CN103833021A - Nitrogen-doped graphene nanobelt and preparation method thereof - Google Patents
Nitrogen-doped graphene nanobelt and preparation method thereof Download PDFInfo
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- CN103833021A CN103833021A CN201210490926.4A CN201210490926A CN103833021A CN 103833021 A CN103833021 A CN 103833021A CN 201210490926 A CN201210490926 A CN 201210490926A CN 103833021 A CN103833021 A CN 103833021A
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Abstract
The invention relates to a nitrogen-doped graphene nanobelt and a preparation method thereof. The preparation method comprises the following steps: preparing a carbon oxide nano wall slurry; and preparing the nitrogen-doped graphene nanobelt. In the nitrogen-doped graphene nanobelt preparation process, a technique of mixing the nitrogen source and carbon oxide nano wall by a liquid phase is utilized, so that the nitrogen-doped graphene nanobelt has the advantages of better doping effect and favorable uniformity; and the ionic liquid used as the solvent can effectively prevent the graphene nanobelt from reaggregation, so that the preparation process can be completed through simple separation and drying.
Description
Technical field
The present invention relates to the synthetic field of chemical material, relate in particular to a kind of nitrogen-doped graphene nano belt and preparation method thereof.
Background technology
The kind of carbon material comprises the soccerballene (C of zero dimension
60deng), carbon nanotube, the carbon nanofiber etc. of one dimension, the Graphene of two dimension, three-dimensional graphite, diamond etc.Carbon nanometer wall (english abbreviation CNW) is the carbon nano structure with two-dimensional diffusion structure, its most typical shape characteristic can be grown perpendicular to substrate material surface exactly, and for thickness is greater than the wall shape structure of Graphene, they are completely different from the feature of soccerballene, carbon nanotube, Graphene etc., can be used as the raw material of other carbon material of preparation.
Graphene nanobelt not only has the performance of Graphene, also possesses some special performances, and for example its length-to-diameter ratio is very large, can be up to thousands of times, can replace copper conductor at integrated circuit connection, further to improve integrated level, also can carry out modification to its structure and be prepared into switch device.But at present due to the problem that has size control difficulty in graphene nanobelt preparation process, yields poorly, thereby limit its application.
Summary of the invention
Goal of the invention of the present invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of nitrogen-doped graphene nano belt and preparation method thereof is provided, adopt liquid-phase mixing nitrogenous source and carbonoxide nanometer wall technique, the nitrogen-doped graphene nano belt doping effect that makes to obtain is better, have good uniformity, and adopt ionic liquid to make solvent effectively to prevent that graphene nanobelt from reuniting again.
For reaching goal of the invention of the present invention, the technical solution used in the present invention is: a kind of preparation method of nitrogen-doped graphene nano belt, comprise the steps: that (a) prepares carbonoxide nanometer wall slurry: get carbon nanometer wall and join in the vitriol oil, add potassium permanganate and stir, add again deionized water to carry out suction filtration, wash with hydrochloric acid afterwards, suction filtration is neutral to filtrate, obtains carbonoxide nanometer wall slurry.
(b) prepare nitrogen-doped graphene nano belt: by after carbonoxide nanometer wall slurry drying, join in ionic liquid and evenly mix, add after nitrating agent microwave under the power of 1000～2000w to peel off 10～300 minutes, filter through first, the filter residue obtaining is filtered through organic solvent again, be filtered to filtrate with deionized water and be neutral, finally described filter residue and drying to constant weight is got final product to obtain to nitrogen-doped graphene nano belt.
In described step (a), the mass volume ratio of described carbon nanometer wall, the described vitriol oil, described potassium permanganate and described hydrogen peroxide is: 50g:1150ml:150g:250ml.
In described step (b), described nitrating agent is industrial ammonia or urea; The mass volume ratio of described carbonoxide nanometer wall, described ionic liquid and described industrial ammonia is 1g:(5～1000) ml:(5～50) ml, the mass volume ratio of described carbonoxide nanometer wall, described ionic liquid and described urea is 1g:(5～1000) ml:(1～20) g.
Described ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3,5-methylimidazole fluoroform sulfimide, 1,3-diethyl-4-methylimidazole fluoroform sulfimide, 1, at least one in 3-diethyl-5-Methylimidazole fluoroform sulfimide.
In described step (b), described organic solvent is 1-Methyl-2-Pyrrolidone or DMF.
In described step (a), described carbon nanometer wall is prepared by following steps: (c) etched substrate: substrate etching was cleaned up after 0.5～10 minute with the dilute acid soln of 0.01～1mol/L;
(d) prepare carbon nanometer wall: described substrate is placed in to oxygen-free environment and is heated to 600～900 ℃; then open substrate surface described in UV-irradiation; pass into again carbonaceous material and protective gas and keep 30～300 minutes, obtaining carbon nanometer wall at described substrate surface.
In described step (c), described substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, and described dilute acid soln is the one in hydrochloric acid, nitric acid, sulfuric acid, and the concentration of described dilute acid soln is 0.1～0.5mol/L.
In described step (c), the time of described etching is 1～3 minute, described for substrate deionized water, ethanol, acetone clean successively.
In described step (d); described carbonaceous material is the one in methane, ethane, propane, acetylene, ethanol; described protective gas is the one in helium, nitrogen, argon gas; the flow velocity that passes into described carbonaceous material is 10～1000sccm, and the volume ratio of described carbonaceous material and described protective gas is (2～10): 1.
The present invention also comprises the nitrogen-doped graphene nano belt of utilizing above-mentioned preparation method to make.
Compared with prior art, nitrogen-doped graphene nano belt of the present invention and preparation method thereof, there is following advantage: 1. adopt etching method to prepare vertical carbon nanometer wall with photochemical catalysis chemical Vapor deposition process, its preparation technology is simple, condition is easily controlled, improved production efficiency when shortening etching time, and photochemical catalysis can effectively reduce temperature of reaction, reduce energy consumption, reduce production costs, and can effectively avoid the problem occurring in the plasma method preparation process in existing method, make the thickness of carbon nanometer wall more even, structure is more complete.
2. adopt liquid-phase mixing nitrogenous source and carbonoxide nanometer wall technique, make nitrogen-doped graphene nano belt doping effect better, good uniformity, adopts ionic liquid to make solvent and can effectively prevent that graphene nanobelt from reuniting again, by simple separation, dryly can complete preparation process.
3. the productive rate of nitrogen-doped graphene nano belt is high, and the specific conductivity of nano belt is also improved, and raw material can be prepared voluntarily, has reduced production cost.
4. in preparation process, required equipment is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Accompanying drawing explanation
Fig. 1 is the prepared carbon nanometer wall SEM figure of the embodiment of the present invention 1.
Fig. 2 is the prepared nitrogen-doped graphene nano belt SEM figure of the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
The preparation process of nitrogen-doped graphene nano belt of the present invention is roughly divided into following steps: 1. etched substrate: substrate is put into the dilute acid soln etching 0.5～10 minute that concentration is 0.01～1mol/L, after etching, clean with deionized water, ethanol, acetone.
This step object is: by etching makes metal liner end eclipse surface produce defect to metal substrate, can effectively improve the surface tissue of metal substrate, make carbon nanometer wall energy enough in this metal substrate surface growth.
Wherein, the preferred time of this metal substrate of etching is 60～180 seconds, and the preferred acid strength of etching metal substrate is 0.1～0.5mol/L.Preferred etching condition above, can reach the effect of good etching, improves the growth efficiency of carbon nanometer wall.
2. prepare carbon nanometer wall: cleaned substrate is put into reaction chamber and get rid of the air of reaction chamber; then substrate is heated to 600～900 ℃; open again ultraviolet source equipment; make UV-irradiation at substrate surface; follow (2～10) by volume: 1 passes into carbonaceous material (flow is 10～1000sccm) and protective gas, and keeps 30～300 minutes.
This step object is: the air of getting rid of in reaction chamber can be removed the oxygen in reaction chamber, avoids the participation of oxygen and affects the growth of carbon nanometer wall, for the growth of carbon nanometer wall provides a stable environment.
After having reacted, stop passing into carbonaceous material, stop substrate heating; and close ultraviolet source equipment, question response chamber stops passing into protective gas after being cooled to room temperature, obtains carbon nanometer wall at substrate surface; it is scraped from substrate surface, just obtain pulverous carbon nanometer wall.
Wherein, substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, and dilute acid soln is the one in hydrochloric acid, nitric acid, sulfuric acid.Protective gas is the one in helium, nitrogen, argon gas, and carbonaceous material is the one in methane, ethane, propane, acetylene, ethanol.
3. prepare carbonoxide nanometer wall slurry: pulverous carbon nanometer wall that above-mentioned steps 2 is prepared joins in the vitriol oil of 0 ℃, add again potassium permanganate, keep the temperature of mixture to remain on below 10 ℃, stir after 2h, stir 24h in room-temperature water bath, under condition of ice bath, slowly add again deionized water, after 15min, add again the deionized water suction filtration that contains 30% concentration hydrogen peroxide, mixture color becomes glassy yellow afterwards, wash with the hydrochloric acid that concentration is 10%, suction filtration is after neutrality to filtrate again, obtains carbonoxide nanometer wall slurry.
Wherein, the mass volume ratio of carbon nanometer wall, the vitriol oil, potassium permanganate and hydrogen peroxide is: 50g:1150ml:150g:250ml.
4. prepare nitrogen-doped graphene nano belt: by after carbonoxide nanometer wall slurry drying, join in the container that ionic liquid is housed and evenly mix, then add nitrating agent, container microwave under the power of 1000～2000w is peeled off 10～300 minutes, then filter for the first time, the filter residue obtaining is passed through to organic solvent filter 23～6 time again, be filtered to filtrate with deionized water and be neutral, finally the filter residue cleaning up is dried in the drying baker of 60～100 ℃ to constant weight and gets final product to obtain nitrogen-doped graphene nano belt.
Wherein, nitrating agent is industrial ammonia or urea, and the mass volume ratio of carbonoxide nanometer wall, ionic liquid and described industrial ammonia is 1g:(5～1000) ml:(5～50) ml; The mass volume ratio of carbonoxide nanometer wall, ionic liquid and urea is 1g:(5～1000) ml:(1～20) g.
Organic solvent is 1-Methyl-2-Pyrrolidone (english abbreviation, NMP) or DMF (english abbreviation, DMF), can effectively remove ionic liquid.
Ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid (EtMeImBF
4), 1-ethyl-3-methylimidazole fluoroform sulfimide (EtMeImN (CF
3sO
2)
2), 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF
3sO
3), 1-ethyl-3-methylimidazole trifluoroacetic acid (EtMeImCF
3cO
2), 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon (EtMeImC (CF
3sO
2)
3), 1-ethyl-3-methylimidazole five acetyl fluoride imines (EtMeImN (C
2f
5sO
2)
2), 1-ethyl-3-methylimidazole two cyaniding nitrogen (EtMeImN (CN)
2), 1-ethyl-3,5-methylimidazole fluoroform sulfimide (1-Et-3,5-Me
2imN (CF
3sO
2)
2), 1,3-diethyl-4-methylimidazole fluoroform sulfimide (1,3-Et2-4-MeImN (CF
3sO
2)
2), 1,3-diethyl-5-Methylimidazole fluoroform sulfimide (1,3-Et2-5-MeIm N (CF
3sO
2)
2) at least one.
The present invention also comprises the nitrogen-doped graphene nano belt of utilizing above-mentioned preparation method to make.
With embodiment 1, the preparation process of nitrogen-doped graphene nano belt of the present invention is specifically described below.
Embodiment 1:1. etched substrate: nickel foil is put into the dilute hydrochloric acid solution etching 0.5 minute that concentration is 1mol/L, and etching is well cleaned with deionized water, ethanol, acetone afterwards.
2. prepare carbon nanometer wall: by cleaned nickel foil put into reaction chamber and and get rid of the air of described reaction chamber after nickel foil is heated to 900 ℃; then open ultraviolet source equipment; make UV-irradiation on nickel foil surface; then pass into carbonaceous material methane (flow is 200sccm) and protective gas nitrogen; the volume ratio of methane and nitrogen is 2:1, and keeps 100 minutes.
After having reacted, stop passing into carbonaceous material, stop nickel foil heating and close light source; question response chamber stops passing into protective gas after being cooled to room temperature; can obtain carbon nanometer wall on nickel foil surface, it is scraped from nickel foil surface, just obtain carbon nanometer wall powder.
3. prepare carbonoxide nanometer wall slurry: prepare carbonoxide nanometer wall slurry: 50g carbon nanometer wall is added to 0 ℃, in the vitriol oil of 1.15L, add again 150g potassium permanganate, the temperature of mixture remains on below 10 ℃, stir 2h, then stir after 24h in room-temperature water bath, under condition of ice bath, slowly add 4.6L deionized water, after 15min, add again 14L deionized water (wherein contain 250ml concentration be 30% hydrogen peroxide), mixture color becomes glassy yellow afterwards, suction filtration, wash with the hydrochloric acid that 2.5L concentration is 10% again, suction filtration, until filtrate is neutral.
4. prepare nitrogen-doped graphene nano belt: by after carbonoxide nanometer wall slurry drying, get 1g carbonoxide nanometer wall, join 50ml 1-ethyl-3-methylimidazole Tetrafluoroboric acid (EtMeImBF is housed
4) evenly mix in the container of ionic liquid, then add nitrating agent industrial ammonia 50ml, in the microwave oven that is 2000w at power by container, microwave was peeled off after 30 minutes, then filter for the first time, the filter residue obtaining is passed through to organic solvent 1-Methyl-2-Pyrrolidone (NMP) again to be filtered 6 times, be filtered to filtrate with deionized water and be neutral, finally the filter residue cleaning up is dried in the drying baker of 60 ℃ to constant weight and gets final product to obtain nitrogen-doped graphene nano belt.
In carbon nanometer wall SEM figure from Fig. 1, can find out, the carbon nanometer wall thickness that adopts photochemical catalysis chemical Vapor deposition process to prepare is even, is 20～40nm, and basic vertical substrates growth, and high consistency is good.As shown in the nitrogen-doped graphene nano belt SEM figure of Fig. 2, carbon nanometer wall is stripped from into after nitrogen-doped graphene nano belt, and width is even, is about 30～60nm, and length is about 5～10um.
Following table 1 is the design parameter of embodiment 2～11, and the processing step of embodiment 2～11 is identical with embodiment 1, and difference is processing parameter and processing condition, at this, its processing step is repeated no more.
Table 1
, there is following advantage in nitrogen-doped graphene nano belt of the present invention and preparation method thereof.
1. adopt etching method to prepare vertical carbon nanometer wall with photochemical catalysis chemical Vapor deposition process, its preparation technology is simple, condition is easily controlled, improved production efficiency when shortening etching time, and photochemical catalysis can effectively reduce temperature of reaction, reduce energy consumption, reduce production costs, and can effectively avoid the problem occurring in the plasma method preparation process in existing method, and make the thickness of carbon nanometer wall more even, structure is more complete.
2. adopt liquid-phase mixing nitrogenous source and carbonoxide nanometer wall technique, make nitrogen-doped graphene nano belt doping effect better, good uniformity, adopts ionic liquid to make solvent and can effectively prevent that graphene nanobelt from reuniting again, by simple separation, dryly can complete preparation process.
3. the productive rate of nitrogen-doped graphene nano belt is high, and the specific conductivity of nano belt is also improved, and raw material can be prepared voluntarily, has reduced production cost.
4. in preparation process, required equipment is all common chemical industry equipment, can save research and development equipment cost, is applicable to scale operation.
Foregoing; it is only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skills are according to main design of the present invention and spirit; can carry out very easily corresponding flexible or modification, therefore protection scope of the present invention should be as the criterion with the desired protection domain of claims.
Claims (10)
1. a preparation method for nitrogen-doped graphene nano belt, is characterized in that, comprises the steps:
(a) prepare carbonoxide nanometer wall slurry: get carbon nanometer wall and join in the vitriol oil, add potassium permanganate and stir, then adding deionized water to carry out suction filtration, wash afterwards with hydrochloric acid, suction filtration is neutral to filtrate, obtains carbonoxide nanometer wall slurry;
(b) prepare nitrogen-doped graphene nano belt: by after carbonoxide nanometer wall slurry drying, join in ionic liquid and evenly mix, add after nitrating agent microwave under the power of 1000～2000w to peel off 10～300 minutes, filter through first, the filter residue obtaining is filtered through organic solvent again, be filtered to filtrate with deionized water and be neutral, finally described filter residue and drying to constant weight is got final product to obtain to nitrogen-doped graphene nano belt.
2. preparation method according to claim 1, it is characterized in that, in described step (a), the mass volume ratio of described carbon nanometer wall, the described vitriol oil, described potassium permanganate and described hydrogen peroxide is: 50g:1150ml:150g:250 ml.
3. preparation method according to claim 1, is characterized in that, in described step (b), described nitrating agent is industrial ammonia or urea; The mass volume ratio of described carbonoxide nanometer wall, described ionic liquid and described industrial ammonia is 1g:(5～1000) ml:(5～50) ml, the mass volume ratio of described carbonoxide nanometer wall, described ionic liquid and described urea is 1g:(5～1000) ml:(1～20) g.
4. preparation method according to claim 3, it is characterized in that, described ionic liquid is 1-ethyl-3-methylimidazole Tetrafluoroboric acid, 1-ethyl-3-methylimidazole fluoroform sulfimide, 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid, 1-ethyl-3-methylimidazole trifluoroacetic acid, 1-ethyl-3-methylimidazole fluoroform sulphonyl carbon, 1-ethyl-3-methylimidazole five acetyl fluoride imines, 1-ethyl-3-methylimidazole two cyaniding nitrogen, 1-ethyl-3, 5-methylimidazole fluoroform sulfimide, 1, 3-diethyl-4-methylimidazole fluoroform sulfimide, 1, at least one in 3-diethyl-5-Methylimidazole fluoroform sulfimide.
5. preparation method according to claim 1, is characterized in that, in described step (b), described organic solvent is 1-Methyl-2-Pyrrolidone or DMF.
6. preparation method according to claim 1, is characterized in that, in described step (a), described carbon nanometer wall is prepared by following steps:
(c) etched substrate: substrate etching was cleaned up after 0.5～10 minute with the dilute acid soln of 0.01～1mol/L;
(d) prepare carbon nanometer wall: described substrate is placed in to oxygen-free environment and is heated to 600～900 ℃; then open substrate surface described in UV-irradiation; pass into again carbonaceous material and protective gas and keep 30～300 minutes, obtaining carbon nanometer wall at described substrate surface.
7. preparation method according to claim 6, it is characterized in that, in described step (c), described substrate is a kind of in iron foil, nickel foil, cobalt paper tinsel, described dilute acid soln is the one in hydrochloric acid, nitric acid, sulfuric acid, and the concentration of described dilute acid soln is 0.1～0.5mol/L.
8. preparation method according to claim 6, is characterized in that, in described step (c), the time of described etching is 1～3 minute, described for substrate deionized water, ethanol, acetone clean successively.
9. preparation method according to claim 6; it is characterized in that; in described step (d); described carbonaceous material is the one in methane, ethane, propane, acetylene, ethanol; described protective gas is the one in helium, nitrogen, argon gas; the flow velocity that passes into described carbonaceous material is 10～1000 sccm, and the volume ratio of described carbonaceous material and described protective gas is (2～10): 1.
10. the nitrogen-doped graphene nano belt that the arbitrary described preparation method of claim 1 to 9 makes.
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| CN103935976A (en) * | 2013-01-18 | 2014-07-23 | 海洋王照明科技股份有限公司 | Carbon nanometer wall and graphene nanoribbon as well as preparing method thereof |
| CN106450311A (en) * | 2016-10-14 | 2017-02-22 | 焦作聚能能源科技有限公司 | Graphite composite anode material and preparation method thereof |
| JP2017064675A (en) * | 2015-10-02 | 2017-04-06 | 株式会社Ihi | Catalyst and solid polymer fuel cell prepared therewith |
| CN110155998A (en) * | 2019-05-13 | 2019-08-23 | 东南大学 | A kind of ribbon nitrogen-doped graphene and its preparation method and application |
| CN113299929A (en) * | 2021-03-03 | 2021-08-24 | 昆明理工大学 | Preparation method of F, S, N co-doped Fe-N-C fuel cell oxygen reduction catalyst |
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| CN103935976A (en) * | 2013-01-18 | 2014-07-23 | 海洋王照明科技股份有限公司 | Carbon nanometer wall and graphene nanoribbon as well as preparing method thereof |
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| CN106450311A (en) * | 2016-10-14 | 2017-02-22 | 焦作聚能能源科技有限公司 | Graphite composite anode material and preparation method thereof |
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| CN113299929A (en) * | 2021-03-03 | 2021-08-24 | 昆明理工大学 | Preparation method of F, S, N co-doped Fe-N-C fuel cell oxygen reduction catalyst |
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