CN102887501B - A kind of preparation method of nitrating Graphene - Google Patents
A kind of preparation method of nitrating Graphene Download PDFInfo
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Abstract
The invention provides a kind of method adopting chemical Vapor deposition process to prepare nitrating Graphene, comprising step has: provide resistant to elevated temperatures substrate, solid-state/or the organic carbon source compound of liquid state and solid-state and/or liquid organic nitrogen source compounds; By organic carbon source compound and organic nitrogen source compounds mixing, and be mixed with mixture solution or suspension liquid; Mixture solution or suspension liquid are coated in substrate surface; Under anaerobic, the substrate being coated with mixture is warming up to 500 ~ 1300 DEG C and makes mixture reaction, generate nitrating Graphene.The preparation method of nitrating Graphene of the present invention does not need to add catalyzer in addition, effectively improves the production technique simplifying nitrating Graphene, reduces production cost, such that itrogen content of getter with nitrogen doped in nitrating Graphene is easy to control, uniform doping, and electrochemical stability performance is high.
Description
Technical field
The invention belongs to the technical field of carbon material, be specifically related to a kind of preparation method of nitrating Graphene.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal that strong K sea nurse (AndreK.Geim) of peace moral etc. of Univ Manchester UK in 2004 finds, is the very thin carbon material of single or multiple lift.Because the structure of its uniqueness and photoelectric property become the study hotspot in the fields such as carbon material, nanotechnology, Condensed Matter Physics and functional materials, many scientific workers are attracted.Single-layer graphene has large specific surface area, and excellent conduction, heat conductivility and low thermal expansivity, can be used for effect transistor, electrode materials, matrix material, liquid crystal display material, sensor.The method preparing Graphene at present mainly contains graphite breakaway, chemistry redox method, ultrasonic stripping method etc.But, prepared on a large scale in the process of Graphene by redox method at present, Graphene after reduction is also containing oxygen-containing functional groups such as-the OH ,-C-O-C-of small amount and-COOH, and these functional groups can reduce electrochemical stability and the electrochemical stability of Graphene.
At present, there is the correlative study adopting process for preparing graphenes by chemical vapour deposition, but, existing chemical Vapor deposition process needs to utilize catalyzer, and this catalyzer is metal or metallic compound makees catalyzer, but when being placed on substrate by this catalyzer, catalyst distribution can be caused uneven.In order to solve the problem of this catalyst distribution inequality, catalyst deposit to substrate, is increased the homogeneity of above-mentioned catalyst distribution by existing general chemical Vapor deposition process, physical vaporous deposition, vacuum thermal evaporation, magnetron sputtering method, plasma enhanced chemical vapor deposition method and print process.Therefore, existing employing process for preparing graphenes by chemical vapour deposition needs to add catalyzer in addition, and high to equipment requirements, and complicated operation, causes high cost.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, provide that a kind of technique is simple, productive rate is high, production cost is low, the preparation method of the nitrating Graphene be easy to operate and control.
In order to realize foregoing invention object, the technical scheme of the embodiment of the present invention is as follows:
A preparation method for nitrating Graphene, comprises the steps:
Substrate, solid-state and/or liquid organic carbon source compound and solid-state and/or liquid organic nitrogen source compounds are provided;
By described organic carbon source compound and organic nitrogen source compounds mixing, and be mixed with mixture solution or suspension liquid;
Described mixture solution or suspension liquid are coated in described substrate surface;
Under oxygen-free environment, vacuum condition, the described substrate being coated with mixture solution or suspension liquid is warming up to 500 ~ 1300 DEG C and makes mixture reaction, generate described nitrating Graphene.
The preparation method of above-mentioned nitrating Graphene is by solid-state and/or liquid organic carbon source compound, the mixing of solid-state and/or liquid organic nitrogen source compounds, be mixed with solution or suspension liquid, and be directly coated in the surface of substrate, make organic carbon source compound and organic nitrogen source compounds direct reaction, do not need to add catalyzer in addition, effectively simplify the production technique of nitrating Graphene, reduce production cost, simultaneously, adopt the nitrating Graphene of chemical Vapor deposition process synthesis, make that itrogen content of getter with nitrogen doped in nitrating Graphene is easy to control, uniform doping, electrochemical stability performance is high.
Accompanying drawing explanation
Fig. 1 is preparation method's process flow diagram of embodiment of the present invention nitrating Graphene;
Fig. 2 is the Electronic Speculum figure of nitrating Graphene prepared by the embodiment of the present invention 1;
Fig. 3 is the X-ray electronic spectrum of nitrating Graphene prepared by the embodiment of the present invention 1.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide that a kind of technique is simple, productive rate is high, production cost, the preparation method of the nitrating Graphene be easy to operate and control.The technical process of the preparation method of this nitrating Graphene as shown in Figure 1, comprises the steps:
S1: substrate, solid-state and/or liquid organic carbon source compound and solid-state and/or liquid organic nitrogen source compounds are provided;
S2: by organic carbon source compound and organic nitrogen source compounds mixing, and be mixed with mixture solution or suspension liquid;
S3: mixture solution or suspension liquid are coated in substrate surface;
S4: under oxygen-free environment, vacuum condition, is warming up to 500 ~ 1300 DEG C by the substrate being coated with mixture solution or suspension liquid and makes mixture reaction, generates described nitrating Graphene.
Particularly, in the preparation method step S1 of above-mentioned nitrating Graphene, substrate should be high temperature resistant, and as the high temperature of 500 ~ 1300 DEG C in step S4, it is preferably one or more arbitrary combination in Copper Foil, iron foil, nickel foil.The substrate of this preferred material is high temperature resistant, and thermal stability is good.
Above-mentioned organic carbon source compound is preferably at least one in ferrocene, dicyclopentadienylcobalt, nickelocene, two luxuriant manganese, and organic nitrogen source compounds is preferably at least one in urea, aniline, N-methyl-p-nitroaniline.This preferred organic carbon source compound and organic nitrogen source compounds have good solubility energy, uniform solution can be mixed with, and the surface of substrate can be coated in uniformly, form even and thin rete, thus effectively reduce the thickness of the nitrating Graphene of surviving in following step S4.Wherein, containing metal ion in this preferred organic carbon source compound, the existence of this metal ion, is conducive to the generation of nitrating Graphene, to improve the productive rate of nitrating Graphene.Certain above-mentioned organic carbon source compound and organic nitrogen source compounds also solid-state and/or liquid organic carbon source compound and solid-state and/or liquid organic nitrogen source compounds can substitute with other.When selected organic carbon source compound and/or organic nitrogen source compounds be insoluble organic carbon source compound and/or organic nitrogen source compounds time, (as ball milling) can be ground and prepared uniform suspension liquid.
In the preparation method step S2 of above-mentioned nitrating Graphene, the mode of this organic carbon source compound and organic nitrogen source compounds mixing can adopt ultrasonic mixing, is uniformly mixed, one or more arbitrary combination in ball grinding stirring.Reach and made both well-mixed objects.In order to mixed organic carbon source compound and organic nitrogen source compounds being evenly coated on substrate, this mixture should be mixed with solution or suspension liquid, after organic carbon source compound and organic nitrogen source compounds can first mix by the mode prepared, then solubilizing agent (as deionized water etc.) makes organic carbon source compound and organic nitrogen source compounds be uniformly dispersed in a solvent; Also solvent (as deionized water etc.) can be added in mixing process, this organic carbon source compound, organic nitrogen source compounds and solvent are preferably adopted ultrasonic mixing, is uniformly mixed, the mode of one or more arbitrary combination in ball grinding stirring mixes, thus form mixture solution or the suspension liquid that mass percentage concentration is preferably 5 ~ 30%.This mixture solution concentration does not strictly limit, as prepared saturated mixture solution etc.
In the preparation method step S3 of above-mentioned nitrating Graphene, method mixture solution or suspension liquid being coated to substrate surface preferably adopts one or more arbitrary combination in spread coating, spin-coating method, infusion method, thus reach the production technique simplifying and prepare nitrating Graphene, reduce the object of production cost.
In this step S3, before substrate surface application of mixture solution or suspension liquid, to be cleaned by this substrate preferably in advance, the mode of cleaning preferably adopts ionized water, ethanol, acetone ultrasonic cleaning post-drying successively, stand-by.Clean this substrate sticks to substrate surface foreign material with removing, reach the object of clean substrate, to be conducive to the coating of mixture solution or suspension liquid.The cleaning in early stage of this substrate see the purging method in the step S11 in following embodiment 1.
In the preparation method step S4 of above-mentioned nitrating Graphene, this oxygen free condition is to remove oxygen, and nitrating Graphene is produced can carry out smoothly, and prevent under the high temperature conditions, the Graphene of generation is oxidized.This oxygen free condition is the oxygen-free atmosphere that rare gas element is formed, e.g., nitrogen atmosphere, argon gas atmosphere etc., preferred oxygen free condition is nitrogen atmosphere; Oxygen free condition also can be the condition vacuumized, and the condition of this vacuum effectively can not only remove oxygen, and can also remove impurity such as flying away aerial dust simultaneously, thus ensures the purity of nitrating Graphene further.In addition, the condition of this vacuum can also promote the reaction of above-mentioned organic carbon source compound and organic nitrogen source compounds, thus improves the productive rate of nitrating Graphene.Wherein, the condition optimization of this vacuum is that vacuum tightness is less than 10
-3the vacuum condition of Pa.Certainly, at oxygen free condition can be the oxygen free condition of normal pressure.
In this step S4, the carbon and nitrogen atoms mol ratio of this organic carbon source compound and organic nitrogen source compounds is preferably 2 ~ 20: 1, and the time that this organic carbon source compound and organic nitrogen source compounds carry out reacting is preferably 1 ~ 300 minute.The preferred proportion of this organic carbon source compound and organic nitrogen source compounds consumption, the content of nitrogen element in the nitrating Graphene generated can be made at a best content range, thus improve the electrochemical stability performance of this nitrating Graphene further, make organic carbon source compound and organic nitrogen source compounds fully react simultaneously, improve the utilization ratio of reactant, thus further reduce production cost.Fully react both the preferred time that this organic carbon source compound and organic nitrogen source compounds carry out reacting can ensure, the nitrating Graphene generated fully is deposited.
In this step S4, the lifting of underlayer temperature and this organic carbon source compound, providing of organic nitrogen source compounds temperature of reaction preferably adopt the method for one or more the combination in hot-wire chemical gas-phase deposition, radio-frequency plasma enhancing chemical vapour deposition, Microwave Plasma Torch Atomic Emission Spect rometry, laser chemical vapor deposition, low-pressure chemical vapor deposition, aumospheric pressure cvd to provide thermal source.According to the difference of aforementioned thermal source presentation mode, therefore, embodiment of the present invention chemical Vapor deposition process is also preferably one or more the combination in hot-wire chemical gas-phase deposition, radio-frequency plasma enhancing chemical vapour deposition, Microwave Plasma Torch Atomic Emission Spect rometry, laser chemical vapor deposition, low-pressure chemical vapor deposition, aumospheric pressure cvd accordingly.When providing thermal source namely to adopt laser induced chemical vapor depostion method to synthesize nitrating Graphene as adopted laser induced chemical vapor depostion method, because laser energy is concentrated, organic carbon source compound and organic nitrogen source compounds reaction efficiency can be made to improve further, thus improve the production efficiency of nitrating Graphene.
In this step S4, after organic carbon source compound contacts with organic nitrogen source compounds reaction, stop the heating to substrate, under the condition ensureing anaerobic, reaction system is cooled.
Further, in a preferably embodiment of the present invention, the preparation method of above-mentioned nitrating Graphene also comprises the step of the purifying of the nitrating Graphene synthesized in step S4.The step of this nitrating Graphene purifying is preferably: cooled substrate is put into dilute acid soln and soak 0.1 ~ 24 hour, removes and does not participate in the reactant of reaction, the by product of production and other impurity completely, then clean with deionized water, then dry.Wherein, diluted acid kind can but at least one be not only only in hydrochloric acid, sulfuric acid, nitric acid.The concentration of this diluted acid is preferably greater than 0.01mol/L, is less than 1mol/L.
From the above mentioned, the preparation method of above-mentioned nitrating Graphene is by solid-state and/or liquid organic carbon source compound, solid-state and/or liquid organic nitrogen source compounds mixing, be mixed with solution or suspension liquid, and be directly coated in the surface of substrate, make organic carbon source compound and organic nitrogen source compounds direct reaction, do not need to add catalyzer in addition, effectively improve the production technique simplifying nitrating Graphene, reduce production cost, simultaneously, adopt the nitrating Graphene of chemical Vapor deposition process synthesis, make itrogen content of getter with nitrogen doped in nitrating Graphene easy to control, uniform doping, electrochemical stability performance is high.Wherein, by controlling the consumption of organic carbon source compound and nitrogenous source chemical combination, making the content of nitrogen element in the nitrating Graphene synthesized at a best content range, thus improving the electrochemical stability performance of this nitrating Graphene further.
Now for the preparation method of concrete nitrating Graphene, the present invention is further elaborated.
Embodiment 1:
The preparation method of nitrating Graphene, comprises the steps:
S11. by nickel foil substrate deionized water, ethanol, acetone ultrasonic cleaning post-drying, and adopt be uniformly mixed method ground mode by carbon and nitrogen atoms mol ratio be 5: 1 ferrocene and urea mix, deionized water is added in the process be uniformly mixed, it is 20wt% mixing solutions that ferrocene and urea are mixed with mass percentage concentration, is then spun on substrate surface;
S12. the substrate being coated with mixing solutions is put into reaction chamber, and enclosed reaction chamber, adopt mechanical pump, reaction chamber is evacuated to 10 by lobe pump and molecular pump step by step
-3below Pa, and after keeping 10 minutes, closure molecule pump, starts heating;
S13. when underlayer temperature reaches 500 DEG C, keep temperature-resistant, start to generate nitrating Graphene;
S14. question response is after 300 minutes, stops silicon, and is cooled to room temperature, obtains nitrating Graphene;
S15. the dust technology that the substrate of nitrating Graphene puts into 0.7mol/L by surface deposition soaks 0.1 hour, removes the reactant, ferrous metal particle and other impurity that do not participate in completely reacting, then cleans with deionized water, dry, collect this nitrating Graphene.
The nitrating Graphene synthesized by the present embodiment 1 carries out Electronic Speculum (SEM) scanning analysis, and Electronic Speculum (SEM) scanned picture of this nitrating Graphene as shown in Figure 2.As shown in Figure 2, the nitrating Graphene that the present embodiment 1 synthesizes is two-dimensional film shape, and its size is about 0.5 ~ 5 μm.
The nitrating Graphene synthesized by the present embodiment 1 carries out X-ray electronic spectrum (XPS) analysis, and its XPS result as shown in Figure 3.According to the result of Fig. 3, the nitrating Graphene nitrogen content that the present embodiment 1 synthesizes is about 8.3%.
Embodiment 2
The preparation method of nitrating Graphene, comprises the steps:
S21. by nickel foil substrate deionized water, ethanol, acetone ultrasonic cleaning post-drying, and adopt ball milling hybrid system ground mode by carbon and nitrogen atoms mol ratio be 10: 1 nickelocene and aniline mix, deionized water is added in the process be uniformly mixed, it is 5wt% mixing solutions that nickelocene and aniline are mixed with mass percentage concentration, is then spun on substrate surface;
S22. the substrate being coated with mixing solutions is put into reaction chamber, and enclosed reaction chamber, adopt mechanical pump, reaction chamber is evacuated to 10 by lobe pump and molecular pump step by step
-3below Pa, and after keeping 30 minutes, closure molecule pump, starts heating;
S23. when underlayer temperature reaches 1300 DEG C, keep temperature-resistant, start to generate nitrating Graphene;
S24. question response is after 1 minute, stops silicon, and is cooled to room temperature, obtains nitrating Graphene;
S25. the dust technology that the substrate of nitrating Graphene puts into 0.4mol/L by surface deposition soaks 8 hours, removes the reactant, nickel metallic particles and other impurity that do not participate in completely reacting, then cleans with deionized water, dry, collect this nitrating Graphene.
Embodiment 3
The preparation method of nitrating Graphene, comprises the steps:
S31. by iron foil substrate deionized water, ethanol, acetone ultrasonic cleaning post-drying, and adopt be uniformly mixed method ground mode by carbon and nitrogen atoms mol ratio be 2: 1 dicyclopentadienylcobalt and urea mix, deionized water is added in the process be uniformly mixed, it is 30wt% mixing solutions that dicyclopentadienylcobalt and urea are mixed with mass percentage concentration, and then blade coating is in substrate surface;
S32. the substrate being coated with mixing solutions is put into reaction chamber, and enclosed reaction chamber, adopt mechanical pump, reaction chamber is evacuated to 10 by lobe pump and molecular pump step by step
-3below Pa, and after keeping 1 minute, closure molecule pump, starts heating;
S33. when underlayer temperature reaches 1000 DEG C, keep temperature-resistant, start to generate nitrating Graphene;
S34. question response is after 100 minutes, stops silicon, and is cooled to room temperature, obtains nitrating Graphene;
S35. the dust technology that the substrate of nitrating Graphene puts into 0.2mol/L by surface deposition soaks 16 hours, removes the reactant, cobalt metallic particles and other impurity that do not participate in completely reacting, then cleans with deionized water, dry, collect this nitrating Graphene.
Embodiment 4
The preparation method of nitrating Graphene, comprises the steps:
S41. by iron foil substrate deionized water, ethanol, acetone ultrasonic cleaning post-drying, and adopt be uniformly mixed method ground mode by carbon and nitrogen atoms mol ratio be 20: 1 two luxuriant manganese and urea mix, deionized water is added in the process be uniformly mixed, it is 10wt% mixing solutions that dicyclopentadienylcobalt and urea are mixed with mass percentage concentration, is then spun on substrate surface;
S42. the substrate being coated with mixing solutions is put into reaction chamber, and enclosed reaction chamber, adopt mechanical pump, reaction chamber is evacuated to 10 by lobe pump and molecular pump step by step
-3below Pa, and after keeping 20 minutes, closure molecule pump, starts heating;
S43. when underlayer temperature reaches 700 DEG C, keep temperature-resistant, start to generate nitrating Graphene;
S44. question response is after 200 minutes, stops silicon, and is cooled to room temperature, obtains nitrating Graphene;
S45. the dust technology that the substrate of nitrating Graphene puts into 0.08mol/L by surface deposition soaks 24 hours, removes the reactant, manganese metallic particles and other impurity that do not participate in completely reacting, then cleans with deionized water, dry, collect this nitrating Graphene.
Embodiment 5
The preparation method of nitrating Graphene, comprises the steps:
S51. by iron foil substrate deionized water, ethanol, acetone ultrasonic cleaning post-drying, and adopt be uniformly mixed method ground mode by carbon and nitrogen atoms mol ratio be 20: 1 two luxuriant manganese, ferrocene, urea and aniline mix, deionized water is added in the process be uniformly mixed, being mixed with mass percentage concentration is 15wt% mixing solutions, is then spun on substrate surface; Wherein, the mol ratio of two luxuriant manganese and ferrocene is 1: 2, and the mol ratio of urea and aniline is 1: 1;
S52. the substrate being coated with mixing solutions is put into reaction chamber, and enclosed reaction chamber, adopt mechanical pump, reaction chamber is evacuated to 10 by lobe pump and molecular pump step by step
-3below Pa, and after keeping 20 minutes, closure molecule pump, starts heating;
S53. when underlayer temperature reaches 1200 DEG C, keep temperature-resistant, start to generate nitrating Graphene;
S54. question response is after 200 minutes, stops silicon, and is cooled to room temperature, obtains nitrating Graphene;
S55. the dust technology that the substrate of nitrating Graphene puts into 0.08mol/L by surface deposition soaks 24 hours, removes the reactant, manganese metallic particles and other impurity that do not participate in completely reacting, then cleans with deionized water, dry, collect this nitrating Graphene.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method for nitrating Graphene, comprises the steps:
Substrate, solid-state and/or liquid organic carbon source compound and solid-state and/or liquid organic nitrogen source compounds are provided; Wherein, described organic carbon source compound is at least one in dicyclopentadienylcobalt, nickelocene, two luxuriant manganese; Described organic nitrogen source compounds is at least one in urea, aniline, N-methyl-p-nitroaniline; The carbon and nitrogen atoms mol ratio of described organic carbon source compound and organic nitrogen source compounds is 2 ~ 20:1;
By described organic carbon source compound and organic nitrogen source compounds mixing, and be mixed with mixture solution or suspension liquid;
Described mixture solution or suspension liquid are coated in described substrate surface;
10 are less than in oxygen-free environment, vacuum tightness
-3under the vacuum condition of Pa, the described substrate being coated with mixture solution or suspension liquid is warming up to 500 ~ 1300 DEG C and makes mixture reaction 1 ~ 300 minute, generate described nitrating Graphene;
Catalyzer is not added in the preparation method of described nitrating Graphene.
2. the preparation method of nitrating Graphene according to claim 1, is characterized in that: the mass percent concentration of described mixture solution or suspension liquid is 5 ~ 30%.
3. the preparation method of nitrating Graphene according to claim 1, is characterized in that: described substrate is at least one in Copper Foil, iron foil, nickel foil.
4. the preparation method of nitrating Graphene according to claim 1, is characterized in that: also comprise the step of described nitrating Graphene being carried out purifying.
5. the preparation method of nitrating Graphene according to claim 4, is characterized in that: the step that described nitrating Graphene carries out purifying is greater than 0.01mol/L for nitrating Graphene is put into concentration, is less than in 1mol/L dilute acid soln and carries out immersion 0.1 ~ 24 hour.
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| CN103265023A (en) * | 2013-06-07 | 2013-08-28 | 新疆师范大学 | Preparation method of nitrogen-doped graphene |
| CN103265024A (en) * | 2013-06-08 | 2013-08-28 | 新疆师范大学 | Method for preparing graphene compound |
| CN103407991B (en) * | 2013-07-10 | 2015-02-18 | 西北工业大学 | Preparation method of nickel/nickel oxide-decorated nitrogen-doped graphene material |
| EP2857550A1 (en) * | 2013-10-02 | 2015-04-08 | Basf Se | Amine precursors for depositing graphene |
| TWI622554B (en) * | 2015-06-22 | 2018-05-01 | Univ Chung Yuan Christian | Method for producing nitrogen-doped graphene and manufacturing method of composite heat sink |
| CN106145101B (en) * | 2016-07-06 | 2018-08-10 | 北京光科博冶科技有限责任公司 | A kind of bigger serface nitrogen-doped graphene and preparation method thereof |
| CN106517133B (en) * | 2016-10-09 | 2018-08-21 | 华中科技大学 | Ultra-thin layer of charcoal of nitrating three-dimensional co-continuous porous structure and its preparation method and application |
| CN109911887A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of N doping porous graphene |
| CN114349060B (en) * | 2021-12-29 | 2024-03-12 | 山西大学 | Preparation method of carbon-coated magnetic nanoparticle nitrogen-doped magnetic graphene |
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