CN103779081A - Graphene/graphene oxide thin film and preparation method thereof, and usage - Google Patents
Graphene/graphene oxide thin film and preparation method thereof, and usage Download PDFInfo
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- CN103779081A CN103779081A CN201210406046.4A CN201210406046A CN103779081A CN 103779081 A CN103779081 A CN 103779081A CN 201210406046 A CN201210406046 A CN 201210406046A CN 103779081 A CN103779081 A CN 103779081A
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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 provides a graphene/graphene oxide thin film and a preparation method thereof and application. The preparation method comprises a first step of preparation of a graphene oxide thin film, a second step of preparation of a grapheme suspension, and a third step of preparation of a graphene/graphene oxide thin film, wherein vacuum filtration is carried out on a graphene oxide suspension, a water solution with a cross-linked agent is added, filtering and drying continue to be carried out, a thin film is obtained, the thin film is removed from a filtering film, and the graphene oxide thin film is obtained; and the graphene oxide thin film obtained in the first step is put on a spin coater for spinning, the grapheme suspension obtained in the second step drops on the spin coater to which the graphene oxide thin film is attached, removal is carried out after 20 to 60min, and the graphene/graphene oxide thin film is obtained after drying. The graphene/graphene oxide thin film is light in weight, high in conductivity, strong in mechanical properties, good in stability and the like. A super capacitor adopts the graphene/graphene oxide thin film as a current collector and is large in energy-storage capacity and long in service life.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of graphene/graphene oxide film and its production and use.
Background technology
Collector is a kind of structure or part that collects electric current, major function is that the electric current that active material is produced collects, and electron channel is provided, and accelerates electric charge and shifts, improve and discharge and recharge a coulomb efficiency, need to meet the features such as conductivity is high, good mechanical property, quality is light, internal resistance is little as collector.
Conventionally, anodal aluminium foil, the negative pole of adopting of collector adopts copper/nickel foil, and advantage is good conductivity, and quality is soft, more common also relatively inexpensive, but the density of metal collector is large, quality weight, makes battery or super capacitor energy density lower; And in charge and discharge cycles repeatedly and the situation such as overcharge, electrolyte, on metal collector surface, reduction reaction occurs, and makes its corrosion, electrode reaction resistance increases, and causes capacity attenuation obviously to be accelerated, and reduces the safety in utilization of battery or ultracapacitor.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of graphene/graphene oxide film and its production and use, this graphene/graphene oxide film has excellent mechanical performance, and conductivity is strong, quality is light, can be applicable in ultracapacitor, as collector, greatly improve stored energy capacitance and the useful life of ultracapacitor, and preparation method's technique is simple.
First aspect, the invention provides a kind of preparation method of graphene/graphene oxide film, comprises the following steps:
(1) preparation of graphene oxide film: graphene oxide suspension is passed through to miillpore filter vacuum filtration, filter complete, obtain filter cake, on filter cake, add the aqueous solution of aziridine crosslinker or epoxy silane crosslinking agent, continue to filter, until filter completely, filter cake is placed in to baking oven dries, after oven dry, obtain film, then film is taken off from filter membrane, obtain graphene oxide film;
(2) preparation of graphene suspension;
(3) preparation of graphene/graphene oxide film: the graphene oxide film in (1) is placed on sol evenning machine, rotation, according to the mass ratio of Graphene and graphene oxide 1: 1-1:3, the graphene suspension of (2) gained is dropped on the sol evenning machine with graphene oxide film lentamente, after 20-60min, take off, in vacuum drying chamber, 40-80 ° of dry processing of C, obtains graphene/graphene oxide film.
In step (1), preferably, graphene oxide suspension makes by the following method: get graphite oxide and be scattered in deionized water, ethanol, methyl alcohol or isopropyl alcohol, and ultrasonic, make graphene oxide suspension.
Preferably, the temperature of oven dry is 40 ° of C.
Preferably, the thickness of graphene oxide film is 3-10 μ m.
Preferably, the mass fraction of the aqueous solution of aziridine crosslinker or epoxy silane crosslinking agent is 10%-50%.
Preferably, the mass ratio of aziridine crosslinker or epoxy silane crosslinking agent and graphene oxide is 1:9-999.
Preferably, the concentration of graphene oxide suspension is 0.25-1g/L.
Be easier to prepare complete, uniform graphene oxide film by graphene oxide suspension, because a large amount of carboxyls, hydroxy functional group are contained in graphene oxide surface, by graphene oxide suspension by after miillpore filter vacuum filtration again by the processing of crosslinking agent, carboxyl, hydroxyl in crosslinking agent and graphene oxide react, thereby obtain having the graphene oxide film compared with high-mechanical property.
In step (2), preferably, graphene suspension makes by the following method: Graphene is joined to 1-METHYLPYRROLIDONE (NMP), DMF (DMF) or N, in N-dimethylacetylamide (DMAc), carry out ultrasonic dispersion, form graphene suspension.
Preferably, the concentration of graphene suspension is 1-5g/L.
In step (3), preferably, the speed of rotation is 250-1000rpm/min.
Using graphene oxide film complete, even and that there is stronger mechanical performance as substrate, then obtain graphene/graphene oxide film at its surperficial spin coating graphene film, single-layer graphene has good conduction, heat conductivility and low thermal coefficient of expansion, strengthened the electric conductivity of graphene/graphene oxide film, the graphene/graphene oxide film obtaining has the advantages such as quality is light, conductivity is high, mechanical performance is strong, good stability.
Second aspect, the invention provides a kind of graphene/graphene oxide film, and described graphene/graphene oxide film is for to make according to aforementioned preparation method.
The third aspect, the invention provides a kind of ultracapacitor, comprises collector, electrode and electrolyte, and described collector is described graphene/graphene oxide film.
Described graphene/graphene oxide film quality is light, while being applied to battery or ultracapacitor, the energy density of battery or ultracapacitor is greatly improved; Graphene/graphene oxide film has excellent mechanical performance and electric conductivity, uses that this graphene/graphene oxide film is large as the ultracapacitor energy storage capacity of collector, the life-span is long.And graphene/graphene oxide thin film stability is better, can further improve the safety in utilization of battery or ultracapacitor.
Graphene film provided by the invention and its production and use, has following beneficial effect:
Be easier to prepare complete, uniform graphene oxide film by graphene oxide suspension, because a large amount of carboxyls, hydroxy functional group are contained in graphene oxide surface, by graphene oxide suspension by after miillpore filter vacuum filtration again by the processing of crosslinking agent, carboxyl, hydroxyl in crosslinking agent and graphene oxide react, thereby obtain having the graphene oxide film compared with high-mechanical property.Using graphene oxide film complete, even and that there is stronger mechanical performance as substrate, then obtain graphene/graphene oxide film at its surperficial spin coating graphene film, single-layer graphene has good conduction, heat conductivility and low thermal coefficient of expansion, strengthened the electric conductivity of graphene/graphene oxide film, the graphene/graphene oxide film obtaining has the advantages such as quality is light, conductivity is high, mechanical performance is strong, good stability.
Graphene/graphene oxide film quality prepared by the present invention is light, while being applied to battery or ultracapacitor, can make the energy density of battery or ultracapacitor be greatly improved; Graphene/graphene oxide film is complete evenly, have excellent mechanical performance and electric conductivity, uses that this graphene/graphene oxide film is large as the ultracapacitor energy storage capacity of collector, the life-span is long.And graphene/graphene oxide thin film stability is better, can further improve the safety in utilization of battery or ultracapacitor.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) preparation of graphene oxide film: get 1g graphite oxide and be scattered in deionized water, ultrasonic, making concentration is the graphene oxide suspension of 0.25g/L, passed through miillpore filter vacuum filtration, when seeing while not having obvious filtrate on filter cake, on filter cake, adding mass fraction is 10% the aziridine crosslinker aqueous solution, the mass ratio of aziridine crosslinker and graphene oxide is 1:999, continue to filter, until filter completely, obtain filter cake, filter cake is placed in to baking oven dries in 40 ° of C, after oven dry, obtain film, then film is taken off from filter membrane, obtain the graphene oxide film of 3 μ m.
(2) preparation of graphene suspension: 1g Graphene is joined and carries out ultrasonic dispersion 1h in nmp solvent, the graphene suspension that to form concentration be 1g/L.
(3) graphene/graphene oxide film preparation: the graphene oxide film in (1) is placed on sol evenning machine, with the speed rotation of 250rpm/min, according to the mass ratio 1:1 of Graphene and graphene oxide, by the suspension of (2) gained, drop in slowly on the sol evenning machine with graphene oxide film, after 20min, take off, in the vacuum drying chamber of 40 ° of C, dry processing, just can obtain graphene/graphene oxide film.
Embodiment 2
(1) preparation of graphene oxide film: get 1g graphite oxide and be scattered in ethanol, ultrasonic, making concentration is the graphene oxide suspension of 0.5g/L, passed through miillpore filter vacuum filtration, when seeing while not having obvious filtrate on filter cake, on filter cake, adding mass fraction is 30% epoxy silane cross-linking agent aqueous solution, the mass ratio of epoxy silane crosslinking agent and graphene oxide is 1:19, continue to filter, until filter completely, obtain filter cake, filter cake is placed in to baking oven dries in 40 ° of C, after oven dry, obtain film, then film is taken off from filter film, obtain the graphene oxide film of 8 μ m.
(2) preparation of graphene suspension: 0.5g Graphene is joined and carries out ultrasonic dispersion 1h in DMF solvent, the graphene suspension that to form concentration be 3g/L.
(3) graphene/graphene oxide film preparation: the graphene oxide film in (1) is placed on sol evenning machine, with the speed rotation of 800rpm/min, according to the mass ratio 1:2 of Graphene and graphene oxide, by the suspension of (2) gained, drop in slowly on the sol evenning machine with graphene oxide film, after 40min, take off, in the vacuum drying chamber of 60 ° of C, dry processing, just can obtain graphene/graphene oxide film.
Embodiment 3
(1) preparation of graphene oxide film: get 1g graphite oxide and be scattered in isopropyl alcohol, ultrasonic, making concentration is the graphene oxide suspension of 1g/L, passed through miillpore filter vacuum filtration, when seeing while not having obvious filtrate on filter cake, on filter cake, adding mass fraction is 50% epoxy silane cross-linking agent aqueous solution, the mass ratio of epoxy silane crosslinking agent and graphene oxide is 1:9, continue to filter, until filter completely, obtain filter cake, filter cake is placed in to baking oven dries in 40 ° of C, after oven dry, obtain film, then film is taken off from filter membrane, obtain the graphene oxide film of 10 μ m.
(2) preparation of graphene suspension: 0.3g Graphene is joined and carries out ultrasonic dispersion 2h in DMAc solvent, the graphene suspension that to form concentration be 5g/L.
(3) graphene/graphene oxide film preparation: the graphene oxide film in (1) is placed on sol evenning machine, with the speed rotation of 1000rpm/min, according to the mass ratio 1:3 of Graphene and graphene oxide, by the suspension of (2) gained, drop in slowly on the sol evenning machine with graphene oxide film, after 60min, take off, in the vacuum drying chamber of 80 ° of C, dry processing, just can obtain graphene/graphene oxide film.
Comparative example:
(1) preparation of graphene oxide film: get 1g graphite oxide and be scattered in isopropyl alcohol, ultrasonic, making concentration is the graphene oxide suspension of 1g/L, passed through miillpore filter vacuum filtration, filter cake is placed in to baking oven dries in 40 ° of C, after oven dry, obtain film, then film is taken off from filter membrane, obtain the graphene oxide film of 10 μ m.
(2) preparation of graphene suspension: Graphene is joined and carries out ultrasonic dispersion 2h in DMAc solvent, the graphene suspension that to form concentration be 5g/L.
(3) graphene/graphene oxide film preparation: the graphene oxide film in (1) is placed on sol evenning machine, with the speed rotation of 1000rpm/min, according to the mass ratio 1:3 of Graphene and graphene oxide, by the suspension of (2) gained, drop in slowly on the sol evenning machine with graphene oxide film, after 60min, take off, in the vacuum drying chamber of 80 ° of C, dry processing, just can obtain graphene/graphene oxide film.
Effect embodiment
Graphene/graphene oxide film prepared by the embodiment of the present invention 1 carries out conductance measurement and hot strength test.
1, the mensuration of conductivity: sample is at room temperature used to the two electrical measurement four point probe tester testing conductivities of D41-11D/ZM type.In the time that measuring current is shown as probe coefficient, press electricalresistivityρ's button, screen directly shows that electricalresistivityρ is worth, and directly calculates conductivity according to γ=l/ ρ.
Test result is as shown in table 1:
Table 1
As shown in Table 1, after adding crosslinking agent, the conductivity of graphene/graphene oxide film does not have larger reduction.
2, hot strength test: extension test carries out on dynamic mechanical analyzer (DMA Q800/TA), and sample is cut into 3 × 15mm
2rectangular sheet carry out tension test test.
Test result is as shown in table 2:
Table 2
As shown in Table 2, after adding crosslinking agent, the hot strength of graphene/graphene oxide film increases.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for graphene/graphene oxide film, is characterized in that, comprises the following steps:
(1) preparation of graphene oxide film: graphene oxide suspension is passed through to miillpore filter vacuum filtration, filter complete, obtain filter cake, on filter cake, add the aqueous solution of aziridine crosslinker or epoxy silane crosslinking agent, continue to filter, until filter completely, filter cake is placed in to baking oven dries, after oven dry, obtain film, then film is taken off from filter membrane, obtain graphene oxide film;
(2) preparation of graphene suspension;
(3) preparation of graphene/graphene oxide film: the graphene oxide film in (1) is placed on sol evenning machine, rotation, according to the mass ratio of Graphene and graphene oxide 1: 1-1:3, the graphene suspension of (2) gained is dropped on the sol evenning machine with graphene oxide film lentamente, after 20-60min, take off, in vacuum drying chamber, 40-80 ° of dry processing of C, obtains graphene/graphene oxide film.
2. the preparation method of graphene/graphene oxide film as claimed in claim 1, is characterized in that: the mass fraction of the aqueous solution of described aziridine crosslinker or epoxy silane crosslinking agent is 10%-50%.
3. the preparation method of graphene/graphene oxide film as claimed in claim 1, is characterized in that: the mass ratio of described aziridine crosslinker or epoxy silane crosslinking agent and graphene oxide is 1:9-999.
4. the preparation method of graphene/graphene oxide film as claimed in claim 1, it is characterized in that: described graphene oxide suspension makes by the following method: get graphite oxide and be scattered in deionized water, ethanol, methyl alcohol or isopropyl alcohol, ultrasonic, make graphene oxide suspension.
5. the preparation method of graphene/graphene oxide film as claimed in claim 1, is characterized in that: the thickness of described graphene oxide film is 3-10 μ m.
6. the preparation method of graphene/graphene oxide film as claimed in claim 1, it is characterized in that: described graphene suspension makes by the following method: Graphene is joined to 1-METHYLPYRROLIDONE, N, dinethylformamide or N, in N-dimethylacetylamide, carry out ultrasonic dispersion, form graphene suspension.
7. the preparation method of graphene/graphene oxide film as claimed in claim 1, is characterized in that: the concentration of described graphene oxide suspension is 0.25-1g/L, and the concentration of described graphene suspension is 1-5g/L.
8. the preparation method of graphene/graphene oxide film as claimed in claim 1, is characterized in that: the speed of described rotation is 250-1000rpm/min.
9. a graphene/graphene oxide film, is characterized in that: by the method preparation described in 1 ~ 8 arbitrary claim.
10. a ultracapacitor, comprises collector, electrode and electrolyte, it is characterized in that: described collector is graphene/graphene oxide film as claimed in claim 9.
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Cited By (4)
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| CN107810049A (en) * | 2015-05-28 | 2018-03-16 | 曼彻斯特大学 | The purification of water |
| CN108358198A (en) * | 2018-03-07 | 2018-08-03 | 中国工程物理研究院化工材料研究所 | Multiple environment response driving graphene oxide film, preparation method and application |
| CN108376615A (en) * | 2018-03-03 | 2018-08-07 | 济宁利特纳米技术有限责任公司 | A kind of button ultracapacitor graphene-based electrode slice and preparation method thereof |
| CN108910870A (en) * | 2018-07-20 | 2018-11-30 | 西安交通大学 | A kind of pollution-free shifting process of CVD graphene obtains the laminated film and method of graphene oxide and graphene composite structure |
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| CN102403050A (en) * | 2010-09-08 | 2012-04-04 | 中国科学院金属研究所 | Composite material based on nanometer, preparation method of composite material and application in flexible energy storage device |
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| US20100323178A1 (en) * | 2007-05-14 | 2010-12-23 | Northwestern University | Ceramic composite thin films |
| CN102403050A (en) * | 2010-09-08 | 2012-04-04 | 中国科学院金属研究所 | Composite material based on nanometer, preparation method of composite material and application in flexible energy storage device |
| CN101948108A (en) * | 2010-10-02 | 2011-01-19 | 上海交通大学 | Optimized preparation method of oxidized graphite paper |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107810049A (en) * | 2015-05-28 | 2018-03-16 | 曼彻斯特大学 | The purification of water |
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| CN108910870A (en) * | 2018-07-20 | 2018-11-30 | 西安交通大学 | A kind of pollution-free shifting process of CVD graphene obtains the laminated film and method of graphene oxide and graphene composite structure |
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