CN109767923B - Structural function integrated super capacitor and preparation method thereof - Google Patents
Structural function integrated super capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a structural function integrated super capacitor and a preparation method thereof. And (2) compounding the carbon fiber or the woven material thereof with a carbon-based electrode material to form a highly conductive three-dimensional network, modifying with a conductive polymer to obtain a carbon fiber composite electrode, and assembling the obtained carbon fiber composite electrode on two sides of the solid electrolyte to obtain the supercapacitor. Compared with the prior art, the invention has the advantages of high tensile strength, improved conductivity, increased specific surface area, improved specific capacitance, liquid leakage prevention and the like.
Description
Technical Field
The invention relates to a capacitor, in particular to a structural function integrated super capacitor and a preparation method thereof.
Background
Among various energy storage devices, a super capacitor (also called as an electrochemical capacitor) is a novel charge storage device, and compared with a common battery, the super capacitor has the advantages of high power density, large-current charge and discharge support, long cycle life, environmental protection, no pollution and good temperature characteristic, and the super capacitor does not relate to chemical reaction in the charge and discharge process, and the electrode material of the super capacitor cannot be damaged; compared with the common capacitor, the capacitor has the advantages of large capacity and the like. Therefore, the super capacitor has wide application prospects in the fields of new energy, transportation and industry, and is suitable for the fields of electric buses, automobile starting, wind power generation, power system power grid transformation and the like.
In recent years, with the increase of the dependence degree of people on energy storage devices, the energy storage devices with single function cannot meet the increasing demands of people. The new research direction focuses on a multifunctional energy storage system, and chinese patent CN106941179A discloses a preparation method of a graphene polyaniline modified carbon cloth electrode material, which is used as an anode in a bioelectrochemical system reactor, although the biological anode acclimation is accelerated, the material is not densified, has no structure and has no further exploration performance in the aspects of bearing load.
Chinese patent CN106997808A discloses a supercapacitor based on graphene/silicon-aluminum gel material. The silicon-aluminum gel material is used as the interlayer, and although the interlayer has certain compressive strength, the interlayer is low in tensile strength, and is not ideal in specific capacitance and is not a proper structural material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a structural and functional integrated supercapacitor and a preparation method thereof, wherein the structural and functional integrated supercapacitor is high in tensile strength, improved in conductivity, increased in specific surface area, improved in specific capacitance and prevented from liquid leakage.
The purpose of the invention can be realized by the following technical scheme: a structural function integrated super capacitor is characterized by comprising a solid electrolyte and carbon fiber composite electrodes arranged on two sides of the solid electrolyte.
The solid electrolyte adopts one or more of polyethylene oxide (PEO), polymethyl methacrylate (PMMA), polyvinylidene fluoride (PAN) and polyvinyl chloride (PVC) polymer electrolytes.
The solid electrolyte is a thin film with the thickness of 0.8-1 mm.
The carbon fiber composite electrode is carbon fiber or is mixed with other materials.
The carbon fiber composite electrode is formed by compounding carbon fibers or woven materials thereof with a carbon-based electrode material and conductive polymers, and the specific compounding method is that the conductive polymers and the carbon-based electrode material are compounded, and then the obtained total modifier is uniformly coated on the carbon fiber material. Such as aniline monomer, in an aqueous graphene dispersion. And then smearing is carried out to form a high-conductivity three-dimensional network. The loading capacity of the total modifier formed by compounding the carbon-based electrode material and the conductive polymer material on the single surface of the carbon fiber or the woven material thereof is 5mg-2。
The carbon-based electrode material is one or more of graphene or carbon nano tubes.
The carbon-based electrode material is compounded with the conductive polymer, so that the specific surface area of the electrode is increased, and the specific capacitance of the composite electrode is enhanced. The method for obtaining the total electrode modifier material by compounding the carbon-based electrode material and the conductive polymer comprises the following steps: ultrasonically dispersing a water dispersion solute of graphene or a carbon nano tube and a conductive polymer monomer in a hydrochloric acid solution according to a mass ratio of 5-100:1, then reacting the water dispersion solute with a hydrochloric acid solution of ammonium persulfate at 0-5 ℃ for 10 hours, stirring the solution at room temperature for 8 hours, performing suction filtration, and performing freeze drying for 1d to obtain an electrode total modifier formed by compounding a carbon-based electrode material and a conductive polymer material. Wherein the molar ratio of ammonium persulfate to the conductive high molecular monomer is 1-2:1, and the concentration of the hydrochloric acid solution is 1 mol/L.
The compounding method of the carbon fiber or the weaving material thereof and the carbon-based electrode material/conductive polymer comprises the following steps: the total modifier obtained by compounding the carbon-based electrode material and the conductive polymer and PVDF are mixed according to the weight ratio of 10: 1, dropping a proper amount of N-methyl pyrrolidone to be mixed into paste, and uniformly coating the paste on two surfaces of the carbon fiber or the weaving material thereof by using a small brush.
The conductive polymer is one or more of polyacetylene, polypyrrole, polythiophene and polyaniline.
The concentration of the carbon-based electrode material in the initial aqueous dispersion is (0.05-1) g.L-1。
A preparation method of a structure-function integrated super capacitor comprises the following steps: and (2) compounding the carbon fiber or the woven material thereof with a carbon-based electrode material to form a highly conductive three-dimensional network, modifying with a conductive polymer to obtain a carbon fiber composite electrode, and assembling the obtained carbon fiber composite electrode on two sides of the solid electrolyte to obtain the supercapacitor.
The invention provides a method for combining the mechanical bearing function of a material with the function of an energy storage system at the same time, so as to realize the combination of the characteristics of structure/function integrated energy conversion, flexibility, structural strength and the like. The structure has good application prospect particularly in the fields of aerospace, aviation and the like which are sensitive to weight abnormity and have urgent requirements on material/structure, light structure and multiple functions, and can reduce the weight of a carrier airplane and save fuel for combustion; and the load capacity can be increased, and the effective load is improved.
Compared with the prior art, the invention has the following advantages:
(1) the assembled super capacitor with the novel structure not only meets certain capacitance characteristics, but also can work under the condition of bearing certain load, and particularly has high tensile strength along the direction of carbon fibers, so that the integration of an energy storage structure is realized.
(2) The carbon fiber composite material is used as an electrode, and an active substance is introduced, so that the conductivity is improved, the specific surface area is increased, and the specific capacitance is improved.
(3) The adopted solid polymer electrolyte eliminates the composition requirement of a diaphragm, and simultaneously avoids the problem of liquid leakage in the assembly process.
Drawings
FIG. 1 is a schematic diagram of a supercapacitor according to the present invention;
FIG. 2 is an enlarged view of the carbon fibers or woven material thereof of FIG. 1;
fig. 3 is a schematic structural diagram of an embodiment of the supercapacitor of the present invention.
The labels in the figure are: 1 is carbon fiber or a weaving material thereof, 2 is a conductive polymer and carbon-based electrode material compound, 3 is a solid electrolyte, and 4 is a carbon fiber compound electrode.
Detailed Description
The following is a detailed description of the embodiments of the present invention, which is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1
Preparing a graphene doped PANI compound: placing 100ml of the mixture in a triangular flask with a concentration of 0.05g.L-1The graphene aqueous dispersion is subjected to ultrasonic treatment (300W) for 30min to uniformly disperse the graphene, and then 0.2g of aniline monomer and 60ml of 1mol.L are added-1And (4) performing ultrasonic treatment on the hydrochloric acid for 30min again, and adsorbing the aniline monomer to the surface of the graphene nanosheet by virtue of the pi-pi stacking effect. 1.08g of ammonium persulfate was dissolved in 60ml of 1mol.L in a beaker in advance-1Hydrochloric acid solution, when the temperature of the solution in the triangular flask is reduced to about 0 ℃, quickly dripping ammonium persulfate solution into the triangular flask, keeping the reaction temperature at 3 ℃ for about 10 hours, continuously stirring at room temperature for 8 hours, stopping reaction, filtering,washing with deionized water until the filtrate is colorless, freeze-drying for 24h in vacuum, carefully grinding uniformly to prepare 1% graphene, and storing the sample in a drying dish.
Mixing the electrode modification material obtained above with PVDF according to the proportion of 10: 1, dropping a proper amount of N-methyl pyrrolidone to form a paste, and uniformly coating the paste on two sides of a carbon cloth by using a small brush, wherein the loading amount of a single side is 5mg-2And drying for 5 hours at 60 ℃ for later use.
Preparation of solid polymer electrolyte: 0.6g of PVA and 0.2g of CMC are weighed into a clean beaker, and a proper amount of deionized water is added, stirred and heated to 90 ℃ so that the PVA and the CMC are fully dissolved and uniformly mixed. Then 1.2g of KOH aqueous solution is added drop by drop, the mixture is continuously stirred and heated until the mixture is viscous, the mixture in the beaker is poured on a molding die to be spread, and the mixture is cooled to form a film, wherein the thickness is controlled to be 0.8-1 mm.
The supercapacitor comprises a solid electrolyte 3 and polyaniline/graphene modified carbon fiber composite electrodes 4 arranged on two sides of the solid electrolyte, the assembled supercapacitor is structurally shown in fig. 1 and comprises carbon fibers or a woven material 1 (the structure is shown in fig. 2), a conductive polymer and carbon-based electrode material compound 2, the carbon fibers or the woven material 1 are wrapped in the conductive polymer and carbon-based electrode material compound 2 to form the carbon fiber composite electrode 4, and the solid electrolyte 3 is sandwiched in the middle.
The tensile strength of the super capacitor prepared in the embodiment is 1820MPa, and the specific capacitance is 82F.g-1。
Example 2
Preparing a graphene doped PANI compound: placing 100ml of the mixture in a triangular flask with a concentration of 0.25g.L-1The graphene aqueous dispersion is subjected to ultrasonic treatment (300W) for 30min to uniformly disperse the graphene, and then 0.2g of aniline monomer and 60ml of 1mol.L are added-1And (4) performing ultrasonic treatment on the hydrochloric acid for 30min again, and adsorbing the aniline monomer to the surface of the graphene nanosheet by virtue of the pi-pi stacking effect. 1.08g of ammonium persulfate was dissolved in 60ml of 1mol.L in a beaker in advance-1Hydrochloric acid solution, when the temperature of the solution in the triangular flask is reduced to about 0 ℃, persulfuric acid is addedAnd quickly dropwise adding the ammonium solution into a triangular flask, keeping the reaction temperature at 3 ℃ for about 10 hours, continuously stirring at room temperature for 8 hours, stopping the reaction, performing suction filtration, washing with deionized water until the filtrate is colorless, performing vacuum freeze drying for 24 hours, carefully and uniformly grinding to prepare 5% graphene, and storing the sample in a drying dish.
Mixing the electrode modification material obtained above with PVDF according to the proportion of 10: 1, dropping a proper amount of N-methyl pyrrolidone to form a paste, and uniformly coating the paste on two sides of a carbon cloth by using a small brush, wherein the loading amount of a single side is 5mg-2And drying for 5 hours at 60 ℃ for later use.
Preparation of solid polymer electrolyte: 0.6g of PVA and 0.2g of CMC are weighed into a clean beaker, and a proper amount of deionized water is added, stirred and heated to 90 ℃ so that the PVA and the CMC are fully dissolved and uniformly mixed. Then 1.2g of KOH aqueous solution is added drop by drop, the mixture is continuously stirred and heated until the mixture is viscous, the mixture in the beaker is poured on a molding die to be spread, and the mixture is cooled to form a film, wherein the thickness is controlled to be 0.8-1 mm.
And assembling according to the structure shown in fig. 3 to obtain a structure/function integrated supercapacitor, wherein the supercapacitor comprises a solid electrolyte 3 and polyaniline/graphene modified carbon fiber composite electrodes 4 arranged on two sides of the solid electrolyte.
The tensile strength of the super capacitor prepared in the embodiment is 1355MPa, and the specific capacitance is 73F.g-1。
Example 3
Preparing a graphene doped PANI compound: placing 100ml of the mixture in a triangular flask with a concentration of 1g.L-1The graphene aqueous dispersion is subjected to ultrasonic treatment (300W) for 30min to uniformly disperse the graphene, and then 0.2g of aniline monomer and 60ml of 1mol.L are added-1And (4) performing ultrasonic treatment on the hydrochloric acid for 30min again, and adsorbing the aniline monomer to the surface of the graphene nanosheet by virtue of the pi-pi stacking effect. 1.08g of ammonium persulfate was dissolved in 60ml of 1mol.L in a beaker in advance-1Hydrochloric acid solution, when the temperature of the solution in the triangular flask is reduced to about 0 ℃, quickly dripping ammonium persulfate solution into the triangular flask, keeping the reaction temperature at 3 ℃ for about 10 hours, continuously stirring at room temperature for 8 hours, stopping the reaction, performing suction filtration, washing with deionized water until the filtrate is colorless, performing vacuum freeze drying for 24 hours,and carefully and uniformly grinding to prepare 20% graphene, and storing the sample in a drying dish.
Mixing the electrode modification material obtained above with PVDF according to the proportion of 10: 1, dropping a proper amount of N-methyl pyrrolidone to form a paste, and uniformly coating the paste on two sides of a carbon cloth by using a small brush, wherein the loading amount of a single side is 5mg-2And drying for 5 hours at 60 ℃ for later use.
Preparation of solid polymer electrolyte: 0.6g of PVA and 0.2g of CMC are weighed into a clean beaker, and a proper amount of deionized water is added, stirred and heated to 90 ℃ so that the PVA and the CMC are fully dissolved and uniformly mixed. Then 1.2g of KOH aqueous solution is added drop by drop, the mixture is continuously stirred and heated until the mixture is viscous, the mixture in the beaker is poured on a molding die to be spread, and the mixture is cooled to form a film, wherein the thickness is controlled to be 0.8-1 mm.
And assembling according to the structure shown in fig. 3 to obtain a structure/function integrated supercapacitor, wherein the supercapacitor comprises a solid electrolyte 3 and polyaniline/graphene modified carbon fiber composite electrodes 4 arranged on two sides of the solid electrolyte.
The tensile strength of the super capacitor prepared in the embodiment is 1468MPa, and the specific capacitance is 68F.g-1。
Example 4
Preparing a graphene/carbon nanotube doped PANI compound: placing 100ml of the mixture in a triangular flask with a concentration of 0.5g.L-1The graphene aqueous dispersion liquid of (2), wherein the mass ratio of graphene to carbon nanotubes is 2:1, carrying out ultrasonic treatment (300W) for 30min to uniformly disperse the graphene/carbon nano tube, and then adding 0.2g of aniline monomer and 60ml of 1mol.L-1The hydrochloric acid was sonicated again for 30 min. 1.08g of ammonium persulfate was dissolved in 60ml of 1mol.L in a beaker in advance-1And (3) hydrochloric acid solution, when the temperature of the solution in the triangular flask is reduced to about 0 ℃, quickly dropwise adding ammonium persulfate solution into the triangular flask, keeping the reaction temperature at 3 ℃ for about 10 hours, continuously stirring at room temperature for 8 hours, stopping the reaction, performing suction filtration, washing with deionized water until filtrate is colorless, performing vacuum freeze drying for 24 hours, carefully and uniformly grinding to prepare 10% graphene/carbon nano tube, and placing the sample in a drying dish for storage.
The obtained electrode modification material and PVDF (polyvinylidene fluoride)According to the following steps of 10: 1, dropping a proper amount of N-methyl pyrrolidone to form a paste, and uniformly coating the paste on two sides of a carbon cloth by using a small brush, wherein the loading amount of a single side is 5mg-2And drying for 5 hours at 60 ℃ for later use.
Preparation of solid polymer electrolyte: 0.6g of PVA and 0.2g of CMC are weighed into a clean beaker, and a proper amount of deionized water is added, stirred and heated to 90 ℃ so that the PVA and the CMC are fully dissolved and uniformly mixed. Then 1.2g of KOH aqueous solution is added drop by drop, the mixture is continuously stirred and heated until the mixture is viscous, the mixture in the beaker is poured on a molding die to be spread, and the mixture is cooled to form a film, wherein the thickness is controlled to be 0.8-1 mm.
And assembling the structure/function integrated super capacitor according to the structure shown in fig. 3, wherein the super capacitor comprises a solid electrolyte 3 and carbon fiber composite electrodes 4 which are arranged on two sides of the solid electrolyte and modified by polyaniline/graphene/carbon nano tubes.
The tensile strength of the super capacitor prepared in the embodiment is 1792MPa, and the specific capacitance is 81F.g-1。
Claims (5)
1. A structure function integrated super capacitor is characterized by comprising a solid electrolyte and carbon fiber composite electrodes arranged on two sides of the solid electrolyte; the solid electrolyte is a thin film with the thickness of 0.8-1 mm;
the carbon fiber composite electrode is a high-conductivity three-dimensional network formed by compounding carbon fibers or woven materials thereof with a carbon-based electrode material and a conductive polymer, and the specific compounding method is that the conductive polymer and the carbon-based electrode material are compounded, and then the obtained total modifier is uniformly coated on the carbon fiber material;
the carbon-based electrode material is one or more of graphene or carbon nano tubes;
the method for obtaining the total electrode modifier material by compounding the carbon-based electrode material and the conductive polymer comprises the following steps: ultrasonically dispersing solute of graphene or carbon nano tube water dispersion liquid and conductive high molecular monomer in hydrochloric acid solution according to the mass ratio of 5-100:1, then reacting the mixture with hydrochloric acid solution of ammonium persulfate at 0-5 ℃ for 10h, and placing the mixture in a chamberStirring for 8h at the temperature, filtering, and freeze-drying for 1d to obtain a total electrode modifier formed by compounding a carbon-based electrode material and a conductive polymer material; the concentration of the initial aqueous dispersion of the carbon-based electrode material is 0.05-1g.L-1。
2. A structurally-integrated supercapacitor according to claim 1, wherein the solid electrolyte is one or more of polyethylene oxide (PEO), Polymethylmethacrylate (PMMA), polyvinylidene fluoride (PAN), polyvinyl chloride (PVC) polymer electrolytes.
3. The structurally-functionally-integrated supercapacitor according to claim 1, wherein the carbon fiber composite electrode is modified with a conductive polymer to enhance the specific capacitance of the composite electrode.
4. The structurally-functionally-integrated supercapacitor according to claim 3, wherein the conductive polymer is one or more of polyacetylene, polypyrrole, polythiophene and polyaniline.
5. The preparation method of the structurally-functionally-integrated supercapacitor according to claim 1, characterized by comprising the following steps: and (2) compounding the carbon fiber or the woven material thereof with a carbon-based electrode material to form a highly conductive three-dimensional network, modifying with a conductive polymer to obtain a carbon fiber composite electrode, and assembling the obtained carbon fiber composite electrode on two sides of the solid electrolyte to obtain the supercapacitor.
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