CN102522208A - Graphene horizontal structure super capacitor and preparation method thereof - Google Patents
Graphene horizontal structure super capacitor and preparation method thereof Download PDFInfo
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- CN102522208A CN102522208A CN2011104397990A CN201110439799A CN102522208A CN 102522208 A CN102522208 A CN 102522208A CN 2011104397990 A CN2011104397990 A CN 2011104397990A CN 201110439799 A CN201110439799 A CN 201110439799A CN 102522208 A CN102522208 A CN 102522208A
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Abstract
A graphene horizontal structure super capacitor and a preparation method thereof relate to a super capacitor and a preparation method and solve the problem that a vertical structure of the existing super capacitor can not be compatible with physical and chemical performance shown by graphene on a two-dimensional plane. The structure of the capacitor is that a left graphene electric conducting film electrode (2), a right graphene electric conducting film electrode (3), a left metal electrode (4) and a right metal electrode (5) are manufactured on a substrate (1) sequentially, and a solid electrolyte layer (6) is filled between the left graphene electric conducting film electrode (2) and the right graphene electric conducting film electrode (3). The preparation method includes: step 1, preparing an oxidation graphene film; step 2, preparing graphene electric conducting film electrodes; step 3, preparing metal electrodes; and step 4, preparing the horizontal structure super capacitor. The super capacitor can be widely applied to the fields of military equipment such as electronic products, new energy traffic, new energy generating systems, electromagnetic pulse.
Description
Technical field
The present invention relates to the preparation method of ultracapacitor, relate in particular to a kind of preparation method of novel graphene-based horizontal structure ultracapacitor.
Background technology
Ultracapacitor belongs to the low-carbon economy product of standard.Compare with secondary cell, ultracapacitor has the power density height, has extended cycle life, and the charging interval is short, but characteristics such as high current charge-discharge; Wherein, its great advantage is: short time high power output.In view of its characteristics, ultracapacitor can be widely used in military equipment fields such as electronic product, new forms of energy traffic, grid-connected power generation system, distributed energy-storage system and electromagnetic pulse.Current, ultracapacitor is regarded as a kind of powerful physics secondary power supply, and each main developed country is all the research of ultracapacitor being classified as state key strategy project.Electrode material is a component most crucial in the ultracapacitor, and at present the most widely used is carbon electrode, comprises carbon-based materials such as activated carbon, carbon fiber, CNT, carbon aerogels, vitrescence carbon.Graphene has the specific area of superelevation in theory as a kind of novel material with carbon element, particularly on two-dimensional directional, shows good transport properties, is a kind of desirable electrode material.Present stage mainly is confined to traditional vertical stratification device for the research of graphene-based ultracapacitor, and the physical and chemical performance that this vertical stratification and Graphene show on two dimensional surface can not be compatible, thereby be unfavorable for giving full play to of this material property.
Summary of the invention
The present invention to solve technical problem and be: in order to improve the various performance parameters of ultracapacitor; Further optimize the application of grapheme material in ultracapacitor; The present invention provides a kind of preparation method of novel graphene-based horizontal structure ultracapacitor, forms the ultracapacitor with higher capacity density simultaneously.The present invention is exactly the design feature according to Graphene, makes full use of its high conduction characteristic in the horizontal direction, makes up novel horizontal structure ultracapacitor.
Technical scheme of the present invention:
A kind of graphene-based horizontal structure ultracapacitor; This horizontal structure ultracapacitor is sequentially built left side graphene conductive membrane electrode, right graphene conductive membrane electrode, left metal electrode, a right metal electrode on substrate, fills solid-state electrolyte layer between left graphene conductive membrane electrode, the right graphene conductive membrane electrode.
A kind of preparation method of graphene-based horizontal structure ultracapacitor, the preparation method of this horizontal structure ultracapacitor may further comprise the steps:
The preparation of step 1 graphene oxide film
It is 0.01～1% aqueous dispersions that graphene oxide is processed mass concentration;
With this dispersion liquid through drop-coating, vertical deposition method, dip-coating method or layer by layer self-assembling method deposit on the substrate, under 25 ℃～100 ℃, obtain graphene oxide film after the drying;
The preparation of step 2 graphene conductive membrane electrode
Above-mentioned graphene oxide film is placed under the reducing environment together with substrate handles, obtain graphene film; Draw one gash with blade on resulting graphene film surface, measure the tool marks both sides with universal instrument and be in open-circuit condition, obtain left and right graphene conductive membrane electrode;
Or draw one gash on resulting graphene oxide film surface with blade; Again graphene oxide film is placed on to handle under the reducing environment together with substrate and obtains graphene film; Measure the tool marks both sides with universal instrument and be in open-circuit condition, obtain left and right graphene conductive membrane electrode;
The preparation of step 3 metal electrode
The cut and the cut that block left and right graphene conductive membrane electrode with mask plate are peripheral, are exposing a part near the film edge place; Utilize the exposed part vapor deposition left and right metal electrode of vacuum thermal evaporation filming equipment at above-mentioned graphene conductive membrane electrode;
The preparation of step 4 horizontal structure ultracapacitor
With left and right metal electrode as the ultracapacitor collector electrode; Left and right graphene conductive membrane electrode is the left and right electrode of ultracapacitor; Between left and right graphene conductive membrane electrode, fill solid-state electrolyte layer, make graphene-based horizontal structure ultracapacitor.
In the described step 1, when adopting vertical deposition method to prepare graphene oxide film, substrate is placed on graphene oxide, and to process mass concentration be in 0.01～1% the aqueous dispersions, and with the horizontal direction angle be 10 °～80 °.
The preparation of the graphene conductive membrane electrode in the described step 2, the employed instrument of formation open circuit, mode are not limit, and the cut width is less than 2 μ m.
The preparation of described metal electrode, the shape of exposed part and the cut that blocked thereof periphery area is unrestricted on the mask plate.
In the step 1, the thickness of graphene oxide film is 10～1000nm.
In the step 1, substrate (1) is simple glass substrate, quartz substrate.
The present invention compares the beneficial effect that is had with prior art:
The present invention has broken away from the traditional vertical stratification of ultracapacitor and has made thinking, has designed a kind of novel horizontal structure scheme.Simultaneously, this horizontal ultracapacitor is the compatible design feature of grapheme material on the structure, the utilization of amplitude peak the characteristic of Graphene two dimensional surface.Compare with the vertical stratification ultracapacitor, the capacity density of this novel graphene-based horizontal structure ultracapacitor significantly improves.
Description of drawings
The sketch map of the graphene-based horizontal structure ultracapacitor of Fig. 1.
The capacity curve of the graphene-based horizontal structure ultracapacitor of Fig. 2.
Embodiment
A kind of graphene-based horizontal structure ultracapacitor; Like Fig. 1; Sequentially built left side graphene conductive membrane electrode 2, right graphene conductive membrane electrode 3, left metal electrode 4, right metal electrode 5 on substrate 1 are filled solid-state electrolyte layer 6 between left graphene conductive membrane electrode 2, the right graphene conductive membrane electrode 3.
One of preparation method of a kind of graphene-based horizontal structure ultracapacitor, its step comprises:
The preparation of step 1 graphene oxide film
Configuration quality concentration is 0.01% graphene oxide aqueous dispersions.With the simple glass is substrate 1, and glass substrate 1 is placed in the container that fills above-mentioned dispersion liquid from the horizontal by 10 °, puts the slow evaporation drying of incubator or baking oven then into, and temperature is controlled at 100 ℃.After treating the moisture evaporate to dryness, on glass substrate, obtain graphene oxide film, average thickness is 10nm.
The preparation of step 2 graphene conductive membrane electrode
The graphene oxide film that step 1 is obtained is at Ar/H
2Mix reducing gases (5Vol.%H
2) protection down handles 30min in 500 ℃ and obtain the graphene conductive film.Draw gash with cutter one in graphene conductive film middle, measure the tool marks both sides with universal instrument and be in open-circuit condition, form left and right graphene conductive membrane electrode 2,3 in the tool marks both sides.
The preparation of step 3 metal electrode
The cut and the cut that block graphene conductive membrane electrode in the step 2 with mask plate are peripheral, are exposing the strip part near the film edge place.With the spun gold is deposition material, utilizes the exposed part gold evaporation of vacuum thermal evaporation filming equipment at above-mentioned graphene conductive membrane electrode, forms left and right metal electrode 4,5.
The preparation of step 4 horizontal structure ultracapacitor
With left and right metal electrode 4,5 as the ultracapacitor collector electrode; Left and right graphene conductive membrane electrode 2,3 is the left and right electrode of ultracapacitor; The mixture (the mixing quality ratio is 0.3: 1: 0.1) that poly (vinyl alcohol) binder, phosphoric acid conductive agent, polyethyleneimine: amine plasticizer are formed is filled between the left and right graphene conductive membrane electrode (2,3) and peripheral part as solid electrolyte, and specific capacity can reach 57 μ F/cm
2
A kind of preparation method's of graphene-based horizontal structure ultracapacitor two, its step comprises:
The preparation of step 1 graphene oxide film
Configuration quality concentration is 1% graphene oxide aqueous dispersions.With the quartz is substrate 1, with its horizontal positioned.Adopt drop-coating, utilize pipettor that above-mentioned dispersant liquid drop is added on the quartz substrate, form moisture film at substrate surface.Put this quartz substrate in the incubator slow evaporation drying, temperature is controlled at 25 ℃.Treat on substrate, to obtain graphene oxide film behind the moisture evaporate to dryness, average thickness is 1000nm.
The preparation of step 2 graphene conductive membrane electrode
The graphene oxide film that step 1 is obtained is at Ar/H
2Mix reducing gases (5Vol.%H
2) protection down handles 30min in 1050 ℃ and obtain the graphene conductive film.Draw gash with triangular knife one in the film middle, measure the tool marks both sides with universal instrument and be in open-circuit condition, form left and right graphene conductive membrane electrode 2,3 in the tool marks both sides.
The preparation of step 3 metal electrode
The cut and the cut that block the graphene conductive membrane electrode in the step 2 with mask plate are peripheral, are exposing the strip part near the film edge place.With the aluminium wire is deposition material, utilizes the vacuum thermal evaporation filming equipment, at the exposed part AM aluminum metallization of above-mentioned graphene conductive membrane electrode, forms left and right metal electrode 4,5.
The preparation of step 4 horizontal structure ultracapacitor
As the ultracapacitor collector electrode, the left and right sides electrode that left and right graphene conductive membrane electrode is a ultracapacitor, mass ratio are that 0.2: 1: 0.2 polyethylene glycol oxide is adhesive, LiCF with left and right metal electrode
3SO
3The mixture that conductive agent, ethylene carbonate/propylene carbonate plasticizer are formed is filled between the left and right graphene conductive membrane electrode (2,3) and peripheral part as solid electrolyte, and specific capacity can reach 118 μ F/cm
2
A kind of preparation method's of graphene-based horizontal structure ultracapacitor three, its step comprises:
The preparation of step 1 graphene oxide film
Configuration quality concentration is 0.5% graphene oxide aqueous dispersions.With the simple glass is substrate 1, and glass substrate 1 is placed in the container that fills above-mentioned dispersion liquid from the horizontal by 80 °, puts the slow evaporation drying of incubator or baking oven then into, and temperature is controlled at 50 ℃.After treating the moisture evaporate to dryness, on glass substrate, obtain graphene oxide film, average thickness is 470nm.
The preparation of step 2 graphene conductive membrane electrode
The graphene oxide film that step 1 is obtained is at Ar/H
2Mix reducing gases (5Vol.%H
2) protection down handles 30min in 500 ℃ and obtain the graphene conductive film.Draw gash with the wallpaper cutter one in graphene conductive film middle, measure the tool marks both sides with universal instrument and be in open-circuit condition, form left and right graphene conductive membrane electrode 2,3 in the tool marks both sides.
The preparation of step 3 metal electrode
The cut and the cut that block graphene conductive membrane electrode in the step 2 with mask plate are peripheral, are exposing the strip part near the film edge place.With the spun gold is deposition material, utilizes the exposed part gold evaporation of vacuum thermal evaporation filming equipment at above-mentioned graphene conductive membrane electrode, forms left and right metal electrode 4,5.
The preparation of step 4 horizontal structure ultracapacitor
As the ultracapacitor collector electrode, left and right graphene conductive membrane electrode 2,3 is the left and right electrode of ultracapacitor with left and right metal electrode 4,5, and mass ratio is 0.2: 1: 0.2 polytetrafluoroethylene adhesive, LiClO
4The mixture that conductive agent, phthalate plasticizers are formed is filled between the left and right graphene conductive membrane electrode (2,3) and peripheral part as solid electrolyte, and specific capacity can reach 263 μ F/cm
2
A kind of preparation method of graphene-based horizontal structure ultracapacitor four with one of preparation method of a kind of graphene-based horizontal structure ultracapacitor difference for blade gash on resulting graphene oxide film surface stroke; Again graphene oxide film is placed on to handle under the reducing environment together with substrate and obtains graphene film; Measure the tool marks both sides with universal instrument and be in open-circuit condition, obtain left and right graphene conductive membrane electrode.
The capacity curve of the graphene-based horizontal structure ultracapacitor of Fig. 2.It is thus clear that the specific capacity of capacitor increases along with the increase of film thickness, film is unfavorable for the raising of device performance when too thick from curve.
Claims (7)
1. graphene-based horizontal structure ultracapacitor is characterized in that:
Go up sequentially built left side graphene conductive membrane electrode (2), right graphene conductive membrane electrode (3), left metal electrode (4), right metal electrode (5) at substrate (1), fill solid-state electrolyte layer (6) between left graphene conductive membrane electrode (2), the right graphene conductive membrane electrode (3).
2. the preparation method of a graphene-based horizontal structure ultracapacitor is characterized in that:
The preparation method of this horizontal structure ultracapacitor may further comprise the steps:
The preparation of step 1 graphene oxide film
It is 0.01～1% aqueous dispersions that graphene oxide is processed mass concentration;
With this dispersion liquid through drop-coating, vertical deposition method, dip-coating method or layer by layer self-assembling method deposit on the substrate (1), under 25 ℃～100 ℃, obtain graphene oxide film after the drying;
The preparation of step 2 graphene conductive membrane electrode
Above-mentioned graphene oxide film is placed under the reducing environment together with substrate handles, obtain graphene film; Draw one gash with blade on resulting graphene film surface, measure the tool marks both sides with universal instrument and be in open-circuit condition, obtain left and right graphene conductive membrane electrode;
Or draw one gash on resulting graphene oxide film surface with blade; Again graphene oxide film is placed on to handle under the reducing environment together with substrate and obtains graphene film; Measure the tool marks both sides with universal instrument and be in open-circuit condition, obtain left and right graphene conductive membrane electrode;
The preparation of step 3 metal electrode
The cut and the cut that block graphene conductive membrane electrode in the step 2 with mask plate are peripheral, are exposing a part near the film edge place; Utilize the exposed part vapor deposition left and right metal electrode (4,5) of vacuum thermal evaporation filming equipment at above-mentioned graphene conductive membrane electrode;
The preparation of step 4 horizontal structure ultracapacitor
With left and right metal electrode (4,5) as the ultracapacitor collector electrode; Left and right graphene conductive membrane electrode (2,3) is the left and right electrode of ultracapacitor; Between left and right graphene conductive membrane electrode (2,3), fill solid-state electrolyte layer (6), make graphene-based horizontal structure ultracapacitor.
3. the preparation method of a kind of graphene-based horizontal structure ultracapacitor according to claim 2 is characterized in that:
In the described step 1, when adopting vertical deposition method to prepare graphene oxide film, substrate (1) is placed on graphene oxide, and to process mass concentration be in 0.01～1% the aqueous dispersions, and with the horizontal direction angle be 10 °～80 °.
4. the preparation method of a kind of graphene-based horizontal structure ultracapacitor according to claim 2 is characterized in that:
The preparation of the graphene conductive membrane electrode in the described step 2 forms the employed instrument of open circuit and does not limit, and the cut width is less than 2 μ m.
5. the preparation method of a kind of graphene-based horizontal structure ultracapacitor according to claim 2 is characterized in that:
The preparation of described metal electrode, the shape of exposed part and the cut that blocked thereof periphery area is unrestricted on the mask plate.
6. the preparation method of a kind of graphene-based horizontal structure ultracapacitor according to claim 2 is characterized in that:
In the step 1, the thickness of graphene oxide film is 10～1000nm.
7. the preparation method of a kind of graphene-based horizontal structure ultracapacitor according to claim 2 is characterized in that:
In the step 1, substrate (1) is simple glass substrate, quartz substrate.
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| CN104681299A (en) * | 2015-03-27 | 2015-06-03 | 吉林化工学院 | Supercapacitor electrode material of cobaltosic oxide porous nanowire array, and preparation method thereof |
| CN107848804A (en) * | 2015-03-06 | 2018-03-27 | 悉尼科技大学 | Technique, structure and ultra-capacitor |
| CN109626316A (en) * | 2018-12-17 | 2019-04-16 | 广西大学 | A kind of D structure graphene nano power generator and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107848804A (en) * | 2015-03-06 | 2018-03-27 | 悉尼科技大学 | Technique, structure and ultra-capacitor |
| CN107848804B (en) * | 2015-03-06 | 2020-11-06 | 悉尼科技大学 | Process, structure and supercapacitor |
| CN104681299A (en) * | 2015-03-27 | 2015-06-03 | 吉林化工学院 | Supercapacitor electrode material of cobaltosic oxide porous nanowire array, and preparation method thereof |
| CN104681299B (en) * | 2015-03-27 | 2017-11-14 | 吉林化工学院 | Electrode material for super capacitor of cobaltosic oxide porous nano linear array and preparation method thereof |
| CN109626316A (en) * | 2018-12-17 | 2019-04-16 | 广西大学 | A kind of D structure graphene nano power generator and preparation method thereof |
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Application publication date: 20120627 |