
The present invention will solve technical problem and be to overcome prior art defect, a kind of simple for process, low production cost is provided and can improves the nitrating graphene preparation method of effective ratio area.
In order to solve the problems of the technologies described above, the preparation method of nitrating Graphene provided by the invention, specifically comprises the following steps:
Step 1, be dispersed in the aqueous solution montmorillonite as hard template, the suspension that to form massfraction be 0.5-1mg/mL, and pH of suspension value is adjusted to 1-5;
Step 2, using nitrogenous organic molecule in suspension described in carbon source adds step 1, after stirring, add initiator, induce nitrogenous organic molecule generation polymerization;
Step 3, the polymerisate precipitation of step 2 gained is carried out to suction filtration, washing and dry, under nitrogen atmosphere, calcine carbonization;
Step 4, the product of step 3 gained is washed with hydrofluoric acid solution, remove hard template, and use deionized water repetitive scrubbing, suction filtration, oven dry, obtain nitrating Graphene.
In the present invention, in described step 1, hard template has parallel-plate structure, and interlamellar spacing should be 1-3nm.
In the present invention, in described step 1, adopt hydrochloric acid to regulate the pH value of suspension.
In the present invention, the nitrogenous organic molecule in described step 2 is any one or a few in aniline, pyrroles and Dopamine HCL.
In the present invention, the montmorillonite mass ratio adding in the nitrogenous organic molecule in described step 2 and step 1 is 1:1-3.
In the present invention, in described step 2, initiator is that concentration is the tris solution of 10mmol/mL or the ammonium persulphate that concentration is 1mol/mL.
In the present invention, the polymerization time in described step 2 should be between 24-72h.
In the present invention, in described step 3, calcination condition is to be warmed up to 900 ° of C with the heat-up rate of 3 ° of C/min, insulation 2h.
In the present invention, in described step 4, the concentration of hydrofluoric acid solution is 30%.
Principle of work of the present invention: intend, by Graphene nitrating, opening band gap and adjusting conduction type, change the electronic structure of Graphene, improve the free carrier density of Graphene, thereby improve electroconductibility and the stability of Graphene.In addition, the confinement effect that the nanometer layer parallel construction of hard template produces, in carbonization process, can there is to introducing in the carbon grid of Graphene the nitrogen-atoms of the sp2 hydridization of high electrochemical activity, and this hard template can stop the stacking of Graphene effectively, improve the effective ratio area of Graphene.
Beneficial effect of the present invention is: (1), the present invention adopt cheap nitrogenous organic molecule as carbon source, utilize parallel construction and the nano-space confinement effect of hard template, make organism in carbonization process, form the nitrating grapheme material that defect is few, quality is high, effective ratio area is large; (2), the grapheme material prepared of the present invention, ensureing the original advantageous property of Graphene simultaneously, carried out a rational step nitrogen doping, when improving electroconductibility, increased electrochemical activity site; (3), compare with the preparation method such as chemical vapour deposition and chemical stripping method, preparation technology of the present invention is simple, mild condition, with low cost, favorable reproducibility, is easy to application.
Brief description of the drawings
Fig. 1 is the synthetic route schematic diagram that the present invention prepares nitrating Graphene;
Fig. 2 is the electron scanning micrograph of the embodiment of the present invention 1 gained nitrating Graphene sample;
Fig. 3 is the transmission electron microscope photo of the embodiment of the present invention 1 gained nitrating Graphene sample;
Fig. 4 is the full spectrogram of x-ray photoelectron power spectrum (a) of the embodiment of the present invention 1 gained nitrating Graphene sample; High resolution N1s x-ray photoelectron power spectrum spectrogram (b);
Fig. 5 is the cyclic voltammetry curve of the embodiment of the present invention 1 gained nitrating Graphene sample;
Fig. 6 is the charging and discharging curve of the embodiment of the present invention 1 gained nitrating Graphene sample.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
embodiment 1
As shown in Figure 1, first, the hard template montmorillonite 2 00mg that has parallel-plate structure, interlamellar spacing and should be 1nm is dispersed in water, the suspension that to form massfraction be 0.5mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100 mg Dopamine HCLs as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:2.After stirring, adding 25ml concentration is the tris solution of 10mmol/mL, induction Dopamine HCL generation polymerization, and polymerization time is 24h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C with the heat-up rate of 3 ° of C/min, insulation 2 h.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
As shown in Figures 2 and 3, nitrating Graphene fold prepared by embodiment 1 is more, and lamella is thinner, provides larger available ratio surface to contact with electrolytic solution.
As shown in Figure 4, the test of x-ray photoelectron power spectrum shows that nitrating Graphene prepared by embodiment 1 contains abundant nitrogen element, and more the existing with the higher pyrroles's type nitrogen of electrochemical activity of nitrogen element.
As shown in Figure 5,6, prepared electrode materials is carried out under different scanning rates to cyclic voltammetry and constant current charge-discharge test result curve.When sweep velocity is increased to 100mV/s from 5mV/s, cyclic voltammetry curve all presents obvious rectangular shape, has shown desirable capacitive characteristics.Charging and discharging curve presents linearity curve in the potential region of-1-0, has perfect capacitance behavior.Can be calculated according to discharge curve, its specific storage is 200-300F/g, is better than the electrochemical capacitance performance of the more nitrating grapheme material of having reported.
embodiment 2
First, the hard template montmorillonite 2 00mg that has parallel-plate structure, interlamellar spacing and should be 3nm is dispersed in water, the suspension that to form massfraction be 1mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100mg pyrroles as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:2.After stirring, adding 25ml concentration is the tris solution of 10mmol/mL, and polymerization occurs induction pyrroles, and polymerization time is 24h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C with the heat-up rate of 3 ° of C/min, insulation 2h.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
embodiment 3
First, the hard template montmorillonite 100mg that has parallel-plate structure, interlamellar spacing and should be 2nm is dispersed in water, the suspension that to form massfraction be 1mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100mg Dopamine HCL as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:1.After stirring, adding 25ml concentration is the tris solution of 10mmol/mL, induction Dopamine HCL generation polymerization, and polymerization time is 24h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C with the heat-up rate of 3 ° of C/min and be incubated 2 h.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
embodiment 4
First, the hard template montmorillonite 2 00mg that has parallel-plate structure, interlamellar spacing and should be 3nm is dispersed in water, the suspension that to form massfraction be 1mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100mg Dopamine HCL as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:2.After stirring, adding 25ml concentration is the tris solution of 10mmol/mL, induction Dopamine HCL generation polymerization, polymerization time 48h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C with the heat-up rate of 3 ° of C/min, insulation 2 h.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
embodiment 5
First, the hard template montmorillonite 2 00mg that has parallel-plate structure, interlamellar spacing and should be 1nm is dispersed in water, the suspension that to form massfraction be 1mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100mg aniline as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:2.After stirring, adding 30ml concentration is the ammonium persulphate of 1mol/mL, induction aniline generation polymerization, and polymerization time is 24h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C with the heat-up rate of 3 ° of C/min and be incubated 2 h.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
embodiment 6
First, the hard template montmorillonite 300mg that has parallel-plate structure, interlamellar spacing and should be 1nm is dispersed in water, the suspension that to form massfraction be 0.8mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add Dopamine HCL, each 50 mg of aniline as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:3.After stirring, adding 30ml concentration is the ammonium persulphate of 1mol/mL, induction Dopamine HCL, aniline generation polymerization, and polymerization time is 72h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C insulation 2h with the heat-up rate of 3 ° of C/min.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
embodiment 7
First, the hard template montmorillonite 100mg that has parallel-plate structure, interlamellar spacing and should be 3nm is dispersed in water, the suspension that to form massfraction be 1mg/mL, and add wherein certain hydrochloric acid, regulating its pH value is 1-5.Then, add 100mg Dopamine HCL, aniline and pyrroles's mixture as carbon source, make the mass ratio m of itself and montmorillonite
carbon source/ m
montmorillonite=1:1.After stirring, adding 25ml concentration is the tris solution of 10mmol/mL, induction carbon source generation polymerization, and polymerization time is 56h.The polymerisate precipitation of gained is carried out to suction filtration, washing and dry, in tube furnace, calcine carbonization, under nitrogen atmosphere, be raised to 900 ° of C insulation 2h with the heat-up rate of 3 ° of C/min.The hydrofluoric acid solution that is 30% by concentration by calcinate washing, removes hard template, and uses deionized water repetitive scrubbing, and suction filtration, oven dry, obtain high-quality nitrating Graphene.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, can also make under the premise without departing from the principles of the invention some improvement, and these improve and also should be considered as protection scope of the present invention.
Claims (9)
1. a preparation method for nitrating Graphene, is characterized in that comprising the steps:
Step 1, be dispersed in the aqueous solution montmorillonite as hard template, the suspension that to form massfraction be 0.5-1mg/mL, and pH of suspension value is adjusted to 1-5;
Step 2, using nitrogenous organic molecule in suspension described in carbon source adds step 1, after stirring, add initiator, induce nitrogenous organic molecule generation polymerization;
Step 3, the polymerisate precipitation of step 2 gained is carried out to suction filtration, washing and dry, under nitrogen atmosphere, calcine carbonization;
Step 4, the product of step 3 gained is washed with hydrofluoric acid solution, remove hard template, and use deionized water repetitive scrubbing, suction filtration, oven dry, obtain nitrating Graphene.
2. the preparation method of nitrating Graphene according to claim 1, is characterized in that: in described step 1, hard template has parallel-plate structure, and interlamellar spacing should be 1-3nm.
3. the preparation method of nitrating Graphene according to claim 2, is characterized in that: in described step 1, adopt hydrochloric acid to regulate the pH value of suspension.
4. the preparation method of nitrating Graphene according to claim 3, is characterized in that: the nitrogenous organic molecule in described step 2 is any one or a few in aniline, pyrroles and Dopamine HCL.
5. the preparation method of nitrating Graphene according to claim 4, is characterized in that: the montmorillonite mass ratio adding in the nitrogenous organic molecule in described step 2 and step 1 is 1:1-3.
6. the preparation method of nitrating Graphene according to claim 5, is characterized in that: in described step 2, initiator is that concentration is the tris solution of 10mmol/mL or the ammonium persulphate that concentration is 1mol/mL.
7. the preparation method of nitrating Graphene according to claim 6, is characterized in that: the polymerization time in described step 2 should be between 24-72h.
8. according to the preparation method of the nitrating Graphene described in claim 1 to 7 any one, it is characterized in that: in described step 3, calcination condition is to be warmed up to 900 ° of C with the heat-up rate of 3 ° of C/min insulation 2h.
9. the preparation method of nitrating Graphene according to claim 8, is characterized in that: in described step 4, the concentration of hydrofluoric acid solution is 30%.
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Cited By (10)
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| CN104817062A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen-doped graphene |
| CN104843693A (en) * | 2015-05-07 | 2015-08-19 | 常州大学 | Preparation method of N-doped graphene sheet |
| CN105529472A (en) * | 2015-12-09 | 2016-04-27 | 武汉理工大学 | Co-N double-doped flaky porous two-dimensional carbon material and preparation method thereof |
| CN105668552A (en) * | 2014-12-08 | 2016-06-15 | 中国科学院成都有机化学有限公司 | Preparation method of easy-to-disperse nitrogen-doped graphene powder |
| CN105702473A (en) * | 2014-11-26 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Carbon-based electrode material having super high specific capacitance and combined electrode material thereof |
| CN106882793A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of synthetic method of sulphur and nitrogen co-doped Graphene |
| CN106960729A (en) * | 2017-01-25 | 2017-07-18 | 广西大学 | A kind of preparation method of nitrogen sulphur codope carbon material |
| CN107381543A (en) * | 2016-05-17 | 2017-11-24 | 中国科学院大连化学物理研究所 | A kind of synthetic method of transient metal doped graphene |
| CN109265746A (en) * | 2018-09-14 | 2019-01-25 | 蚌埠创特新材料科技有限公司 | It is a kind of for improving the preparation method of the compounded mix of plastics shock resistance |
| CN109403131A (en) * | 2018-09-29 | 2019-03-01 | 青岛科技大学 | A kind of preparation method of AKD lotion |
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| CN105702473A (en) * | 2014-11-26 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Carbon-based electrode material having super high specific capacitance and combined electrode material thereof |
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| CN105668552A (en) * | 2014-12-08 | 2016-06-15 | 中国科学院成都有机化学有限公司 | Preparation method of easy-to-disperse nitrogen-doped graphene powder |
| CN104843693A (en) * | 2015-05-07 | 2015-08-19 | 常州大学 | Preparation method of N-doped graphene sheet |
| CN104817062A (en) * | 2015-05-07 | 2015-08-05 | 常州大学 | Preparation method of two-dimension nitrogen-doped graphene |
| CN105529472B (en) * | 2015-12-09 | 2019-03-08 | 武汉理工大学 | Flake porous two-dimentional carbon material of a kind of Co-N codope and preparation method thereof |
| CN105529472A (en) * | 2015-12-09 | 2016-04-27 | 武汉理工大学 | Co-N double-doped flaky porous two-dimensional carbon material and preparation method thereof |
| CN106882793A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of synthetic method of sulphur and nitrogen co-doped Graphene |
| CN107381543A (en) * | 2016-05-17 | 2017-11-24 | 中国科学院大连化学物理研究所 | A kind of synthetic method of transient metal doped graphene |
| CN106960729A (en) * | 2017-01-25 | 2017-07-18 | 广西大学 | A kind of preparation method of nitrogen sulphur codope carbon material |
| CN109265746A (en) * | 2018-09-14 | 2019-01-25 | 蚌埠创特新材料科技有限公司 | It is a kind of for improving the preparation method of the compounded mix of plastics shock resistance |
| CN109403131A (en) * | 2018-09-29 | 2019-03-01 | 青岛科技大学 | A kind of preparation method of AKD lotion |
| CN109403131B (en) * | 2018-09-29 | 2021-11-02 | 青岛科技大学 | Preparation method of AKD emulsion |
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Application publication date: 20141022 |