CN111508725B - Preparation of self-supporting carbon material and water system hybrid high-voltage capacitor prepared from self-supporting carbon material - Google Patents
Preparation of self-supporting carbon material and water system hybrid high-voltage capacitor prepared from self-supporting carbon material Download PDFInfo
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- 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
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- 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
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- 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
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- 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
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- 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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Abstract
The invention discloses a preparation method of a self-supporting carbon material and a symmetrical water system hybrid high-voltage capacitor prepared by the same; the invention firstly prepares the self-supporting carbon material through hydrothermal reaction, solution dipping and high-temperature carbonization, and then adopts the processes of solution soaking, rotary evaporation and ice water quenching to prepare the carbon-polymer composite electrode. The carbon-polymer dielectric composite electrode can effectively isolate the contact of electrons and water, thereby improving the working voltage of a water system electrolyte, simultaneously, the dielectric layer can enhance the capacitance performance of the capacitor in the charging and discharging processes, and the carbon-polymer dielectric composite electrode is suitable for preparing a high-energy density capacitor. The carbon-polymer composite electrode is assembled into a novel symmetrical water system hybrid high-voltage capacitor, and the voltage window can be improved to 2V at 0.4mA/cm2The specific area capacity of the current reaches 333.3mF/cm2Compared with the carbon material electrode without the polymer electrolyte, the energy density of the novel capacitor is improved by 1300%.
Description
Technical Field
The invention belongs to the technical field of energy storage material preparation, relates to preparation of a carbon material and a high-voltage capacitor prepared from the carbon material, and particularly relates to preparation of a self-supporting carbon material and a symmetric water system hybrid high-voltage capacitor prepared from the self-supporting carbon material.
Background
With the rise of electronic automobiles, the safety and the quick charging performance of energy storage devices become more and more important. The super capacitor has the advantages of high power density, long cycle life, short charging time and the like, and is the most promising secondary battery to replace an energy storage device at present. Importantly, water-based electrolytes would be a better choice for supercapacitors than flammable organic solutions and expensive ionic liquid electrolytes, in view of safety, cost and recycling issues. However, the low energy density of water-based supercapacitors remains a great challenge, limiting their spread in practical applications.
According to the formula of the energy density of the capacitor,
the energy density (E) is dependent on the specific capacitance (C) and the operating voltage (V). Increasing the energy density of a supercapacitor can only be achieved by increasing the capacitor capacity or operating voltage. Since the theoretical water decomposition voltage is 1.23V, it is critical to realize a high-pressure water system supercapacitor to suppress water decomposition. At present, there are three methods for increasing the operating voltage of an aqueous capacitor. The method comprises the following steps: using highly concentrated salt solutions, e.g. 1M Na2SO4The working voltage can reach 1.8V (Feng H, Hu H, et al. high structural carbon derived from baseband gases: a single and effective synthesis and its improved electronic properties for high-performance supercapacitors [ J]Journal of Power Sources,302(2016), pp.164-173). The method 2 comprises the following steps: asymmetric positive and negative electrode materials are used to inhibit water decomposition, and the working voltage can be generally more than 2V (Xiong T, Teck Leong Tan, et al. harmonic energy and power sensitivity aware 2.7V asynchronous aqueous superparameter [ J]Advanced Energy materials.2018,8,1702630). The method 3 comprises the following steps: high concentrations of aqueous salt solutions are used to reduce the kinetics of the water splitting reaction, even at voltages above 3V (Yuki Yamada, Kenji Usui, Keitaro Sodeyama, Hydrate-salt electrolytes for high-energy-dense aqueous batteries [ J]Nature Energy,2016,1: 16129). However, for carbon materials, the only commercial capacitor electrode materials, only methods 1 and 3 are applicable. The high salt solution concentration of method 1 generally results in low specific capacitance and low conductivity, reducing the electrochemical performance of the capacitor. In the method 3, the salt-coated aqueous solution has high viscosity and large ion cluster size, so that the method has low capacity and high resistance, and is extremely high in cost, so that the method is not suitable for wide production at present. Prior to the present invention, there was no method to assemble symmetric supercapacitors from carbon materials in 6M KOH conventional electrolyte to achieve operating voltages above 1V.
Disclosure of Invention
The invention provides a self-supporting carbon material preparation method and a symmetrical water system hybrid high-voltage capacitor prepared by the self-supporting carbon material, aiming at the problems that a water system capacitor is low in energy density and difficult to practically apply. The invention prepares a brand new hybrid super capacitor for the first time so as to improve the energy density of the water system super capacitor. Firstly, the dielectric prevents the contact of water and electrons in the process of charging and discharging to inhibit the decomposition of water, thereby improving the working voltage; meanwhile, the dielectric material can store energy through dipole overturning in the charging and discharging processes. It is worth noting that the polarized polymer chain segment can be used as an active site for ion adsorption, thereby improving the capacitance of the capacitor. PVDF and PVDF-based copolymers have high dielectric constants and high breakdown strengths, and are considered ideal candidates for next-generation polymer capacitors. The invention prepares the electrode material of the hybrid capacitor by using a carbon material and PVDF-based dielectric polymer composite electrode. The invention has higher use value and is the optional development direction of the next generation double high capacitor.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of a self-supporting carbon material with high openness and high specific surface, which comprises the following steps:
A. growing zinc oxide of a nano array on the surface of the hydrophilic carbon cloth through a hydrothermal reaction (a specific method reference ACS appl. Mater. interfaces 2018,10, 3549-; the zinc oxide of the nano array can be used as a template and an activator for the in-situ growth of a carbon material in the next step;
B. b, soaking the carbon cloth zinc oxide compound grown in the step A in a carbon source solution for a certain time, and then taking out and drying;
C. heating the dried carbon cloth zinc oxide compound to 150-plus-180 ℃ in the inert gas atmosphere, preserving heat (melting a carbon source to uniformly coat the surface of the zinc oxide), then heating to 800-plus-1000 ℃, preserving heat (preparing a carbon material by carbonization), naturally cooling to room temperature, and taking out;
D. and D, putting the carbon cloth zinc oxide compound taken out in the step C into an acid solution again to wash away zinc oxide, and repeatedly washing the carbon cloth zinc oxide compound to be neutral through deionized water to obtain the self-supporting carbon material.
The self-supporting carbon material prepared by the method has the characteristics of high open specific surface area, high conductivity and integration of an active material and a current collector, and does not need to use a binder.
Preferably, in the step B, the concentration of the carbon source solution is 1M, and the soaking time is 12 hours; the drying temperature is 80 ℃, and the drying time is 1 hour.
Preferably, in the step C, the inert gas is argon, and the introduction amount is 40 mL/min; the heating rate for heating to 150-180 ℃ is 1 ℃/min, and the heating rate for heating to 800-1000 ℃ is 5 ℃/min.
Preferably, in step B, the carbon source solution is a glucose solution.
Preferably, in the step C, the temperature is maintained at 150-180 ℃ for 1 hour, and at 800-1000 ℃ for 2 hours.
Preferably, in step D, the acid solution is at least one of a hydrochloric acid solution and a sulfuric acid solution.
The present invention provides a highly open, high specific surface area, self-supporting carbon material prepared according to the aforementioned method.
The invention provides a carbon-polymer composite electrode material prepared from the self-supporting carbon material, which comprises the self-supporting carbon material and a polymer dielectric layer coated on the self-supporting carbon material.
The invention provides a preparation method of the carbon-polymer composite electrode material, which comprises the following steps:
s1, cutting the self-supporting carbon material into an electrode shape;
s2, adding the fluorine-containing polymer into the N, N-dimethylformamide solution, stirring and dissolving to obtain a solution a;
s3, putting the sheared self-supporting carbon material into the solution a for soaking, performing rotary evaporation under a vacuum condition until the solution is dried to obtain a composite material, and then naturally drying;
and S4, drying the composite material processed in the step S3 by air blowing, taking out, and quenching in ice water to obtain the carbon-polymer composite electrode material.
Preferably, in step S2, the fluoropolymer includes PVDF-HFP, PVDF; the temperature for stirring and dissolving is 80 ℃;
in step S3, the temperature of the rotary evaporation is 80 ℃; the natural drying time is 24 hours;
in step S4, the temperature of the forced air drying was 200 ℃ and the drying time was 10 minutes.
The invention firstly prepares the self-supporting carbon material through hydrothermal reaction, solution impregnation and high-temperature carbonization, and then prepares the carbon-polymer composite electrode material by adopting the processes of solution soaking, rotary evaporation and ice water quenching. Firstly, growing a zinc oxide rod array on the surface of carbon cloth through hydrothermal reaction, wherein the zinc oxide rod can be used as a template and an activator for in-situ growth of a carbon material in the next step, the obtained carbon material has a mutually connected and fluctuant carbon sheet structure, and then forming a compact and hydrophobic dielectric layer on the surface of the carbon material by using a polymer. The carbon-polymer dielectric composite electrode prepared by the invention can effectively isolate the contact of electrons and water, thereby improving the working voltage of a water system electrolyte, and meanwhile, the dielectric layer can enhance the capacitance performance of the capacitor in the charging and discharging processes, so that the carbon-polymer dielectric composite electrode is suitable for preparing a high-energy density capacitor.
The invention provides a novel symmetrical water system hybrid high-voltage capacitor containing the carbon-polymer composite electrode material, which comprises the step of assembling the carbon-polymer composite electrode material, KOH electrolyte and a cellulose diaphragm to obtain the symmetrical water system hybrid high-voltage capacitor.
Compared with the prior art, the invention has the following beneficial effects:
1. the template carbon material grows on the surface of the carbon cloth in situ, the obtained carbon material has the self-supporting characteristic, can be directly used as an electrode material, and avoids the use of a binder compared with a commercial powdery carbon material. Meanwhile, the continuously opened surface is more beneficial to the adhesion of polymer dielectric, the surface area of dielectric energy storage is increased, and the capacity of the capacitor is further increased.
2. The fluoropolymer dielectric effectively blocks electrons from contacting water, increasing the operating voltage of the capacitor. Meanwhile, in the charging and discharging process, the fluoropolymer dielectric has a high dielectric constant, energy can be stored through dipole turnover, and in addition, the polymer after dipole turnover can be used as an active site for ion adsorption, so that the capacitance of the capacitor is improved.
3. As an electrode material of a capacitor, the carbon-polymer composite electrode shows good electrochemical performance, and in 6M KOH electrolyte, the working voltage can reach 2V and is 0.4mA/cm2The specific volume of the alloy reaches 333.3mF/cm under the current density2(ii) a Compared with a pure carbon material electrode without the polymer dielectric medium, the working voltage is improved by 2.5 times, the capacity is improved by 2.14 times, and the energy density is improved by 13 times.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a scanning electron microscope image of a rod array of zinc oxide grown on a carbon cloth prepared in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a self-supporting carbon material prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope of the cross section of the carbon-PVDF-HFP composite electrode prepared in example 1 of the present invention;
FIG. 4 is an optical photograph of the soft-package symmetrical water-based hybrid high-voltage capacitor prepared in example 1 of the present invention;
FIG. 5 is a scanning electron microscope image of a carbon-PVDF composite electrode prepared in example 2 of the present invention before quenching;
FIG. 6 is a scanning electron microscope image of a carbon-PVDF composite electrode prepared in example 2 of the present invention after quenching;
fig. 7 is a graph of energy power density for a carbon-polymer composite electrode and a pure carbon electrode prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The specific preparation process of the carbon-PVDF-HFP symmetrical water system hybrid high-voltage capacitor is as follows:
1. preparation of self-supporting carbon materials
1.1, measuring 70mL of deionized water, and adding 10mL of 30% wt hydrogen peroxide solution and 10mL of 28% wt ammonia solution to prepare a solution A; cutting the carbon cloth into 3 x 3cm2Taking 4 tablets, adding the tablets into the solution A, packaging by using a preservative film, heating at 80 ℃ for 12 hours, taking out, repeatedly washing by using deionized water, and putting into a beaker filled with the deionized water for use;
1.2 the carbon cloth was soaked in 0.005M zinc acetate for 30 minutes and then transferred to a forced air oven at 200 ℃ for 30 minutes to form a ZnO seed layer. Preparing 80mL of 0.05M hexamethylenetetramine and 0.05M zinc nitrate hexahydrate solution, adding 2mL of ammonia water, stirring for 30 minutes to form a solution B, putting the dried carbon cloth into the solution B, transferring the solution B into a hydrothermal reaction kettle, and putting the solution B into a 90 ℃ forced air drying oven for 4 hours; taking out the carbon cloth after the reaction is finished, alternately cleaning the carbon cloth by using deionized water and ethanol to obtain a carbon cloth zinc oxide compound (a scanning electron microscope image of which is shown in figure 1), and drying the carbon cloth zinc oxide compound at 80 ℃ for later use;
1.3 soaking the grown carbon cloth zinc oxide compound in 100mL of 1M glucose solution for 12 hours, taking out and placing in a forced air drying oven, and drying at 80 ℃ for 1 hour;
1.4 putting the dried carbon cloth zinc oxide compound into a porcelain boat, placing the porcelain boat in a tube furnace, heating the porcelain boat to 160 ℃ under 40mL/min argon atmosphere at a heating rate of 1 ℃/min for 1 hour, then heating the porcelain boat to 900 ℃ at a heating rate of 5 ℃/min for 2 hours, naturally cooling the porcelain boat to room temperature, and taking the porcelain boat out;
1.5 putting the carbon cloth zinc oxide compound taken out of the tube furnace into 200mL of 1M HCl for 12 hours to wash away the zinc oxide, repeatedly washing the carbon cloth zinc oxide compound by deionized water until the carbon cloth zinc oxide compound is neutral, and naturally drying the carbon cloth zinc oxide compound to obtain the self-supporting carbon material (the scanning electron microscope picture is shown in figure 2).
2. Preparation of carbon-PVDF-HFP composite electrode
2.1 cutting the carbon material prepared in step 1 into the shape of an electrode (1.5 x 2.8 cm)2)；
2.2 adding 0.15g of PVDF-HFP into 20mL of N, N-dimethylformamide solution, and stirring and dissolving at 80 ℃ to obtain a solution a;
2.3 soaking the electrode material in the solution a, performing rotary evaporation at 80 ℃ until the solution becomes dry, taking out the obtained composite material, placing the composite material in a glass culture dish, and naturally drying for 24 hours;
2.4 placing the composite material in a vacuum drying oven at 200 ℃ for 10 minutes, taking out, immediately putting into ice water, and quenching to obtain the carbon-polymer composite electrode material (the scanning electron microscope image of which is shown in figure 3).
3. Assembly of symmetric water system hybrid high-voltage capacitor
And (3) packaging the carbon-PVDF-HFP composite material obtained in the step (2) by using a cellulose diaphragm and an aluminum plastic film, and assembling a soft-package symmetrical water system hybrid high-voltage capacitor by using 6M KOH as an electrolyte (an optical photograph is shown in FIG. 4).
4. Preparation of comparative sample carbon supercapacitor
And (3) assembling the soft-package symmetrical water system hybrid high-voltage capacitor by using the carbon material obtained in the step (1) as an electrode, using a cellulose diaphragm, packaging by using an aluminum plastic film and using 6M KOH as an electrolyte.
As shown in fig. 7, in the 6M KOH electrolytic solution, the energy density of the capacitor with the composite dielectric is increased by 1300% compared to the carbon material electrode without the polymer electrolyte; the working voltage can reach 2V and is 0.4mA/cm2The specific volume of the alloy reaches 333.3mF/cm under the current density2(ii) a The voltage window of the carbon material without the polyelectrolyte is only 0.8V, and the specific volume under the same current density is only 156.5mF/cm2. Compared with a pure carbon material electrode without the polymer dielectric, the working voltage is improved by 2.5 times, and the capacity is improved by 2.14 times.
Example 2
The specific preparation process of the carbon-PVDF symmetrical water system hybrid high-voltage capacitor is as follows:
1. the preparation of the self-supporting carbon material was consistent with example 1.
2. Preparation of carbon-PVDF composite electrode
2.1 cutting the carbon material prepared in step 1 into the shape of an electrode (1.5 x 2.8 cm)2)；
2.2 adding 0.15g of PVDF into 20mL of N, N-dimethylformamide solution, and stirring and dissolving at 80 ℃ to obtain solution b;
2.3 soaking the electrode material in the solution b, performing rotary evaporation at 80 ℃ until the solution becomes dry, taking out the obtained composite material, placing the composite material in a glass culture dish, and naturally drying for 24 hours (the scanning electron microscope image is shown in figure 5);
2.4 placing the composite material in a vacuum drying oven at 200 ℃ for 10 minutes, taking out, immediately putting into ice water, and quenching to obtain the carbon-polymer composite electrode material (the scanning electron microscope image of which is shown in FIG. 6).
3. Assembly of symmetric water system hybrid high-voltage capacitor
And (3) taking the carbon-PVDF composite material obtained in the step (2) as an electrode, using a cellulose diaphragm, packaging by using an aluminum plastic film, and assembling into a soft-package symmetrical water system hybrid high-voltage capacitor by taking 6M KOH as an electrolyte.
The soft-package symmetrical water system hybrid high-voltage capacitor prepared in the embodiment has the working voltage of 2V and 0.4mA/cm in 6M KOH electrolyte2Under the current density, the specific volume reaches 298.2mF/cm2(ii) a Compared with a pure carbon material electrode without the polymer dielectric medium, the working voltage is improved by 2.5 times, the capacity is improved by 1.9 times, and the energy density is improved by 11.8 times.
It should be noted that such a capacitor cannot be prepared without using the self-supporting carbon material prepared by the method of this embodiment, because the entire electrode is coated with the fluoropolymer material in the method, and if the conventional carbon material is used, the current collector cannot be coated, and the hydrogen evolution and oxygen evolution reactions occur on the current collector.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (8)
1. A carbon-polymer composite electrode material is characterized by comprising a self-supporting carbon material and a polymer dielectric layer coated on the self-supporting carbon material;
the preparation method of the carbon-polymer composite electrode material comprises the following steps:
s1, cutting the self-supporting carbon material into an electrode shape;
s2, adding the fluorine-containing polymer into the N, N-dimethylformamide solution, stirring and dissolving to obtain a solution a;
s3, putting the sheared self-supporting carbon material into the solution a for soaking, performing rotary evaporation under a vacuum condition until the solution is dried to obtain a composite material, and then naturally drying;
s4, after the composite material processed in the step S3 is dried by air blowing, the composite material is taken out and put into ice water for quenching, and the carbon-polymer composite electrode material is obtained;
the preparation method of the self-supporting carbon material comprises the following steps:
A. growing zinc oxide of a nano array on the surface of the hydrophilic carbon cloth through a hydrothermal reaction;
B. b, soaking the carbon cloth zinc oxide compound grown in the step A in a carbon source solution for a certain time, and then taking out and drying;
C. heating the dried carbon cloth zinc oxide compound to 150-;
D. and D, putting the carbon cloth zinc oxide compound taken out in the step C into an acid solution again to wash away zinc oxide, and repeatedly washing the carbon cloth zinc oxide compound to be neutral through deionized water to obtain the self-supporting carbon material.
2. The carbon-polymer composite electrode material according to claim 1, wherein in the step B, the concentration of the carbon source solution is 1M, and the soaking time is 12 hours; the drying temperature is 80 ℃, and the drying time is 1 hour.
3. The carbon-polymer composite electrode material as claimed in claim 1, wherein in the step C, the inert gas is argon gas, and the flow rate is 40 mL/min; the heating rate for heating to 150-180 ℃ is 1 ℃/min, and the heating rate for heating to 800-1000 ℃ is 5 ℃/min.
4. The carbon-polymer composite electrode material according to claim 1 or 2, wherein in step B, the carbon source solution is a glucose solution.
5. The carbon-polymer composite electrode material as claimed in claim 1, wherein in step C, the temperature is maintained at 180 ℃ for 1 hour, and at 1000 ℃ for 2 hours.
6. The carbon-polymer composite electrode material according to claim 1, wherein in the step D, the acid solution is at least one of a hydrochloric acid solution and a sulfuric acid solution.
7. The carbon-polymer composite electrode material according to claim 1, wherein in step S2, the fluorine-containing polymer comprises PVDF-HFP, PVDF; the temperature for stirring and dissolving is 80 ℃;
in step S3, the temperature of the rotary evaporation is 80 ℃; the natural drying time is 24 hours;
in step S4, the temperature of the forced air drying was 200 ℃ and the drying time was 10 minutes.
8. A novel symmetrical water-based hybrid high-voltage capacitor comprising the carbon-polymer composite electrode material of claim 1, wherein the capacitor is obtained by assembling the carbon-polymer composite electrode material, KOH electrolyte and cellulose diaphragm.
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