CN105417528A - Preparation methods for fluorinated graphene hydrogel material and electrodes thereof - Google Patents

Preparation methods for fluorinated graphene hydrogel material and electrodes thereof Download PDF

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Publication number
CN105417528A
CN105417528A CN201510915294.5A CN201510915294A CN105417528A CN 105417528 A CN105417528 A CN 105417528A CN 201510915294 A CN201510915294 A CN 201510915294A CN 105417528 A CN105417528 A CN 105417528A
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fluorinated graphene
graphene hydrogel
deionized water
solution
hydrofluoric acid
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封伟
安浩然
李瑀
冯奕钰
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Tianjin University
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Tianjin University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • 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 relates to preparation methods for a fluorinated graphene hydrogel material and electrodes thereof. The preparation method for the fluorinated graphene hydrogel material comprises the steps that an aqueous graphene oxide solution with the concentration of 0.5-2.0 mg/mL is added into a polytetrafluoroethylene hydrothermal reaction kettle, then a hydrofluoric acid solution is added, the volume ratio of the aqueous graphene oxide solution to the hydrofluoric acid solution is (50-12.5):1, the materials are mixed to be uniform, and then the reaction kettle is covered and sealed; the reaction kettle is put into a muffle furnace, and reacting is performed for 6-24 h at the temperature of 120 DEG C-180 DEG C; a product is taken out and then immersed into deionized water to obtain the fluorinated graphene hydrogel. The preparation method for the electrode material comprises the steps that the fluorinated graphene hydrogel is cut into slices with the thickness of 1-5 mm, the slices are wrapped with filter paper, redundant moisture is removed, and then the fluorinated graphene hydrogel electrode material is obtained. According to the preparation methods, operation is easy, the cost is low, the yield is high, the mass specific capacitance under the electric current density of 1 A g<-1> in a three-electrode system is 220 F g<-1>, and the energy density of the electrode material in a double-electrode system can reach 5.0 Wh kg<-1> or above.

Description

Fluorinated graphene hydrogel material and electrode preparation method thereof
Technical field
The present invention relates to a kind of fluorinated graphene hydrogel material and electrode preparation method thereof, specifically a kind of have the preparation method of the fluorinated graphene of hydrogel structure and the application on ultracapacitor thereof, belongs to energy storage material technical field.
Background technology
Fluorinated graphene is the new derivatives of Graphene, is a kind of two-dimensional material.Owing to having power, heat, sound, the optical and electrical properties of high temperature resistant, excellent chemical stability and uniqueness, be widely used at energy field, such as high-energy-density lithium primary battery positive electrode material, lithium ion battery negative material, dye sensitization solar battery, to electrode, stores up hydrogen catalyst and fuel cell redox reaction catalyzer etc.
Ultracapacitor, as a kind of energy storage device, owing to having high power density and cyclical stability well, is widely used at electromobile, the field such as electric installation and backup power source.Graphene and derivative thereof are due to its excellent electroconductibility, and larger specific surface area and excellent chemical stability are considered to the desirable electrode materials of ultracapacitor.The energy-storage property of graphene-based material can by hindering the self-assembly of graphene nanometer sheet, and the mode building three-dimensional structure such as hydrogel obtains raising.Hydrogel structure not only can remove subsequent extracted step in preparation process but also its distinctive vesicular structure make its can with multiple material compound.
Fluorinated graphene can be made by Graphene and the reaction of highly active fluoro-gas, but this method needs the gas fluorine source of complex apparatus process severe toxicity and highly corrosive, limits its widespread use.And by peel off fluorographite method fluorinated graphene output little, and degree of fluorination is determined by the fluorographite selected, and can not regulate and control easily.In former work, fluorinated graphene does not show gratifying performance as electrode material for super capacitor, and mostly the electrode materials of preparation is that powder type exists, preparing in electrode process the filler needing to add the reduction such as binding agent, conductive agent chemical property.And the electrode materials of hydrogel structure is without the need to using the fillers such as binding agent.The fluorinated graphene electrode materials of current hydrogel structure was not reported.Therefore develop a kind of preparation method with the fluorinated graphene electrode materials of hydrogel structure and seem particularly important.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide preparation to have fluorinated graphene material and the electrode preparation method thereof of hydrogel structure, the method is simple to operate, quick environmental protection.The fluorinated graphene material of preparation has three dimensional hydrogel structure, and have excellent chemical property with the electrode materials that it is prepared, the advantages such as good cyclical stability, are applicable to as electrode material for super capacitor.
Technical scheme of the present invention provides a kind of preparation method of fluorinated graphene hydrogel material, is achieved through the following technical solutions:
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 0.5-2.0mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio 50 ~ 12.5:1, mix, build sealing;
(2) reactor in (1) is put into retort furnace, in 120-180 DEG C, react 6-24h;
(3) taken out by the product obtained in (2) and immerse in deionized water, deionized water is changed in timing, until deionized water is to neutral, obtains fluorinated graphene hydrogel.
In described step (1) hydrofluoric acid to be massfraction be 40% the HF aqueous solution;
Deionized water is changed in described timing, can spend the night or change a deionized water every 24 hours.
The method of electrode is prepared with fluorinated graphene hydrogel material:
(1) fluorinated graphene hydrogel is cut into the sheet that thickness is 1-5mm, removes excessive moisture with filter paper parcel and obtain fluorinated graphene hydrogel electrode materials.
(2) the fluorinated graphene hydrogel electrode materials that obtain in (1) is infiltrated 5h in electrolyte system, after fully infiltrating under three electrodes and two electrodes system in test performance, electrolytic solution is 6molL -1kOH solution.
The present invention is simple to operate, and cost is low, and output is high, and aftertreatment is simple, and do not need special reaction kit, preparation cost is cheap.Can by simply regulating and controlling the degree of fluorination that reaction solution concentration, temperature of reaction time etc. control fluorinated graphene hydrogel easily; In addition, the fluorinated graphene hydrogel obtained can be prepared into electrode by direct slicing, compared with other powdered materials, does not need to use binding agent and conductive agent, and obtained electrode materials has higher capacitive property and excellent cyclical stability, 1Ag under three-electrode system -1under current density, quality is 220Fg than electric capacity -1, at 100Ag -1high current density under capacity still up to 120Fg -1, at 2Ag -1the 2000 circle capability retentions that circulate under current density are 95.1%, and in two electrodes system, its energy density can reach 5.0Whkg -1above, power density can reach 50kWkg -1above.
Accompanying drawing explanation
Fig. 1 is the optical photograph of the fluorinated graphene hydrogel that example 1 prepares;
Fig. 2 is the electron scanning micrograph of the fluorinated graphene hydrogel material that example 1 prepares;
Fig. 3 is the x-ray photoelectron energy spectrogram of the fluorinated graphene hydrogel material that example 1 prepares;
Fig. 4 is the cyclic voltammetry curve figure of the fluorinated graphene hydrogel electrode prepared;
Fig. 5 is the charging and discharging curve of the fluorinated graphene hydrogel electrode prepared.
Specific embodiments
Below by way of specific embodiment, technical solution of the present invention is described.
The graphene oxide used in an embodiment is prepared as follows: by natural flake graphite 2g, NaNO 32g, dense H 2sO 496mL puts into round-bottomed flask, is uniformly mixed at 0 DEG C, backward mixture in add 12gKMnO 4, 0 DEG C is stirred 90min, reacts 2h, then in mixture, drip 80mL deionized water at rising to 35 DEG C.After dropwising, then add 200mL deionized water and 10mLH successively in mixture 2o 2(30%), stir 10min, remove acid and water miscible ion by washing, be washed to neutrality and obtain graphite oxide slurry.Be dispersed in water after graphite oxide pulp dilution.Centrifugal for dispersion liquid precipitation to be dispersed in water is obtained graphene oxide solution.
The graphene oxide used in an embodiment also can use commercially available prod.
One, the preparation of fluorinated graphene hydrogel material:
Example 1
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 0.5mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio are 50:1:, mix, build sealing.
(2) reactor in (1) is put into retort furnace, in 120 DEG C, react 24h.
(3) product obtained in (2) taken out and immerse in deionized water, changing a deionized water every 24 hours, until deionized water is to neutral, obtaining fluorinated graphene hydrogel.
In described step (1) hydrofluoric acid to be massfraction be 40% the HF aqueous solution;
Fluorinated graphene hydrogel size prepared by example 1 is about the right cylinder (as shown in Figure 1) of high 2cm diameter 1.5cm.
The scanning electronic microscope of fluorinated graphene hydrogel prepared by example 1 demonstrates material and is made up of stacking being cross-linked of a large amount of nanometer sheet, the pattern (as shown in Figure 2) of the many folds of shape porous.
In fluorinated graphene hydrogel x-ray photoelectron power spectrum prepared by example 1, display is containing C, O, F element, not containing other elements (as shown in Figure 3).
Example 2
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 2.0mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio are 12.5:1:, mix, build sealing.
(2) reactor in (1) is put into retort furnace, in 150 DEG C, react 6h.
(3) product obtained in (2) taken out and immerse in deionized water, changing a deionized water every 24 hours, until deionized water is to neutral, obtaining fluorinated graphene hydrogel.
In described step (1) hydrofluoric acid to be massfraction be 40% the HF aqueous solution;
Example 3
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 1.0mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio are 25:1, mix, build sealing.
(2) reactor in (1) is put into retort furnace, in 180 DEG C, react 12h.
(3) product obtained in (2) taken out and immerse in deionized water, changing a deionized water every 24 hours, until deionized water is to neutral, obtaining fluorinated graphene hydrogel.
In described step (1) hydrofluoric acid to be massfraction be 40% the HF aqueous solution;
Example 4
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 1.5mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio 30:1, mix, build sealing.
(2) reactor in (1) is put into retort furnace, in 180 DEG C, react 18h.
(3) product obtained in (2) taken out and immerse in deionized water, changing a deionized water every 24 hours, until deionized water is to neutral, obtaining fluorinated graphene hydrogel.
In described step (1) hydrofluoric acid to be massfraction be 40% the HF aqueous solution;
Two, the fluorinated graphene hydrogel material adopting above-mentioned any embodiment to prepare prepares electrode:
Example 5
(1) fluorinated graphene hydrogel is cut into the sheet that thickness is 1mm, removes excessive moisture with filter paper parcel and obtain fluorinated graphene hydrogel electrode materials.
(2) the fluorinated graphene hydrogel electrode materials that obtain in (1) is infiltrated 5h in electrolyte system, after fully infiltrating under three electrodes and two electrodes system in test performance, electrolytic solution is 6molL -1kOH solution.
Demonstrate more excellent chemical property by the cyclic voltammetry curve figure of the fluorinated graphene hydrogel electrode of preparation, voltage window is-1.2V to-0.2V, and scanning speed is 5mVs -1to 100mVs -1as shown in Figure 4.
Display in the charging and discharging curve of the fluorinated graphene hydrogel electrode of preparation can be realized under high charge-discharge electric current the storage of energy, at 1Ag -1current density can reach more than 220 seconds as shown in Figure 4 lower discharge time.
Example 6
(1) fluorinated graphene hydrogel is cut into the sheet that thickness is 5mm, removes excessive moisture with filter paper parcel and obtain fluorinated graphene hydrogel electrode materials.
(2) the fluorinated graphene hydrogel electrode materials that obtain in (1) is infiltrated 5h in electrolyte system, after fully infiltrating under three electrodes and two electrodes system in test performance, electrolytic solution is 6molL -1kOH solution.
Example 7
(1) fluorinated graphene hydrogel is cut into the sheet that thickness is 3mm, removes excessive moisture with filter paper parcel and obtain fluorinated graphene hydrogel electrode materials.
(2) the fluorinated graphene hydrogel electrode materials that obtain in (1) is infiltrated 5h in electrolyte system, after fully infiltrating under three electrodes and two electrodes system in test performance, electrolytic solution is 6molL -1kOH solution.
The present invention is open and propose a kind of fluorinated graphene hydrogel and electrode materials preparation method thereof, those skilled in the art are by using for reference present disclosure, the links such as appropriate change condition route realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change Method and Technology route as herein described or reconfigure not departing from content of the present invention, spirit and scope, realizes final technology of preparing.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.

Claims (4)

1. a preparation method for fluorinated graphene hydrogel material, is characterized in that step is as follows:
(1) in tetrafluoroethylene hydrothermal reaction kettle, add the graphene oxide water solution of 0.5-2.0mg/mL, then add hydrofluoric acid solution, graphene oxide water solution and hydrofluoric acid solution volume ratio 50 ~ 12.5:1, mix, build sealing;
(2) reactor in (1) is put into retort furnace, in 120-180 DEG C, react 6-24h;
(3) taken out by the product obtained in (2) and immerse in deionized water, deionized water is changed in timing, until deionized water is to neutral, obtains fluorinated graphene hydrogel.
2. the method for claim 1, is characterized in that hydrofluoric acid in described step (1) to be massfraction is the HF aqueous solution of 40%.
3. the method for claim 1, is characterized in that deionized water is changed in described timing, for spending the night or changing a deionized water every 24 hours.
4. prepare the method for electrode with fluorinated graphene hydrogel material, it is characterized in that step is as follows:
(1) fluorinated graphene hydrogel is cut into the sheet that thickness is 1-5mm, removes excessive moisture with filter paper parcel and obtain fluorinated graphene hydrogel electrode materials;
(2) the fluorinated graphene hydrogel electrode materials that obtains in (1) is infiltrated in electrolyte system, after fully infiltrating under three electrodes and two electrodes system in test performance, electrolytic solution is 6molL -1kOH solution.
CN201510915294.5A 2015-12-09 2015-12-09 Preparation methods for fluorinated graphene hydrogel material and electrodes thereof Pending CN105417528A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108264036A (en) * 2018-03-29 2018-07-10 中国科学院福建物质结构研究所 A kind of preparation method of fluorine graphene oxide
CN114408906A (en) * 2022-03-15 2022-04-29 枣庄市三兴高新材料有限公司 Method for purifying coal-based graphite and simultaneously preparing fluorinated graphene

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103153848A (en) * 2010-12-22 2013-06-12 海洋王照明科技股份有限公司 Fluorographene and preparation method thereof
CN103288069A (en) * 2013-05-10 2013-09-11 西北工业大学 Method for preparing fluorinated graphene through microwave hydrothermal method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103153848A (en) * 2010-12-22 2013-06-12 海洋王照明科技股份有限公司 Fluorographene and preparation method thereof
CN103288069A (en) * 2013-05-10 2013-09-11 西北工业大学 Method for preparing fluorinated graphene through microwave hydrothermal method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108264036A (en) * 2018-03-29 2018-07-10 中国科学院福建物质结构研究所 A kind of preparation method of fluorine graphene oxide
CN114408906A (en) * 2022-03-15 2022-04-29 枣庄市三兴高新材料有限公司 Method for purifying coal-based graphite and simultaneously preparing fluorinated graphene

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