CN105006572A - Production method and application of nitrogen doped graphene dispersion film - Google Patents
Production method and application of nitrogen doped graphene dispersion film Download PDFInfo
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- CN105006572A CN105006572A CN201410163215.5A CN201410163215A CN105006572A CN 105006572 A CN105006572 A CN 105006572A CN 201410163215 A CN201410163215 A CN 201410163215A CN 105006572 A CN105006572 A CN 105006572A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a production method and an application of a nitrogen doped graphene dispersion film. The film is formed by treating a nitrogen doped graphene dispersion liquid through a film forming technology, and the dispersion liquid comprises nitrogen doped graphene, an anionic dye and a solvent. The anion organic dye is adopted to disperse the nitrogen doped graphene for the first time in order to realize a long-term uniform and stable dispersion effect and benefit a subsequent film forming technology, and any existing nitrogen doped graphene is used as a raw material to produce the nitrogen doped graphene dispersion film with different thicknesses and different dimensions according to different demands. The production method has the advantages of simple process, low cost, short reaction time, high efficiency, non-toxicity, and small pollution to environment, and the obtained film has very good three dimensional structure and high specific surface area, can be widely used in fields of electronic devices, composite materials, sensing, biological analysis and energy storage materials, and is especially used in the production of flexible and non-flexible supercapacitors, flexible lithium ion batteries and fuel batteries.
Description
Technical field
The present invention relates to a kind of graphene-based material, particularly a kind of nitrogen-doped graphene disperses preparation method and the application of film forming.
Background technology
Graphene (Graphene) is a kind of zero energy gap semiconductor material, and being applied to microelectronic component need regulate its band gap or carrier concentration etc.Chemical doping is a kind of effective ways realizing controlled material physics, chemical property, as passed through element or the molecular chemistry doped graphene material of electron rich or electron deficient, the carrier concentration of Graphene can be regulated and controled, thus realize the regulation and control to its physical and chemical performance such as bandwidth and catalytic property.Theoretical study results shows, introduce as Graphene can be transformed into semiconductor from the semimetal of zero band gap by the hetero-atoms such as N, B effectively in graphene sheet layer, form the Graphene of n-type or the doping of p-type, predictive of the potential application foreground of doped graphene in fields such as optics, electricity, magnetics.After this, numerous experimental science man is devoted to the chemical doping technique study of Graphene.Have by chemical vapour deposition (CVD) (CVD) method, using methane gas as carbon source, ammonia as nitrogenous source, to be deposited on the 25nm copper film of silicon substrate surface for catalyst, keep 10 minutes under the high temperature of 800 DEG C, obtained which floor nitrogen-doped graphene of minority.Also have the method adopting electrothermal reaction, take ammonia as nitrogenous source, nitrogen-atoms is replaced the carbon atom in Graphene lattice, prepared nitrogen-doped graphene; Take graphene oxide as initiation material and ammonia be nitrogenous source, realize the reduction of GO and the doping of nitrogen by high annealing simultaneously, obtained nitrogen-doped graphene; With oxidation state graphite and melamine for reaction raw materials high annealing legal system is for the method for nitrogen-doped graphene; Take graphene oxide dispersion as initiation material and different nitrogenous sources, by hydro thermal method or solvent-thermal method, prepare nitrogen-doped graphene and hydrogel.In addition, use arc discharge method is also had to prepare boron or nitrogen-doped graphene.
But the preparation of existing nitrogen-doped graphene film is only limitted to prior for graphene oxide film forming, then by high annealing be realize the doping of nitrogen and the reduction of graphene oxide under the prerequisite of nitrogenous source at ammonia simultaneously, thus obtained nitrogen-doped graphene film.The method need adopt the professional equipments such as high annealing, also needs to use corrosive ammonia etc., and its preparation condition is harsh, cost is high, danger is large, therefore is not suitable for large-scale production.In addition, the nitrogen-doped graphene specific area prepared by thermal annealing method is little, limits promoting the use of of prepared product.Current, development fast, method that is simple, green and that efficiently prepare nitrogen-doped graphene film has been called one of the study hotspot and emphasis of industry.
Summary of the invention
An object of the present invention is to provide a kind of nitrogen-doped graphene film and preparation method thereof, and it has the features such as cost is low, quick, efficient, thus overcomes deficiency of the prior art.
Two of object of the present invention is the application providing aforementioned nitrogen-doped graphene film, the application particularly in energy storage device.
For realizing aforementioned invention object, present invention employs following technical scheme:
A kind of nitrogen-doped graphene film, mainly formed by film technique process nitrogen-doped graphene dispersion liquid, described nitrogen-doped graphene dispersion liquid comprises nitrogen-doped graphene, anionic dye and solvent, and wherein the mass ratio of nitrogen-doped graphene and anionic dye is 1 ~ 400:1.
A preparation method for nitrogen-doped graphene film, comprising: get in the solvent that nitrogen-doped graphene is dispersed in containing anionic dye, form nitrogen-doped graphene dispersion liquid,
And, utilize nitrogen-doped graphene dispersion liquid described in film technique process, form described nitrogen-doped graphene film.
Further, described solvent comprises water or organic solvent, described anionic dye can be selected from but be not limited to methyl orange, Yihong, Congo red, algae is red, any one or two or more combinations in nigrosine, picric acid, acid fuchsin.
Any one nitrogen-doped graphene film aforesaid is preparing the application in energy storage device, and described energy storage device comprises capacitor or battery.
A kind of energy storage device, comprise positive and negative electrode, barrier film and electrolyte, and at least described plus or minus electrode comprises any one nitrogen-doped graphene film aforesaid.
Further, described energy storage device includes but not limited to flexibility and inflexibility ultracapacitor, flexible lithium ion battery or fuel cell.
Compared with prior art, beneficial effect of the present invention comprises:
(1) anionic organic dyes is adopted to disperse nitrogen-doped graphene first, long-term uniform and stable dispersion effect can be reached, for follow-up film-forming process provides necessary precondition, efficiently solve nitrogen-doped graphene scattering problem, and the nitrogen-doped graphene that existing any one method is prepared and obtained all can be used as raw material of the present invention application, and different-thickness can be prepared according to different demand, the nitrogen-doped graphene film of different size size, obtained product has extraordinary three-dimensional structure, for the application in electron stored energy provides high-specific surface area, electronic device can be widely used in, composite material, sensing, bioanalysis, the fields such as energy storage material.
(2) preparation method of the present invention is simple and easy to do, and course of reaction is easy to control, safety, cost are low, is easy to promote the use of.
Accompanying drawing explanation
Fig. 1 a-1b be respectively embodiment 1 obtain the optics picture of nitrogen-doped graphene hydrogel.
Fig. 2 a-2b be respectively embodiment 1 obtain the SEM picture after nitrogen-doped graphene freeze drying.
Fig. 3 be embodiment 1 obtain the elementary analysis collection of illustrative plates of nitrogen-doped graphene.
Fig. 4 be embodiment 1 obtain the photo of nitrogen-doped graphene-methyl orange aqueous dispersions.
Fig. 5 a-5b be respectively embodiment 1 obtain the optics picture of nitrogen-doped graphene film.
Fig. 6 a-6b be respectively embodiment 1 obtain the SEM picture of nitrogen-doped graphene film.
Embodiment
As previously shown, in view of existing nitrogen-doped graphene is dispersed into that the difficulty existed in film method is large, production cost is high, reaction equipment needed thereby complexity, severe reaction conditions, yields poorly, is difficult to the technical problems such as suitability for industrialized production, inventor is after studying for a long period of time and putting into practice, provide the method for a kind of nitrogen-doped graphene dispersion film forming, its technological process mainly comprises: one, prepare nitrogen-doped graphene raw material; Two, by nitrogen-doped graphene stock dispersion in solvent, prepare the stable dispersions of certain solubility; Three, utilize and multi-formly carry out film forming, obtain flexible nitrogen-doped graphene film.
Further say, the method for nitrogen-doped graphene dispersion film forming of the present invention comprises the steps:
Utilize prepare nitrogen-doped graphene raw material without preparation method, then by its stable dispersion in the aqueous solution or organic solution of anionic organic dyes, the nitrogen-doped graphene film utilizing different film techniques to prepare different-thickness, different size size.
The preparation method of aforementioned nitrogen-doped graphene raw material includes but not limited to one or more in hydro thermal method, solvent-thermal method, chemical vapour deposition technique, liquid-phase impregnation process, calcination method, microwave method, and the embodiment of these methods all can be seen in the pertinent literature announced before making the present invention.
Aforementioned anionic organic dyestuff include but not limited to methyl orange, Yihong, Congo red, algae is red, nigrosine, picric acid, acid fuchsin etc. one or more.
Aforementioned solvents comprises water or organic solvent, such as, can be selected from but be not limited to ethanol, isopropyl alcohol, n-butanol etc.
Aforementioned film technique includes but not limited to one or more of vacuum filtration method, spin-coating method, spraying process, czochralski method, LB embrane method, roller coating etc.
Aforesaid nitrogen-doped graphene film can be used for preparing energy storage device, such as but not limited to active material or the collector of flexible and inflexibility ultracapacitor, and the negative material in flexible lithium ion battery or collector, or the catalyst in fuel cell.
In flexible and inflexibility ultracapacitor and flexible lithium ion battery, example is applied as with it, such devices can comprise positive pole, negative pole, electrolyte, barrier film and shell etc., wherein, negative or positive electrode can be made up of active material (that is, aforementioned nitrogen-doped graphene film) and collector (such as aluminium foil etc.); Electrolyte can be selected from but be not limited to tetraethylammonium tetrafluoroborate, alkaline electrolyte, acidic electrolysis bath, PVA-acidic electrolysis bath and PVA-alkaline electrolyte etc.; Barrier film material can be selected from but be not limited to polyethylene, polypropylene, polyethylene and polyacrylic mixture, polytetrafluoroethylene, nonwoven fabrics etc.
The shell of foregoing soft and inflexibility ultracapacitor or flexible lithium ion battery can select the features such as flexible material is made, and it should have flexible, has ductility, and sealing is good.
The nitrogen-doped graphene film that the present invention obtains can also be widely used in the fields such as electronic device, composite material, sensing, bioanalysis, energy storage material.
Below in conjunction with accompanying drawing and some preferred embodiments, technical scheme of the present invention is described in further detail.
embodiment 1
(1) preparation of nitrogen-doped graphene
Get 5 mL 4 mg/mL graphene oxide aqueous dispersions, 6 g urea and 12.5 mL deionized waters to mix, after ultrasonic 1 h fully mixes, pour in polytetrafluoroethyllining lining and put into autoclave, hydro-thermal reaction 12 h at 180 DEG C, naturally room temperature is down to, take out sample deionized water and soak dialysis after 24 hours, obtain nitrogen-doped graphene hydrogel product, its optics picture is as Fig. 1 a-1b, product can carry out freeze drying further, its pattern can consult Fig. 2 a-2b, and its Elemental analysis data refers to Fig. 3.
(2) preparation of nitrogen-doped graphene dispersion liquid
Above-mentioned preparation is obtained nitrogen-doped graphene product and put into 200 mL 1 × 10
-4in mol/L methyl orange aqueous solution, ultrasonic 2 h, can obtain the nitrogen-doped graphene-methyl orange aqueous dispersions of homogeneous dispersion, its form refers to Fig. 4.
(3) preparation of nitrogen-doped graphene film
Get nitrogen-doped graphene-methyl orange aqueous solution 30 mL of above-mentioned homogeneous dispersion, add 50 mL deionized waters and dilute, the method for recycling vacuum filtration carries out film forming, and namely obtain nitrogen-doped graphene film after drying at 80 DEG C, its pattern refers to Fig. 5 a-Fig. 6 b.
Separately get aforementioned nitrogen-doped graphene film and be directly assembled into button ultracapacitor as electrode material, test its electric property, under current density is 1 A/g, its capacitance reaches ~ 300 F/g.
embodiment 2
(1) preparation of nitrogen-doped graphene
Get 10 mL 4 mg/mL graphene oxide aqueous dispersions, 6 g urea and 25 mL deionized waters to mix, after ultrasonic 1 h fully mixes, pour in polytetrafluoroethyllining lining and put into autoclave, hydro-thermal reaction 12 h at 180 DEG C, naturally be down to room temperature, take out sample deionized water and soak dialysis after 24 hours, obtain nitrogen-doped graphene product, product can carry out freeze drying further, and its shape and element composition is close with embodiment 1.
(2) preparation of nitrogen-doped graphene dispersion liquid
Above-mentioned preparation is obtained nitrogen-doped graphene product and put into 200 mL 1 × 10
-4in mol/L methyl orange aqueous solution, ultrasonic 2 h, can obtain the nitrogen-doped graphene-methyl orange aqueous dispersions of homogeneous dispersion.
(3) preparation of nitrogen-doped graphene film
Get nitrogen-doped graphene-methyl orange aqueous solution 30 mL of above-mentioned homogeneous dispersion, add 50 mL deionized waters and dilute, the method for recycling vacuum filtration carries out film forming, and namely obtain nitrogen-doped graphene film after drying at 80 DEG C, its pattern is close with embodiment 1.
Separately get nitrogen-doped graphene film and be directly assembled into all-solid-state flexible ultracapacitor as electrode material, test its electric property, under current density is 1 A/g, its capacitance reaches ~ 200 F/g.
Should be appreciated that above explanation, drawing and embodiment can not resolve to restriction design philosophy of the present invention.Hold in ken of the present invention and identically know that the knowledgeable can to technological thought of the present invention with the improvement of various form, such improvement and change and also should belong to protection scope of the present invention.
Claims (10)
1. a preparation method for nitrogen-doped graphene dispersion film forming, it is characterized in that it is mainly formed by film technique process nitrogen-doped graphene dispersion liquid, described nitrogen-doped graphene dispersion liquid comprises nitrogen-doped graphene, anionic dye and solvent.
2. the preparation method of nitrogen-doped graphene dispersion film forming according to claim 1, is characterized in that the mass ratio of nitrogen-doped graphene and anionic dye contained by described nitrogen-doped graphene dispersion liquid is 1 ~ 400:1.
3. according to the nitrogen-doped graphene dispersion film forming described in claim 1, it is characterized in that described solvent comprises water or organic solvent, described anionic dye comprise methyl orange, Yihong, Congo red, algae is red, any one or two or more combinations in nigrosine, picric acid, acid fuchsin.
4. a preparation method for nitrogen-doped graphene film, is characterized in that comprising: get in the solvent that nitrogen-doped graphene is dispersed in containing anionic dye, form nitrogen-doped graphene dispersion liquid,
And, utilize nitrogen-doped graphene dispersion liquid described in film technique process, form described nitrogen-doped graphene film.
5. the preparation method of nitrogen-doped graphene film according to claim 4, is characterized in that described film technique comprises any one or two or more combinations in vacuum filtration method, spin-coating method, spraying process, czochralski method, LB embrane method, roll coating process.
6. the preparation method of the nitrogen-doped graphene film according to any one of claim 4-5, it is characterized in that described solvent comprises water or organic solvent, described anionic dye comprise methyl orange, Yihong, Congo red, algae is red, any one or two or more combinations in nigrosine, picric acid, acid fuchsin.
7. the preparation method of the nitrogen-doped graphene film according to any one of claim 4-6, is characterized in that the preparation technology of described N doping graphite comprises hydro thermal method, solvent-thermal method, chemical vapour deposition technique, liquid-phase impregnation process, calcination method or microwave method.
8. according to any one of claim 1-7, nitrogen-doped graphene film is preparing the application in energy storage device, and described energy storage device comprises capacitor or battery.
9. an energy storage device, comprises positive and negative electrode, barrier film and electrolyte, it is characterized in that at least described plus or minus electrode comprises the nitrogen-doped graphene film according to any one of claim 1-7.
10. energy storage device according to claim 9, is characterized in that comprising flexibility and inflexibility ultracapacitor, flexible lithium ion battery or fuel cell.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105551580A (en) * | 2015-12-24 | 2016-05-04 | 安徽大学 | High-transmittance conductive thin film and preparation method therefor |
| CN110060877A (en) * | 2019-04-26 | 2019-07-26 | 北京化工大学 | A kind of supercapacitor polyatom doped carbon/polyaniline composite material preparation method |
| WO2021017598A1 (en) * | 2019-07-26 | 2021-02-04 | 瑞新材料科技(香港)有限公司 | Method for manufacturing electrode having protective layer |
| CN113148993A (en) * | 2021-04-20 | 2021-07-23 | 中国航发北京航空材料研究院 | Preparation method of nitrogen-doped graphene aqueous slurry |
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| CN105551580A (en) * | 2015-12-24 | 2016-05-04 | 安徽大学 | High-transmittance conductive thin film and preparation method therefor |
| CN105551580B (en) * | 2015-12-24 | 2017-05-31 | 安徽大学 | A kind of high transmittance conductive film and preparation method thereof |
| CN110060877A (en) * | 2019-04-26 | 2019-07-26 | 北京化工大学 | A kind of supercapacitor polyatom doped carbon/polyaniline composite material preparation method |
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| CN113148993A (en) * | 2021-04-20 | 2021-07-23 | 中国航发北京航空材料研究院 | Preparation method of nitrogen-doped graphene aqueous slurry |
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