CN106710895B - The preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure - Google Patents
The preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure Download PDFInfo
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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 kind of preparation methods of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure, include the following steps: 1) to prepare liquor potassic permanganate；2) carbon material solution in a solvent by carbon material dispersion, is prepared；3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying；4) the carbon material spin coated substrate that step 3) obtains is impregnated into reaction in liquor potassic permanganate, the covering surface of liquor potassic permanganate is set to be greater than the spin coating face of carbon material solution, carbon material spin coated substrate is taken out after the reaction was completed, and the liquor potassic permanganate spin coating for being attached to carbon material spin coated substrate surface is uniform, compound spin coated substrate is obtained after drying；5) step 3) and step 4) are repeated on compound spin coated substrate, until reaching the number of plies requirement of setting；6) the compound spin coated substrate that step 5) is prepared is annealed under inert gas protection, obtains the electrode material for super capacitor of superthin layer carbon material bipolar plate structure after cooling.
Description
Technical field
The invention belongs to electrode for capacitors technical fields, are specifically a kind of the super of superthin layer carbon material bipolar plate structure
The preparation method of capacitor electrode material.
Background technique
The research and development of novel energy-storing material always are the research hotspot of countries in the world scientist, miscellaneous energy storaging product
Also fast sale is gradually introduced to the market.It is small in size, easy to carry, capacity is big, stability is strong, the storage for the features such as can repeatedly recycling
Energy device can be got the favour of people always.Supercapacitor is applied as novel energy storage device with its unique advantage
Every field in the life such as military affairs, traffic, communication, medical treatment.Supercapacitor as the best energy storage device complementary with battery,
It to be mainly characterized by the ability of sparking stronger, powerful output is provided.Traditional capacitor is mainly due to relying on
Physical reactions complete thermal energy storage process, realize energy storage by the surface area adsorption charge of material itself, directly limit capacitor in this way
The capacity of device.Supercapacitor also known as fake capacitance or faraday's capacitor, in conjunction with the characteristics of traditional capacitor and battery energy storage
Energy storage is realized in such a way that redox reaction and physical absorption charge combine, so that relying solely on material surface suction originally
Attached charge realizes that the condenser capacity of energy storage has obtained the promotion of several times.
However, the factor for restricting capacity of super capacitor is numerous, such as electrolyte, collector etc., wherein with capacitor sheet
The voltage swing that body can be provided is especially of crucial importance, supercapacitor why also cannot be exactly directly as power source
Because of the multiple proportion that directly proportional to voltage square of the size of its capacity, and the voltage very little that its monomer capacitor can be provided,
So the size of potential window become limit its development technical bottleneck make capacity hardly result in biggish promotion.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of super capacitor electrodes of superthin layer carbon material bipolar plate structure
The preparation method of pole material can be improved the potential window of electrode material, promote the voltage of supercapacitor, increase super capacitor
The capacity of device.
In order to achieve the above objectives, the invention provides the following technical scheme:
A kind of preparation method of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure, including walk as follows
It is rapid:
1) liquor potassic permanganate is prepared；
2) carbon material solution in a solvent by carbon material dispersion, is prepared；
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying；
4) the carbon material spin coated substrate for obtaining the step 3) impregnates reaction in the liquor potassic permanganate, makes Gao Meng
The covering surface of sour potassium solution is greater than the spin coating face of carbon material solution, takes out the carbon material spin coated substrate after the reaction was completed, and will
The liquor potassic permanganate spin coating for being attached to carbon material spin coated substrate surface is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until reaching the number of plies requirement of setting；
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.
Further, the liquor potassic permanganate prepared in the step 1) is saturation liquor potassic permanganate.
Further, the carbon material uses the allotrope for the carbon being dispersed in solvent.
Further, the carbon material uses graphene.
Further, in the step 4), 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, in the step 5), it is up to the compound spin coated substrate drying processing that the setting number of plies requires.
Further, in the step 6), annealing temperature is 100 ~ 1200 DEG C, cooling using Temperature fall when cooling.
Further, heating rate when 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, passes through spin coating
Method makes potassium permanganate and carbon material that the multilayered structure of one layer of a stacking be formed on the substrate, and potassium permanganate reacts life with carbon material
The oxide of Cheng Meng, and since the covering surface of liquor potassic permanganate is greater than the spin coating face of carbon material solution, so that the oxygen of manganese
Carbon material is divided into the mutually isolated superthin layer of multilayer by compound, and when electrolyte enters in electrode material, superthin layer carbon material becomes
One virtual bipolar plates constitute entire electrode by a series of concatenated batteries, to substantially increase the current potential of electrode material
Window, using the electrode material as electrode material for super capacitor in use, greatly improving the voltage of supercapacitor, energy
It is enough that the voltage limit of aqueous electrolyte is promoted to 2.6V from 1.23V, maintain great power and capacity.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
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 for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
Figure；
Fig. 3 is the XPS of the electrode material for super capacitor for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
Figure；
Fig. 4 is that the electrode material for super capacitor for the superthin layer carbon material bipolar plate structure that embodiment 1-6 is prepared exists
Electrochemistry CV figure in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
Fig. 5 is that the electrode material for super capacitor for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared exists
CV figure in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration under different voltage windows；
Fig. 6 is that the electrode material for super capacitor for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared exists
The CV figure of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
Fig. 7 is that the electrode material for super capacitor for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared exists
Specific capacitance value in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration under the different total numbers；
Fig. 8 is the electrode material for super capacitor assembling for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
After device, the CV figure of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；
Fig. 9 is the electrode material for super capacitor assembling for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
Discharge curve after device, in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration under different discharge-rates；
Figure 10 is the electrode material for super capacitor assembling for the superthin layer carbon material bipolar plate structure that embodiment 1 is prepared
Energy density and power density diagram after device, in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It better understands 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 40 DEG C；The carbon material spin coated substrate, and the Gao Meng that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 15 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 50 DEG C after annealing, and heating rate is 3 DEG C/min, and 30min, last Temperature fall are kept after being warming up to 500 DEG C
It is cooling, obtain 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 100 DEG C；The carbon material spin coated substrate, and the Gao Meng that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 3 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 20 DEG C after annealing, and heating rate is 20 DEG C/min, keeps 10min after being warming up to 1200 DEG C, is finally dropped naturally
Temperature is 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 25 DEG C；The carbon material spin coated substrate, and the Gao Meng that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 6 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 30 DEG C after annealing, and heating rate is 1 DEG C/min, and 60min, last Temperature fall are kept after being warming up to 100 DEG C
It is cooling, obtain 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 60 DEG C；The carbon material spin coated substrate, and the Gao Meng that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 9 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 40 DEG C after annealing, and heating rate is 10 DEG C/min, keeps 25min after being warming up to 800 DEG C, is finally dropped naturally
Temperature is 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 80 DEG C；The carbon material spin coated substrate, and the Gao Meng that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Sour potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 12 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 40 DEG C after annealing, and heating rate is 15 DEG C/min, keeps 20min after being warming up to 1000 DEG C, is finally dropped naturally
Temperature is 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 with
Lower step:
1) potassium permanganate saturated aqueous solution is prepared using potassium permanganate powder.
2) carbon material solution in a solvent by carbon material dispersion, is prepared；Wherein, carbon material uses and is dispersed in solvent
In carbon allotrope, the carbon material of the present embodiment uses graphene oxide, specifically are as follows: be oxidized to graphite powder
Graphite oxide, then by graphite oxide ultrasonic disperse be graphene oxide, then graphene oxide is dispersed in water, is prepared into dense
Degree is the carbon material solution of 4 mg/ml.
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying.
4) the carbon material spin coated substrate that step 3) obtains is impregnated into liquor potassic permanganate reaction, makes liquor potassic permanganate
Covering surface be greater than carbon material solution spin coating face；It impregnates reaction temperature and is less than or equal to 100 DEG C, the soaking temperature of the present embodiment is adopted
With 5 DEG C；The carbon material spin coated substrate, and the permanganic acid that carbon material spin coated substrate surface will be attached to are taken out after the reaction was completed
Potassium solution spin coating is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until drying after the number of plies for reaching setting requires
It is dry；It is 18 times that the present embodiment, which repeats step 3) and the number of step 4),.
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, is surpassed after cooling
The electrode material for super capacitor of coating carbon material bipolar plate structure.The present embodiment moves back composite substrate under protection of argon gas
Fire, initial temperature is 40 DEG C after annealing, and heating rate is 8 DEG C/min, and 40min, last Temperature fall are kept after being warming up to 300 DEG C
It is cooling, obtain the electrode material for super capacitor of superthin layer carbon material bipolar plate structure.
As shown in Figure 1, the preparation process signal of the electrode material for super capacitor for superthin layer carbon material bipolar plate structure
Figure makes potassium permanganate and graphene oxide that the multilayered structure of one layer of a stacking, Gao Meng be formed on the substrate by the method for spin coating
Sour potassium and graphite oxide alkene reaction generate the oxide of manganese, and graphene oxide is reduced to graphene after annealing, and due to
The covering surface of liquor potassic permanganate is greater than the spin coating face of graphene oxide solution so that the oxide of manganese graphene is divided into it is more
The mutually isolated superthin layer of layer, when electrolyte enters in electrode material, superthin layer graphene becomes a virtual bipolar plates, makes whole
A electrode is made of a series of concatenated batteries, to substantially increase the potential window of electrode material.
As shown in Fig. 2, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
Expect TEM figure, it may be clearly seen that between the graphene that the modified oxide of manganese is laminated one layer one, and can be by high-resolution
TEM figure sees clearly brilliant picture.
As shown in figure 3, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
The XPS of material schemes, and a figure is that manganese element is schemed in the XPS of 2p track, and b figure is that manganese element is schemed in the XPS of 3s track；A figure embodies manganese member
Element is 11.8eV in the band difference of 2p track, meets the requirement of manganese dioxide Mn4+；Meanwhile on the 3s track of b figure manganese element
Band difference is 4.8eV, this imply that there is the manganese of multivalent state.
As shown in figure 4, for the electrode of super capacitor of the embodiment 1-6 superthin layer carbon material bipolar plate structure being prepared
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 shows maximum potential window and maximum specific capacity.
As shown in figure 5, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
The CV figure under voltage window different in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration is expected, even in big total number situation
Lower electrode material still can be realized insertion and the abjection lithium ion of lithium ion, this is because this material mainly relies on electrolyte
Lithium ion disengaging 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,
It still being capable of a large amount of energy storage under high-power.
As shown in fig. 6, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
The CV figure for expecting the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration, illustrates the electrode that embodiment 1 is prepared
The voltage of 2.6V theoretically may be implemented in material in water-based sulfuric acid lithium electrolyte, this currently without any about water system
The capacitor of electrolyte may be implemented.
As shown in fig. 7, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
Expect the specific capacitance value in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration under the different total numbers, maximum value 152F, in 5mV/s
The total number under.
As shown in figure 8, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
After material is assembled into device, the CV figure of the different total numbers in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration；It 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 charge and discharge is also maintained when high current.
As shown in figure 9, the electrode of super capacitor material for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
Discharge curve after material is assembled into device, in the lithium sulfate aqueous solution electrolysis liquid of 1mol/L concentration under different discharge-rates；
As can be seen that charging and discharging curve was presented substantially is symmetrical triangle, the good capacitive character of electrode material is embodied again, together
When still keep very big capacity under high current, the capacitance of 120F is kept under 1.5A/g electric current.
As shown in Figure 10, the electrode of super capacitor for the superthin layer carbon material bipolar plate structure being prepared for embodiment 1
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
Capacitor realizes the excellent performance that 66.6Wh/kg is kept when power is 3000W/kg.
Above-mentioned experimental data proves, in above-described embodiment obtained electrode material, graphene is divided into more by the oxide of manganese
The mutually isolated superthin layer of layer, when electrolyte enters in electrode material, superthin layer graphene becomes a virtual bipolar plates, makes whole
A electrode is made of a series of concatenated batteries, to substantially increase the potential window of electrode material, is greatly improved super
The voltage of grade capacitor promotes 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, can also be such as porous carbon materials, active carbon materials
Other different types of carbon materials such as material, carbon nanotube；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 to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (7)
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: packet
Include following steps:
1) liquor potassic permanganate is prepared；
2) carbon material solution in a solvent by carbon material dispersion, is prepared；
3) carbon material solution is spun in substrate, carbon material spin coated substrate is obtained after drying；
4) the carbon material spin coated substrate for obtaining the step 3) impregnates reaction in the liquor potassic permanganate, makes potassium permanganate
The covering surface of solution is greater than the spin coating face of carbon material solution, takes out the carbon material spin coated substrate after the reaction was completed, and will be attached to
The liquor potassic permanganate spin coating on carbon material spin coated substrate surface is uniform, and compound spin coated substrate is obtained after drying；
5) step 3) and step 4) are repeated on the compound spin coated substrate, until reaching the number of plies requirement of setting；
6) the compound spin coated substrate that the step 5) is prepared is annealed under inert gas protection, obtains superthin layer 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 liquor potassic permanganate prepared in the step 1) 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 isomer graphene for the carbon being dispersed in solvent.
4. 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: in the step 4), temperature is reacted in immersion of the carbon material spin coated substrate in the liquor potassic permanganate
Degree is less than or equal to 100 DEG C.
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: in the step 5), be up to the compound spin coated substrate drying processing that the setting number of plies requires.
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: in the step 6), annealing temperature is 100~1200 DEG C, cooling using Temperature fall when cooling.
7. the preparation side of the electrode material for super capacitor of superthin layer carbon material bipolar plate structure according to claim 6
Method, it is characterised in that: heating rate when annealing is 1-20 DEG C/min.
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