CN105826083B - A kind of preparation of graphene-based electrode material and the construction method of capacitor - Google Patents

A kind of preparation of graphene-based electrode material and the construction method of capacitor Download PDF

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CN105826083B
CN105826083B CN201610248510.XA CN201610248510A CN105826083B CN 105826083 B CN105826083 B CN 105826083B CN 201610248510 A CN201610248510 A CN 201610248510A CN 105826083 B CN105826083 B CN 105826083B
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邵姣婧
陈祥荣
罗顺
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Guizhou University
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    • 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 present invention provides a kind of preparation method of graphene-based electrode material, is 0.5 2 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic agitation or manually rock 0.5 1h, obtain A product；A product stand 0.5 1h at a temperature of 60 80 DEG C, until graphene oxide hydrosol surface forms complete graphene oxide film, obtain B product；By the use of fexible film as matrix, B product are deposited on matrix, are dried, obtain C product；The iodate hydrogen solution that mass fraction is 55 58% is added to C kinds, 3 48h are reduced at 15 80 DEG C, cleans, obtains D product；D product are put into the potassium permanganate of 0.5 5mmol/L and soak 5 48h, cleans, obtains E product, the graphene/Mn oxide laminated film being deposited on to obtain the final product on flexible substrate.The graphene-based electrode material can be easy to operate directly as the electrode material of flexible film super capacitor, takes that short, consumptive material is few, environmentally friendly, while also has good bending property.It is and good with the capacitor chemical property that the electrode material is built.

Description

A kind of preparation of graphene-based electrode material and the construction method of capacitor
Technical field
The present invention relates to a kind of preparation of graphene-based flexible super capacitor electrode material and the construction method of capacitor, The preparation of the graphene-based film electrode material for super capacitor of particularly a kind of plane based on gas-liquid interface construction from part and electricity The construction method of container.
Background technology
Due to the development of wearable electronic device, requirement of the people to flexible energy storage device also gradually increases, flexible super Therefore capacitor also receives much concern.Wherein, based on the flexible super capacitance of two-dimensional film electrode with its lightweight, miniaturization, bendable The features such as bent, particularly attractive attention.Graphene is as a kind of two-dimensional nano-carbon material, its carbon atom is with sp2Hydridization side Formula forms the cellular planar structure of hexatomic ring, it has the electron mobility (200,000cm of superelevation2/ V.s), greatly compare table Area (2630m2/ g), good heat conductivility (5300W/mK) and excellent mechanical strength (40N/m fracture strengths, 1TPa Young's modulus), it is a kind of preferable electrode material for super capacitor.It is huge that graphene two-dimensional nano lamellar structure imparts it The ratio of width to height (aspect ratio), can be assembled into Flexible graphene film by stacked in multi-layers, form film assembling If another nano material is reasonably introduced in, can then obtain the graphene-based laminated film of flexibility.
At present, have assembling and the preparation process of many document reports graphene-based flexible film, this is based on structure The flexible super capacitor of graphene membrane electrode has established good working foundation.Wherein, vacuum filtration method and chemical gaseous phase Sedimentation is to prepare the common technology of graphene film, but the obtained graphene film of these methods is generally all deposited on firmly Matter matrix (such as：Woelm Alumina filter membrane, copper foil, silicon chip) on, therefore cannot be directly as flexible film super capacitor Electrode material, and the graphene film being deposited on hard substrate must be transferred to by flexibility by cumbersome matrix transfer step Matrix (such as：Dimethyl silicone polymer (Polydimethylsiloxane, PDMS) or polyethylene terephthalate On (Poly (ethylene terephthalate), PET), matrix transfer process usually requires to etch away hard substrate, institute The flexible substrate of use is typically polymeric matrix, and being eventually deposited at graphene film on polymeric matrix can be directly as The electrode material of flexible super capacitor；In addition, chemical vapour deposition technique is commonly used for preparing pure graphene film, it is difficult to is used for Prepare graphene-based laminated film.Its configuration of flexible super capacitor based on graphene membrane electrode mainly includes tradition " three Mingzhi " configuration and plane configuration, wherein plane configuration be more advantageous to ultracapacitor volume miniaturization and thickness of detector most Smallization.Multi-layer graphite is deposited in quartz substrate and copper foil surface respectively using LBL self-assembly and chemical vapour deposition technique Alkene film and single-layer graphene film, and two kinds of graphene membrane electrode design constructions plane ultracapacitor is based on, two The good chemical property that kind plane ultracapacitor is shown, its area specific capacity is respectively 394 μ F/cm2With 80 μ F/ cm2。(J.J.Yoo,K.Balakrishnan,J.Huang,et al.Nano Letters 2011,11,(4),1423- 1427.) however, LBL self-assembly prepares graphene film usually requires to utilize positively charged nano material and negatively charged Graphene oxide solution, using electrostatic adelphotaxy between the two, is repeatedly received matrix at two kinds as presoma Immerse-cleaning-cyclic process dried in rice material solution, until reach required film thickness, therefore layer by layer from group The relatively time consuming complexity of dress process, and the graphene film obtained is often laminated film；Though chemical vapor deposition processes So there is significant advantage in terms of pure graphene film is prepared, but its preparation process be related to high temperature high fever so some consumed energy Journey, and it is difficult to the controllable preparation that a step realizes graphene-based laminated film.It is discussed above to prepare graphene-based film Two kinds of common methods, its most critical issue are that the graphene film obtained by two methods is deposited directly upon hard substrate On, flexible super capacitor can not be directly applied to, could be by obtained graphite only by complicated matrix transfer step The transfer of alkenyl film is deposited on flexible substrate, however, film to be transferred to this transfer on flexible substrate from hard substrate Step needs to dissolve hard substrate using severe corrosive reagent, and whole process is very time-consuming, consumptive material, not environmentally.
The content of the invention
It is an object of the present invention to provide a kind of preparation of graphene-based electrode material and the construction method of capacitor.Institute The graphene-based electrode material prepared can be easy to operate directly as the electrode material of flexible film super capacitor, take it is short, Consumptive material is few, environmentally friendly, while also has good bending property, and pliability is good.And the plane built with electrode material of the present invention Ultracapacitor chemical property is good, and area specific capacity exists
1000μF/cm2More than, plane flexible super capacitor can be not only built, traditional Sanming City can also be built Type flexible super capacitor is controlled, while is also beneficial to the miniaturization of device and lightening.
The present invention is realized using following technical scheme：A kind of preparation method of graphene-based electrode material, including following step Suddenly：
1st, it is 0.5-2 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, stir Mix, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtain A product；
2nd, A product stand 0.5-1h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxygen Graphite alkene film, obtains B product；
3rd, B product are deposited on the flexible substrate, are dried, obtain C product as matrix, i.e. flexible substrate using fexible film；
4th, the iodate hydrogen solution that mass fraction is 55-58% is added into C product, 3-48h is reduced at 15-80 DEG C, through second Alcohol and distilled water cleaning, obtain D product；
5th, D product are put into the potassium permanganate of 0.5-5mmol/L and soak 5-48h, cleaned through ethanol and distilled water, obtain E product, Graphene/Mn oxide the laminated film being deposited on to obtain the final product on flexible substrate.
The preparation method of foregoing graphene-based electrode material, the graphite oxide described in step 1 carry out in the steps below Prepare：
A. it is 1 in mass ratio by potassium peroxydisulfate and phosphorus pentoxide:After 1 mixing, at 75-85 DEG C, by potassium peroxydisulfate：It is dense H2SO4For 15g：The ratio of 80-150ml adds dense H2SO4, 20-30min is stirred, until solution is limpid, obtains mixed solution；To mixed Close in solution and add graphite powder, stir 4-5h under 75-85 DEG C of water bath condition, be cooled to room temperature, continue to add into mixed solution Enter deionized water, the solid sample in mixed solution is cleaned and collected by vacuum filtration method, using going during vacuum filtration Ionized water cleaning sample, until filtrate is neutrality, the solid sample filtered after cleaning is dried, the stone pre-oxidized Ink powder end；
B. the powdered graphite pre-oxidized adds dense H2SO4In, stirred evenly under the conditions of 0-5 DEG C of ice-water bath, into solution Potassium permanganate powder is slowly added to, after then stirring 3-5h under 30-40 DEG C of water-bath, then continues to stir in 0-5 DEG C of ice-water bath 10-20min is mixed, is slow added into deionized water, continues to stir 2-3h, it is molten to add the hydrogen peroxide that mass fraction is 30% Liquid, it is stirring while adding, 12h is stood after adding, collects solid sample, the dilute hydrochloric acid solution for being 4-5% with mass fraction cleans, instead Multiple eccentric cleaning, untill the pH value of cleaning solution is changed into neutrality, then is dried in vacuo 45-50h, up to graphite oxide powder.
The preparation method of foregoing graphene-based electrode material, by graphite oxide and the mass ratio of deionized water in step 1 For 1:1000 add graphite oxide into deionized water.
The preparation method of foregoing graphene-based electrode material, time of repose is 0.8h in step 2.
The preparation method of foregoing graphene-based electrode material, the recovery time is 28h in step 4.
The preparation method of foregoing graphene-based electrode material, step 5 are that D product are put into the potassium permanganate of 3mmol/L 28h is soaked, obtains E product, the graphene/Mn oxide laminated film being deposited on to obtain the final product on flexible substrate.
The preparation method of foregoing graphene-based electrode material, the fexible film are polyethylene terephthalate, That is PET matrix or dimethyl silicone polymer, i.e. PDMS matrixes.
The preparation method of foregoing graphene-based electrode material, the dense H2SO4Mass fraction be 98%.
The invention has the advantages that：
1st, prepared graphene-based electrode material can be not required to directly as the electrode material of flexible film super capacitor Cumbersome matrix transfer step is wanted, is not related to the energy consumption process such as high temperature and pressure, it is not required that complicated LBL self-assembly process, consumption When it is short, consumptive material is few, environmentally friendly.
2nd, electrode material of the present invention builds to obtain capacitor.Obtained capacitor has the property of general flexible super capacitor Can, chemical property is good, and area specific capacity is in 1000 μ F/cm2More than, flexible storage can be used as in wearable electronic devices field Can component use.
3rd, prepared graphene-based electrode material has good bending property, is found through experiment, the graphene-based electricity Pole material still maintains fabulous integrality in the rear film for undergoing 1000 bendings.Plane flexible super can not only be built Capacitor, can also build traditional sandwich type flexible super capacitor.
4th, the present invention using air liquid interface assemble come when by the use of flexiplast as matrix, it is not necessary to by unsupported stone Mertenyl thin-film package is inside flexiplast matrix.
5th, the miniaturization of device and lightening is conducive to.The general graphite directly filtered using graphene aqueous dispersions Alkene film, film are thicker.The present invention is with the graphene oxide film obtained with air liquid interface construction from part, then the institute after reduction The thickness of obtained graphene-based film only has tens to hundreds of nanometers.
6th, the graphite oxide that the method for the present invention prepares gained has higher degree of oxidation, has excellent water solubility, no Need ultrasonic wave added that graphite oxide can be made to disperse to form homogeneous phase aqueous solution in aqueous, be conducive to obtain the oxidation of big lamella Graphene sheet layer, helps to reduce the interior resistance of graphene-based flexible membrane electrode made from the later stage.
The present invention is further illustrated by the following examples, but not as limitation of the present invention
Embodiment
Embodiment 1.
A kind of preparation method of graphene-based electrode material, comprises the following steps：
1st, it is 1 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic force 0.8h is manually rocked in stirring, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtains A product；
2nd, A product stand 0.8h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation Graphene film, obtains B product；
3rd, B product are deposited on the matrix, are dried, obtain C product as matrix using fexible film；The fexible film is Polyethylene terephthalate, i.e. PET matrix；
4th, the iodate hydrogen solution that mass fraction is 57%, the reductase 12 8h at 15-80 DEG C, through ethanol and steaming are added to C kinds Distilled water is cleaned, and obtains D product；
5th, D product are put into the potassium permanganate of 3mmol/L and soak 28h, cleaned through ethanol and distilled water, obtain E product, up to heavy Graphene/Mn oxide laminated film of the product on flexible substrate.
Graphite oxide described in step 1 is prepared in the steps below：
A. by 15g potassium peroxydisulfates and 15g phosphorus pentoxides P2O5It is added in the round bottom beaker of 550mL, in 75-85 DEG C of water The dense H of 115mL is added under bath temperature2SO4, make mixed solution mixing 25min under magnetic stirring, mixed solution becomes limpid；Will 22g powdered graphites are added in solution mixed above, it is stirred 4.5h under 75-85 DEG C of water bath condition, afterwards will mixing Solution temperature is slowly lowered to room temperature, is then slowly added 1.7L deionized waters, will finally be mixed using vacuum filtration method molten Solid sample in liquid is cleaned and collected, and deionized water cleaning sample is used during vacuum filtration, until filtrate is neutrality, The solid sample filtered after cleaning is dried, the powdered graphite pre-oxidized；
B. the 750mL concentrated sulfuric acids are added into the powdered graphite of pre-oxidation, are stirred under the conditions of 0-5 DEG C of ice-water bath It is even, then 100g potassium permanganate powders are slowly added into flask, after treating that potassium permanganate powder adds, obtain reaction solution；Reaction Liquid is transferred in 35-40 DEG C of water bath, is continued after being stirred 4h, and reaction solution, which is transferred in 0-5 DEG C of ice-water bath, to be continued to stir Mix, then slowly add the deionized water of 750mL into reaction solution, and stirring 2.5h is continued under the conditions of ice-water bath；By 40mL matter The hydrogenperoxide steam generator that amount fraction is 30% is added in reaction solution, stirring while adding, is added rear reaction solution and is stood 12h, collects Deposit to the solid sample of drag, then use vacuum filtration method by the solid sample of collection with 3L mass fractions for 4.5% dilute hydrochloric acid solution filtering cleaning is finally centrifuged repeatedly cleaning sample to react away the manganese dioxide impurity in solid sample Product are untill the pH value of cleaning solution is changed into neutrality, and most product carries out vacuum drying 48h at last, and 20-30 DEG C of drying temperature obtains Graphite oxide powder；The dense H2SO4Mass fraction be 98%.
Embodiment 2.
A kind of preparation method of graphene-based electrode material, comprises the following steps：
1st, it is 2 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic force 1h is manually rocked in stirring, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtains A product；
2nd, A product stand 1h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation stone Black alkene film, obtains B product；
3rd, B product are deposited on the matrix, are dried, obtain C product as matrix using fexible film；The fexible film is Dimethyl silicone polymer, i.e. PDMS matrixes；
4th, the iodate hydrogen solution that mass fraction is 58% is added to C kinds, 48h is reduced at 15-80 DEG C, through ethanol and steaming Distilled water is cleaned, and obtains D product；
5th, D product are put into the potassium permanganate of 5mmol/L and soak 48h, cleaned through ethanol and distilled water, obtain E product, up to heavy Graphene/Mn oxide laminated film of the product on flexible substrate.
The preparation method of graphite oxide described in step 1 is the same as embodiment 1.
Embodiment 3.
A kind of preparation method of graphene-based electrode material, comprises the following steps：
1st, it is 0.5 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic Power stirs or manually rocks 0.5h, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtains A product；
2nd, A product stand 0.5h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation Graphene film, obtains B product；
3rd, B product are deposited on the matrix, are dried, obtain C product as matrix using fexible film；The fexible film is Polyethylene terephthalate, i.e. PET matrix；
4th, the iodate hydrogen solution that mass fraction is 55% is added to C kinds, 3h is reduced at 15-80 DEG C, through ethanol and steaming Distilled water is cleaned, and obtains D product；
5th, D product are put into the potassium permanganate of 0.5mmol/L and soak 5h, cleaned through ethanol and distilled water, obtain E product, to obtain the final product Graphene/Mn oxide the laminated film being deposited on flexible substrate.
The preparation method of graphite oxide described in step 1 is the same as embodiment 1.
Embodiment 4.
A kind of preparation method of graphene-based electrode material, comprises the following steps：
1st, it is 1.7 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic Power stirs or manually rocks 0.9h, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtains A product；
2nd, A product stand 0.9h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation Graphene film, obtains B product；
3rd, B product are deposited on the matrix, are dried, obtain C product as matrix using fexible film；The fexible film is Dimethyl silicone polymer, i.e. PDMS matrixes.
4th, add the iodate hydrogen solution that mass fraction is 57% to C kinds, 3-48h reduced at 15-80 DEG C, through ethanol and Distilled water cleans, and obtains D product；
5th, D product are put into the potassium permanganate of 4mmol/L and soak 40h, cleaned through ethanol and distilled water, obtain E product, up to heavy Graphene/Mn oxide laminated film of the product on flexible substrate.
The preparation method of graphite oxide described in step 1 is the same as embodiment 1.
Embodiment 5.
A kind of preparation method of graphene-based electrode material, comprises the following steps：
1st, it is 0.9 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, in magnetic Power stirs or manually rocks 0.6h, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtains A product；
2nd, A product stand 0.6h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation Graphene film, obtains B product；
3rd, B product are deposited on the matrix, are dried, obtain C product as matrix using fexible film；The fexible film is Polyethylene terephthalate, i.e. PET matrix.
4th, the iodate hydrogen solution that mass fraction is 56% is added to C kinds, 10h is reduced at 15-80 DEG C, through ethanol and steaming Distilled water is cleaned, and obtains D product；
5th, D product are put into the potassium permanganate of 1mmol/L and soak 10h, cleaned, obtain through ethanol and distilled water
E product, the graphene/Mn oxide laminated film being deposited on to obtain the final product on flexible substrate.
The preparation method of graphite oxide described in step 1 is the same as embodiment 1.

Claims (7)

  1. A kind of 1. preparation method of graphene-based electrode material, it is characterised in that：Comprise the following steps：
    （1）It is 0.5-2 by graphite oxide and the mass ratio of deionized water:1000 add graphite oxide into deionized water, stirring, Until solution is to stablize homogeneous graphene oxide hydrosol solution, A product are obtained；
    （2）A product stand 0.5-1h at a temperature of 60-80 DEG C, until graphene oxide hydrosol surface forms complete oxidation stone Black alkene film, obtains B product；
    （3）Using fexible film as matrix, i.e. flexible substrate, B product are deposited on the flexible substrate, are dried, obtain C product；
    （4）The iodate hydrogen solution that mass fraction is 55-58% is added into C product, 3-48h is reduced at 15-80 DEG C, through ethanol and After distilled water cleaning, D product are obtained；
    （5）D product are put into the potassium permanganate of 0.5-5mmol/L and soak 5-48h, after ethanol and distilled water cleaning, obtain E Product, the graphene/Mn oxide laminated film being deposited on to obtain the final product on flexible substrate；Step（1）Described in graphite oxide press Step is stated to be prepared：
    A. it is 1 in mass ratio by potassium peroxydisulfate and phosphorus pentoxide:After 1 mixing, at 75-85 DEG C, by potassium peroxydisulfate：Dense H2SO4 For 15g：The ratio of 80-150ml adds dense H2SO4, 20-30min is stirred, until solution is limpid, obtains mixed solution；It is molten to mixing Graphite powder is added in liquid, 4-5h is stirred under 75-85 DEG C of water bath condition, is cooled to room temperature, continues to add into mixed solution and goes Solid sample in mixed solution is cleaned and collected by ionized water, vacuum filtration method, and deionization is used during vacuum filtration Water cleaning sample, until filtrate is neutrality, the solid sample filtered after cleaning is dried, the graphite powder pre-oxidized End；
    B. the powdered graphite pre-oxidized adds dense H2SO4In, stirred evenly under the conditions of 0-5 DEG C of ice-water bath, into solution slowly Potassium permanganate powder is added, after then stirring 3-5h under 30-40 DEG C of water-bath, then continues stirring 10- in 0-5 DEG C of ice-water bath 20min, is slow added into deionized water, continues to stir 2-3h, adds the hydrogenperoxide steam generator that mass fraction is 30%, Bian Jia Side is stirred, and 12h is stood after adding, and collects solid sample, and the dilute hydrochloric acid solution for being 4-5% with mass fraction is cleaned, is centrifuged repeatedly Cleaning, untill the pH value of cleaning solution is changed into neutrality, then is dried in vacuo 45-50h, up to graphite oxide powder.
  2. 2. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that：Step（1）In press oxygen The mass ratio of graphite and deionized water is 1:1000 add graphite oxide into deionized water.
  3. 3. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that：Step（2）Middle standing Time is 0.8h.
  4. 4. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that：Step（4）Middle reduction Time is 28h.
  5. 5. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that：Step（5）For by D product It is put into the potassium permanganate of 3mmol/L and soaks 28h, obtain E product, the graphene/Mn oxide being deposited on to obtain the final product on flexible substrate is multiple Close film.
  6. 6. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that：The fexible film is Polyethylene terephthalate, i.e. PET matrix or dimethyl silicone polymer, i.e. PDMS matrixes.
  7. 7. the preparation method of graphene-based electrode material according to claim 1, it is characterised in that the dense H2SO4Matter It is 98% to measure fraction.
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