CN106710895A - Preparation method for supercapacitor electrode material of ultrathin-layer carbon-material bipolar-plate structure - Google Patents
Preparation method for supercapacitor electrode material of ultrathin-layer carbon-material bipolar-plate structure Download PDFInfo
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- CN106710895A CN106710895A CN201710150173.5A CN201710150173A CN106710895A CN 106710895 A CN106710895 A CN 106710895A CN 201710150173 A CN201710150173 A CN 201710150173A CN 106710895 A CN106710895 A CN 106710895A
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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
- H01G11/84—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
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/30—Electrodes characterised by their material
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method for a supercapacitor electrode material of an ultrathin-layer carbon-material bipolar-plate structure. The preparation method comprises the following steps: 1) preparing potassium permanganate solution; 2) dispersing a carbon material into a solvent and preparing and obtaining carbon material solution; 3) spin coating the carbon-material solution on a substrate and drying to obtain a carbon-material spin-coating substrate; 4) performing soaking reaction of the carbon-material spin-coating substrate in the potassium permanganate solution to enable a covering face of the potassium permanganate solution to be larger than a spin-coating face of the carbon-material solution, taking out the carbon-material spin-coating substrate after reaction is finished, evenly spin coating the potassium permanganate solution on the surface of the carbon-material spin-coating substrate and drying to obtain a compound spin-coating substrate; 5) repeating the step 3) and the step 4) on the compound spin-coating substrate until a set layer requirement is met; 6) annealing the compound spin-coating substrate prepared in the step 5) in inert gas protection and cooling to obtain the supercapacitor electrode material of the ultrathin-layer carbon-material bipolar-plate structure.
Description
Technical field
It is specifically super for a kind of superthin layer carbon material bipolar plate structure the invention belongs to electrode for capacitors technical field
The preparation method of capacitor electrode material.
Background technology
The research and development of novel energy-storing material always are the study hotspot of countries in the world scientist, energy storaging product miscellaneous
Also fast sale is gradually introduced to the market.Small volume, be easy to carry, capacity is big, stability is strong, storage the features such as can repeatedly recycle
Energy device can get the favour of people always.Ultracapacitor is applied as new energy storage device with its unique advantage
Every field in the life such as military affairs, traffic, communication, medical treatment.Ultracapacitor as the optimal energy storage device complementary with battery,
It to be mainly characterized by the ability of sparking stronger, there is provided powerful output.Traditional capacitor is mainly due to dependence
Physical reactions complete thermal energy storage process, and energy storage is realized by material surface area adsorption charge in itself, so directly limit electric capacity
The capacity of device.Ultracapacitor also known as fake capacitance or faraday's capacitor, with reference to the characteristics of traditional capacitor and battery energy storage
Energy storage is realized by the way of redox reaction and physical absorption electric charge are combined so that rely solely on material surface suction originally
Attached electric charge has obtained the lifting of several times realizing the condenser capacity of energy storage.
However, the factor of restriction capacity of super capacitor is numerous, such as electrolyte, collector etc., wherein with capacitor sheet
The voltage swing that body can be provided is particularly of crucial importance, and why ultracapacitor can not be directly as power source, also exactly
Because the multiple proportion that the size of its capacity is directly proportional square to voltage, and the voltage very little that its monomer electric capacity can be provided,
So the size of potential window becomes the technical bottleneck for limiting its development so that capacity hardly results in larger lifting.
The content of the invention
In view of this, it is an object of the invention to provide a kind of super capacitor electrode of superthin layer carbon material bipolar plate structure
The preparation method of pole material, it is possible to increase the potential window of electrode material, lifts the voltage of ultracapacitor, increases super capacitor
The capacity of device.
To reach above-mentioned purpose, the present invention provides following technical scheme：
A kind of preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure, comprises the following steps：
1）Prepare liquor potassic permanganate；
2）By carbon material dispersion in a solvent, carbon material solution is prepared；
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying；
4）By the step 3）The carbon material spin coated substrate for obtaining soaks reaction in the liquor potassic permanganate, makes potassium permanganate
The coverage rate of solution takes out the carbon material spin coated substrate, and will be attached to more than the spin coating face of carbon material solution after the completion of reaction
The liquor potassic permanganate spin coating on the carbon material spin coated substrate surface is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until reaching the number of plies requirement of setting；
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, and superthin layer is obtained after cooling
The electrode material for super capacitor of carbon material bipolar plate structure.
Further, the step 1）The liquor potassic permanganate of middle preparation is saturation liquor potassic permanganate.
Further, the carbon material uses the allotrope of the carbon being dispersed among in solvent.
Further, the carbon material uses Graphene.
Further, the step 4）In, immersion reaction of the carbon material spin coated substrate in the liquor potassic permanganate
Temperature is less than or equal to 100 DEG C.
Further, the step 5）In, it is up to set the compound spin coated substrate drying treatment of number of plies requirement.
Further, the step 6）In, annealing temperature is 100 ~ 1200 DEG C, is cooled down using Temperature fall during cooling.
Further, programming rate during annealing is 1-20 DEG C/min.
The beneficial effects of the present invention are：
The preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure of the present invention, by the method for spin coating
Make potassium permanganate and carbon material that the sandwich construction of one layer of a stacking, potassium permanganate and carbon material reaction generation manganese are formed in substrate
Oxide, and the spin coating face of carbon material solution is greater than due to the coverage rate of liquor potassic permanganate so that the oxide of manganese
Carbon material is divided into the mutually isolated superthin layer of multilayer, when electrolyte enters in electrode material, superthin layer carbon material becomes a Virtual
The bipolar plates of plan, make whole electrode be made up of a series of battery of series connection, so as to substantially increase the potential window of electrode material,
Using the electrode material as electrode material for super capacitor use when, greatly improve the voltage of ultracapacitor, can be
The voltage limit of aqueous electrolyte is promoted to 2.6V from 1.23V, maintains great power and capacity.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carries out
Explanation：
Fig. 1 is the preparation process schematic diagram of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure；
Fig. 2 is the electrode material for super capacitor TEM figures of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared；
Fig. 3 is the XPS figures of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared；
Fig. 4 is the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1-6 is prepared in 1mol/
Electrochemistry CV figures in the lithium sulfate aqueous solution electrolysis liquid of L concentration；
Fig. 5 is the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared in 1mol/L
CV figures in the lithium sulfate aqueous solution electrolysis liquid of concentration under different voltage windows；
Fig. 6 is the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared in 1mol/L
The CV figures of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of concentration；
Fig. 7 is the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared in 1mol/L
Specific capacitance value in the lithium sulfate aqueous solution electrolysis liquid of concentration under the different total numbers；
Fig. 8 is that the electrode material for super capacitor assembling of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared is grown up to be a useful person
After part, the CV figures of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
Fig. 9 is that the electrode material for super capacitor assembling of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared is grown up to be a useful person
After part, the discharge curve under different discharge-rates in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
Figure 10 is that the electrode material for super capacitor assembling of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared is grown up to be a useful person
After part, energy density and power density diagram in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, so that those skilled in the art can be with
It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Embodiment 1
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 40 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the Gao Meng on the carbon material spin coated substrate surface will be attached to
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 15 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 50 DEG C after annealing, and programming rate is 3 DEG C/min, and 30min, last Temperature fall are kept after being warming up to 500 DEG C
Cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
Embodiment 2
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 100 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the Gao Meng on the carbon material spin coated substrate surface will be attached to
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 3 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 20 DEG C after annealing, and programming rate is 20 DEG C/min, and 10min is kept after being warming up to 1200 DEG C, last to drop naturally
Temperature cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
Embodiment 3
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 25 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the Gao Meng on the carbon material spin coated substrate surface will be attached to
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 6 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 30 DEG C after annealing, and programming rate is 1 DEG C/min, and 60min, last Temperature fall are kept after being warming up to 100 DEG C
Cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
Embodiment 4
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 60 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the Gao Meng on the carbon material spin coated substrate surface will be attached to
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 9 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 40 DEG C after annealing, and programming rate is 10 DEG C/min, and 25min is kept after being warming up to 800 DEG C, last to drop naturally
Temperature cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
Embodiment 5
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 80 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the Gao Meng on the carbon material spin coated substrate surface will be attached to
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 12 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 40 DEG C after annealing, and programming rate is 15 DEG C/min, and 20min is kept after being warming up to 1000 DEG C, last to drop naturally
Temperature cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
Embodiment 6
The preparation method of the electrode material for super capacitor of the superthin layer carbon material bipolar plate structure of the present embodiment, including following step
Suddenly：
1）Potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2）By carbon material dispersion in a solvent, carbon material solution is prepared；Wherein, carbon material is used and is dispersed among solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, is specifically：Graphite powder is oxidized to
Graphite oxide, then be graphene oxide by graphite oxide ultrasonic disperse, then graphene oxide is dispersed in water, it is prepared into dense
Spend the carbon material solution for 4 mg/ml.
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4）By step 3）The carbon material spin coated substrate for obtaining soaks reaction in liquor potassic permanganate, makes liquor potassic permanganate
Coverage rate more than carbon material solution spin coating face；Immersion reaction temperature is less than or equal to 100 DEG C, and the soaking temperature of the present embodiment is adopted
With 5 DEG C；The carbon material spin coated substrate is taken out after the completion of reaction, and the permanganic acid on the carbon material spin coated substrate surface will be attached to
Potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until after the number of plies for reaching setting is required, drying；This
Embodiment repeat step 3）With step 4）Number of times be 18 times.
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment by composite substrate argon gas protection under move back
Fire, initial temperature is 40 DEG C after annealing, and programming rate is 8 DEG C/min, and 40min, last Temperature fall are kept after being warming up to 300 DEG C
Cooling, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
As shown in figure 1, for the preparation process of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure is illustrated
Figure, makes potassium permanganate and graphene oxide that the sandwich construction of one layer of a stacking, Gao Meng are formed in substrate by the method for spin coating
Sour potassium and graphite oxide alkene reaction generate the oxide of manganese, and Graphene is reduced to by rear oxidation Graphene of annealing, and due to
The coverage rate of liquor potassic permanganate is greater than the spin coating face of graphene oxide solution so that be divided into for Graphene many by the oxide of manganese
The mutually isolated superthin layer of layer, when electrolyte enters in electrode material, ultra-thin layer graphene becomes the bipolar plates of Virtual plans, makes whole
Individual electrode is made up of a series of battery of series connection, so as to substantially increase the potential window of electrode material.
As shown in Fig. 2 the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
Material TEM figures, it may be clearly seen that the modified oxide of manganese is between the Graphene of one layer of a stacking, and can be by high-resolution
TEM figures see clearly brilliant picture.
As shown in figure 3, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
The XPS figures of material, a figures are that manganese element is schemed in the XPS of 2p tracks, and b figures are that manganese element is schemed in the XPS of 3s tracks；A figures embody manganese unit
Element is 11.8eV in the band difference of 2p tracks, meets the requirement of manganese dioxide Mn4+；Meanwhile, on the 3s tracks of b figure manganese elements
Band difference is 4.8eV, this imply that there is the manganese of multivalent state.
As shown in figure 4, the electrode of super capacitor of the superthin layer carbon material bipolar plate structure prepared for embodiment 1-6
Electrochemistry CV figure of the material in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration, it is seen then that the electrode that embodiment 1 is prepared
Material show maximum potential window, and maximum specific capacity.
As shown in figure 5, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
The CV figures under different voltage windows in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration are expected, even in big total number situation
Lower electrode material can still realize insertion and the abjection lithium ion of lithium ion, because this material is mainly relies on electrolyte
Lithium ion turnover material realize energy storage, it can be seen that have two pairs of redox respectively in 1.1,0.2V and -0.2,0.7V respectively
Peak, indicates insertion and the abjection current potential of this lithium ion.Illustrate that the electrode material is a kind of good electrode material for super capacitor,
Still being capable of largely energy storage under high-power.
As shown in fig. 6, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
Expect the CV figures of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration, illustrate the electrode that embodiment 1 is prepared
Material can realize the voltage of 2.6V in the lithium sulfate electrolyte of water system in theory, this currently without any on water system
The capacitor of electrolyte can be realized.
As shown in fig. 7, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
Expect the specific capacitance value under the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration, maximum is 152F, in 5mV/s
The total number under.
As shown in figure 8, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
After material is assembled into device, the CV figures of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；Be can be seen that from figure
Electrode material maintains good cyclicity after being assembled into device, and the pattern showed under the voltage of 2V is electric double layer rectangle,
And the symmetry of discharge and recharge is also maintained when high current.
As shown in figure 9, the electrode of super capacitor material of the superthin layer carbon material bipolar plate structure prepared for embodiment 1
After material is assembled into device, the discharge curve under different discharge-rates in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
As can be seen that what charging and discharging curve was presented substantially is symmetrical triangle, the good capacitive character of electrode material is embodied again, together
When very big capacity is still kept under high current, under 1.5A/g electric currents keep 120F capacitance.
As shown in Figure 10, it is the electrode of super capacitor of the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
After material is assembled into device, energy density and power density diagram in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration should
Electric capacity realizes the excellent performance that 66.6Wh/kg is kept when power is 3000W/kg.
Above-mentioned experimental data is proved, in the electrode material that above-described embodiment is obtained, be divided into for Graphene many by the oxide of manganese
The mutually isolated superthin layer of layer, when electrolyte enters in electrode material, ultra-thin layer graphene becomes the bipolar plates of Virtual plans, makes whole
Individual electrode is made up of a series of battery of series connection, so as to substantially increase the potential window of electrode material, is greatly improved super
The voltage of level capacitor, lifts the voltage limit of aqueous electrolyte to 2.6V from 1.23V, maintains great power
And capacity.
Certainly, carbon material of the invention is not limited to graphene oxide, such as can also be porous carbon materials, active carbon materials
Other different types of carbon materials such as material, CNT；In addition, having the substrate of carbon material solution in permanganic acid by adjusting spin coating
The conditions such as immersion reaction temperature, material concentration in potassium solution, can control the load capacity of the oxide of the manganese of generation.
Embodiment described above is only the preferred embodiment lifted to absolutely prove the present invention, protection model of the invention
Enclose not limited to this.Equivalent substitute or conversion that those skilled in the art are made on the basis of the present invention, in the present invention
Protection domain within.Protection scope of the present invention is defined by claims.
Claims (8)
1. a kind of preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure, it is characterised in that：Bag
Include following steps：
1）Prepare liquor potassic permanganate；
2）By carbon material dispersion in a solvent, carbon material solution is prepared；
3）Carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying；
4）By the step 3）The carbon material spin coated substrate for obtaining soaks reaction in the liquor potassic permanganate, makes potassium permanganate
The coverage rate of solution takes out the carbon material spin coated substrate, and will be attached to more than the spin coating face of carbon material solution after the completion of reaction
The liquor potassic permanganate spin coating on the carbon material spin coated substrate surface is uniform, and compound spin coated substrate is obtained after drying；
5）The repeat step 3 on the compound spin coated substrate）With step 4）, until reaching the number of plies requirement of setting；
6）By the step 5）The compound spin coated substrate for preparing is annealed under inert gas shielding, and superthin layer is obtained after cooling
The electrode material for super capacitor of carbon material bipolar plate structure.
2. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 1
Method, it is characterised in that：The step 1）The liquor potassic permanganate of middle preparation is saturation liquor potassic permanganate.
3. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 1
Method, it is characterised in that：The carbon material uses the allotrope of the carbon being dispersed among in solvent.
4. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 3
Method, it is characterised in that：The carbon material uses Graphene.
5. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 1
Method, it is characterised in that：The step 4）In, immersion reaction temperature of the carbon material spin coated substrate in the liquor potassic permanganate
Degree is less than or equal to 100 DEG C.
6. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 1
Method, it is characterised in that：The step 5）In, it is up to set the compound spin coated substrate drying treatment of number of plies requirement.
7. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 1
Method, it is characterised in that：The step 6）In, annealing temperature is 100 ~ 1200 DEG C, is cooled down using Temperature fall during cooling.
8. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 7
Method, it is characterised in that：Programming rate during annealing is 1-20 DEG C/min.
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