CN106981375B - Preparation method of ultrahigh-power high-capacity carbon aerogel double electric layer capacitor monomer - Google Patents
Preparation method of ultrahigh-power high-capacity carbon aerogel double electric layer capacitor monomer Download PDFInfo
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- CN106981375B CN106981375B CN201710177773.0A CN201710177773A CN106981375B CN 106981375 B CN106981375 B CN 106981375B CN 201710177773 A CN201710177773 A CN 201710177773A CN 106981375 B CN106981375 B CN 106981375B
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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
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- H01G11/84—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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- 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 relates to the technical field of double electric layer capacitors, in particular to a preparation method of an ultrahigh-power high-capacity carbon aerogel super capacitor monomer. The preparation method comprises the following steps: mixing and stirring the carbon aerogel and the binder uniformly, rolling the mixture into a carbon film, and rolling the carbon film onto a current collector to form an electrode; cutting the electrode into a strip shape or punching the electrode into a rectangular electrode with a tab; and (3) taking cellulose paper as a diaphragm, forming a battery cell by using the strip-shaped or rectangular electrode, and performing post-treatment to obtain the double-electric-layer capacitor monomer. The method has the advantages of simple preparation process, strong practicability and easy realization of industrial production, and the produced double electric layer capacitor has higher energy density.
Description
Technical Field
The invention relates to the technical field of double electric layer capacitors, in particular to a preparation method of an ultrahigh-power high-capacity carbon aerogel super capacitor monomer.
Background
The Electric Double Layer Capacitor (EDLC) has high power characteristics, can provide strong pulse power, has high energy conversion rate, good high-low temperature characteristics, long cycle life, no maintenance, and good performance and economic applicability, and thus has wide application in the fields of tramcar energy storage systems, trolley bus energy storage systems, energy storage charging stations, subway line energy storage systems, wind power generation, vehicle start and stop, heavy machinery, and the like. However, because the EDLC adopts the traditional activated carbon as an electrode, the internal resistance of the monomer of the EDLC is high, and the power density of the monomer only reaches 15kW/kg (Maxwell company in the United states). In order to improve the power density of the monomer, although materials such as highly conductive graphene and carbon nanotubes are used to replace activated carbon, many reports have been made, but the low-density graphene and carbon nanotubes do not really replace the activated carbon, are only used in combination with the activated carbon, or are not made into a single-use high-capacity EDLC monomer, and the price of the graphene and the carbon nanotubes is high.
Disclosure of Invention
The invention aims to increase the power of a double electric layer capacitor monomer and provides a preparation method of an ultrahigh-power high-capacity carbon aerogel supercapacitor monomer. The method has the advantages of simple preparation process, strong practicability and easy realization of industrial production, and the produced double electric layer capacitor has higher energy density.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a single body of an ultrahigh-power high-capacity carbon aerogel double electric layer capacitor comprises the following steps:
(1) mixing and stirring the carbon aerogel and the binder uniformly, rolling the mixture into a carbon film, and rolling the carbon film onto a current collector to form an electrode;
(2) cutting the electrode into a strip shape or punching the electrode into a rectangular electrode with a tab;
(3) and (3) taking cellulose paper as a diaphragm, forming a battery cell by using the strip-shaped or rectangular electrode, and performing post-treatment to obtain the double-electric-layer capacitor monomer.
In the prior art, when an electrode is prepared by using activated carbon, some conductive agents are required to be added into the electrode to improve the conductivity because of the high internal resistance of the activated carbon electrode. However, in the invention, the carbon aerogel has a very high specific surface area, and the conductivity test result shows that the carbon aerogel has very high and stable conductivity in a very wide temperature range (50K-300K), so the carbon aerogel is an electrode material of an electric double layer capacitor which can be used in a wide temperature range, has good conductivity, can be directly mixed with a binder and rolled to a current collector to form an electrode without adding a conductive agent additionally, and can form a capacitor with high capacity by combining with a subsequent preparation process.
Preferably, the mass fractions of the carbon aerogel and the binder in the step (1) are 85% -90% and 10% -15%, respectively. The ratio of the electrode active substance to the binder has obvious influence on the capacitance of a final product, the contact between carbon aerogel particles can be reduced due to the overhigh content of the insulated binder, so that the electronic conductivity of the electrode is reduced, the content of the binder is too low, the adhesion effect is poor, and the carbon aerogel is easy to fall off from a current collector.
Preferably, the carbon aerogel has a specific surface area higher than 2400m2G, pore volume is more than 1.56cm3Activated carbon aerogel in/g. Carbon aerogel is an active material for preparing an electric double layer capacitor, and theoretically, the capacitance value of the electric double layer is in direct proportion to the specific surface area and the pore volume of the carbon aerogel, so that the selection of proper carbon aerogel is very important for the performance of the capacitor.
Preferably, the binder is a mixture of polyvinylidene fluoride (PVDF), sodium carboxymethylcellulose (CMC) and Polytetrafluoroethylene (PTFE), and the mass fractions of the polyvinylidene fluoride, the sodium carboxymethylcellulose and the polytetrafluoroethylene are respectively (5% -20%), (5% -20%) and (60% -90%). The single component as the binder has advantages and disadvantages, such as that PTFE can effectively prevent electrode active substances from falling off in the binding process, and the smooth surface of particles is beneficial to the infiltration of electrolyte, thereby improving the capacity of the capacitor, but the PTFE has excellent insulation property, so that the PTFE can be used as the binder to cause the resistance between carbon aerogel particles to increase; PVDF has good thermal stability and is easy to disperse, but the prepared electrode has poor conductivity and mechanical property; CMC is highly elastic and polar, but has poor bonding properties. The three components are mixed according to a certain proportion, and the minimum using amount of the binder is used, so that the internal resistance of the capacitor electrode is lower on the basis of obtaining excellent electrode strength and adhesion, and the capacitance of the capacitor is increased to the maximum extent.
Preferably, the mass fractions of the polyvinylidene fluoride, the sodium carboxymethylcellulose and the polytetrafluoroethylene are 10%, 10% and 80%, respectively.
Preferably, the current collector in step (1) is chemically etched aluminum foil. Aluminum foil is treated at 70-90 ℃ under 2mol/L HCl +0.2mol/L Al2(SO4)3The mixed solution is etched for 60-80 s. The surface of the aluminum foil is etched, so that the surface roughness of the aluminum foil can be increased, the carbon aerogel can enter etching pores of the aluminum foil more easily, and the contact resistance between the carbon aerogel and a current collector is reduced, so that the resistance is reduced.
Preferably, the thickness of the carbon film in the step (1) is 100-120 μm.
Preferably, the pressure for rolling in step (1) is 100-300 MPa. The magnitude of the pressure in the present invention affects the thickness, density and compactness of the final carbon film. If the pressure is too small, the carbon film has larger gaps, lower density and thicker electrode; on the contrary, the pressure is too high, and the carbon film is wrinkled or even cracked.
Cutting the electrodes into strip-shaped electrodes with the diameter of 120mm multiplied by 4mm in the step (2), winding the two strip-shaped electrodes into a battery cell by a winding machine, drying (150 ℃, 10h), welding terminals, entering a shell, sealing, injecting vacuum at night, and welding an injection port to prepare a round EDLC monomer with the diameter of 60mm multiplied by 140 mm; or punching the electrodes into 210mm × 60mm rectangular electrodes with tabs, fully automatically laminating the rectangular electrodes into a 100-pair electrode cell, drying (150 ℃, 10h), welding terminals, filling into a shell, sealing, vacuum-injecting liquid, and encapsulating an injection port to obtain the 220mm × 80mm × 60mm square EDLC monomer.
Compared with the prior art, the invention has the beneficial effects that:
1) the withstand voltage of the EDLC monomer can reach 3V;
2) the circular EDLC monomer capacity is higher than 3800F, and the power density is higher than 35 kW/kg;
3) the square EDLC monomer capacity is higher than 13000F, and the power density is higher than 22 kW/kg;
4) circular EDLC cells can withstand 100A current cycling life tests; square EDLC cells can withstand 200A current cycling life test;
5) the dry method is adopted to prepare the electrode, and then the capacitor is prepared, so that the whole preparation process is simple and easy to industrialize.
Drawings
FIG. 1 is a scanning electron micrograph of a carbon aerogel according to example 1.
Fig. 2 shows a circular electric double layer capacitor cell manufactured in example 1.
FIG. 3 shows a square-shaped electric double layer capacitor cell obtained in example 2.
Detailed Description
The technical solution of the present invention is further described below by means of specific embodiments and accompanying drawings. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1:
the specific surface area is 2570m2G, pore volume of 1.66cm3Mixing carbon aerogel in per gram (the scanning electron microscope image of the carbon aerogel is shown in figure 1, a carbon aerogel sample presents a continuous porous network structure) with dry binder powder, wherein the mass fractions of the carbon aerogel and the binder are 90% and 10%, respectively, stirring the mixed powder for 6 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a 110 mu m carbon film by using a double-roller machine under 200MPa, and horizontally rolling the carbon film onto two sides of an etched aluminum foil to form a high-density electrode. Cutting a high-density electrode of a splitting machine into strip electrodes with the thickness of 120mm multiplied by 4mm, then taking cellulose paper as a diaphragm, winding the two strip electrodes into a battery cell by a winding machine, drying (150 ℃, 10h), welding terminals, entering a shell, sealing, injecting liquid in vacuum, and welding a liquid injection port to obtain the circular EDLC monomer with the thickness of 60mm multiplied by 140 mm. A circular EDLC monomer sample is shown in figure 2.
In the range of 1.5-3V, a 100A constant current charge and discharge is adopted to test the circular EDLC monomer: the monomer capacity was 3861F, the power density was 37kW/kg, and the capacity retention rate after 1 ten thousand cycles was 97%.
Example 2
The specific surface area is 2570m2G, pore volume of 1.66cm3Mixing carbon aerogel and binder dry powder in a mass ratio of 90% and 10% respectively, stirring the mixed powder for 6 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a 110 mu m carbon film by using a double-roller machine under 200MPa, and horizontally rolling the carbon film to the two sides of the corroded aluminum foil to form the high-density electrode. Punching a high-density electrode into a 210mm multiplied by 60mm rectangular electrode with a tab by using a punching machine, then stacking the rectangular electrode into a 100-pair electrode cell by using cellulose paper as a diaphragm through full-automatic lamination, drying (150 ℃, 10h), welding a terminal, entering a shell, sealing, injecting liquid in vacuum, and encapsulating an injection port to obtain a 220mm multiplied by 80mm multiplied by 60mm square EDLC monomer. A square EDLC monomer sample is shown in figure 3.
In the range of 1.5-3V, a 200A constant current charge-discharge test square EDLC monomer is adopted: the monomer capacity was 13978F, the power density was 24kW/kg, and the capacity retention rate after 1 ten thousand cycles was 98%.
Example 3:
the specific surface area is 2450m2G, pore volume of 1.62cm3Mixing the carbon aerogel and the binder dry powder in a ratio of 85% to 15% by mass, stirring the mixed powder for 5 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a carbon film of 120 mu m by using a double-roller machine under 300MPa, and horizontally rolling the carbon film to the two sides of the corroded aluminum foil to form the high-density electrode. Cutting a high-density electrode of a splitting machine into strip electrodes with the thickness of 120mm multiplied by 4mm, then taking cellulose paper as a diaphragm, winding the two strip electrodes into a battery cell by a winding machine, drying (150 ℃, 10h), welding terminals, entering a shell, sealing, injecting liquid in vacuum, and welding a liquid injection port to obtain the circular EDLC monomer with the thickness of 60mm multiplied by 140 mm.
In the range of 1.5-3V, a 100A constant current charge and discharge is adopted to test the circular EDLC monomer: the monomer capacity is 3815F, the power density is 35kW/kg, and the capacity retention rate is 98% after 1 ten thousand cycles.
Example 4
The specific surface area is 2450m2G, pore volume of 1.62cm3Mixing the carbon aerogel and the binder dry powder in a ratio of 85% to 15% by mass, stirring the mixed powder for 5 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a carbon film of 120 mu m by using a double-roller machine under 300MPa, and horizontally rolling the carbon film to the two sides of the corroded aluminum foil to form the high-density electrode. Punching a high-density electrode into a 210mm multiplied by 60mm rectangular electrode with a tab by using a punching machine, then stacking the rectangular electrode into a 100-pair electrode cell by using cellulose paper as a diaphragm through full-automatic lamination, drying (150 ℃ for 10h), welding a terminal, entering a shell, sealing, injecting liquid in vacuum, and encapsulating an injection port to obtain a 220mm multiplied by 80mm multiplied by 60mm square EDLC monomer.
In the range of 1.5-3V, a 200A constant current charge-discharge test square EDLC monomer is adopted: the monomer capacity is 13654F, the power density is 25kW/kg, and the capacity retention rate is 97% after 1 ten thousand cycles.
Example 5:
the specific surface area is 2810m2G, pore volume of 1.71cm3Mixing the carbon aerogel and the binder dry powder in an amount of 87% and 13% by mass respectively, stirring the mixed powder for 7 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a 108-micrometer carbon film under 150MPa by using a double-roller machine, and horizontally rolling the carbon film to the two sides of the corroded aluminum foil to form the high-density electrode. Cutting a high-density electrode of a splitting machine into strip-shaped electrodes with the thickness of 120mm multiplied by 4mm, then taking cellulose paper as a diaphragm, winding the two strip-shaped electrodes into a battery cell by a winding machine, drying (150 ℃, 10h), welding terminals, entering a shell, sealing, injecting liquid in vacuum, and welding a liquid injection port to obtain a round EDLC monomer with the thickness of 60mm multiplied by 140 mm;
in the range of 1.5-3V, a 100A constant current charge and discharge is adopted to test the circular EDLC monomer: the monomer capacity is 3924F, the power density is 38kW/kg, and the capacity retention rate is 97% after 1 ten thousand cycles.
Example 6
The specific surface area is 2810m2G, pore volume of 1.71cm3Mixing the carbon aerogel and the binder dry powder in an amount of 87% and 13% by mass respectively, stirring the mixed powder for 7 hours by using a high-speed shearing dispersion machine, rolling the mixed powder into a 108-micrometer carbon film under 150MPa by using a double-roller machine, and horizontally rolling the carbon film to the two sides of the corroded aluminum foil to form the high-density electrode. Punching a high-density electrode into a 210mm multiplied by 60mm rectangular electrode with a tab by using a punching machine, then stacking the rectangular electrode into a 100-pair electrode cell by using cellulose paper as a diaphragm through full-automatic lamination, drying (150 ℃, 10h), welding a terminal, entering a shell, sealing, injecting liquid in vacuum, and encapsulating an injection port to obtain a 220mm multiplied by 80mm multiplied by 60mm square EDLC monomer.
In the range of 1.5-3V, a 200A constant current charge-discharge test square EDLC monomer is adopted: the monomer capacity was 13324F, the power density was 26kW/kg, and the capacity retention rate after 1 ten thousand cycles was 96%.
The binders used in examples 1-6 were a mixture of polyvinylidene fluoride, sodium carboxymethylcellulose and polytetrafluoroethylene in mass fractions of 10%, 10% and 80%, respectively.
Comparative example 1
Comparative example 1 differs from example 1 only in that the carbon aerogel of comparative example 1 has a specific surface area of 2300m2Per g, pore volume of 1.51cm3The rest is similar to example 1 and is not repeated herein.
In the range of 1.5-3V, a 100A constant current charge and discharge is adopted to test the circular EDLC monomer: the monomer capacity is 2956F, the power density is 31kW/kg, and the capacity retention rate is 78% after 1 ten thousand cycles.
Comparative example 2
Comparative example 1 is different from example 2 only in that the binder of comparative example 2 is polyvinylidene fluoride, and the rest is similar to example 2 and is not described in detail herein.
In the range of 1.5-3V, a 200A constant current charge-discharge test square EDLC monomer is adopted: the monomer capacity is 10078F, the power density is 18kW/kg, and the capacity retention rate is 75% after 1 ten thousand cycles.
In addition, the technical scope of the invention is not exhaustive, and new technical solutions formed by equivalent replacement of single or multiple technical features in the embodiment technical solutions are also within the scope of the invention; meanwhile, in all the embodiments of the invention, which are listed or not listed, each parameter in the same embodiment represents only one example (i.e., a feasible solution) of the technical scheme.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (3)
1. A preparation method of a single ultrahigh-power high-capacity carbon aerogel double electric layer capacitor is characterized by comprising the following steps of:
(1) mixing and stirring the carbon aerogel and the binder uniformly, rolling the mixture into a carbon film, and rolling the carbon film onto a current collector to form an electrode;
(2) cutting the electrode into a strip shape or punching the electrode into a rectangular electrode with a tab;
(3) taking cellulose paper as a diaphragm, forming a strip-shaped or rectangular electrode into a cell, and performing post-treatment to obtain a double electric layer capacitor monomer;
the binder is a mixture of polyvinylidene fluoride, sodium carboxymethylcellulose and polytetrafluoroethylene, and the mass fractions of the polyvinylidene fluoride, the sodium carboxymethylcellulose and the polytetrafluoroethylene are respectively 10%, 10% and 80%;
the current collector in the step (1) is a chemically etched corrosion aluminum foil, and the aluminum foil is subjected to 2mol/L HCl +0.2mol/L Al at the temperature of 70-90 DEG C2(SO4)3Etching in the mixed solution for 60-80 s;
the mass fractions of the carbon aerogel and the binder in the step (1) are 85-90% and 10-15% respectively;
the carbon aerogel has a specific surface area higher than 2400m2G, pore volume is more than 1.56cm3Activated carbon aerogel in/g.
2. The method for preparing an ultra-high power large capacity carbon aerogel electric double layer capacitor monomer as claimed in claim 1, wherein the thickness of the carbon film in step (1) is 100-120 μm.
3. The method for preparing an ultra-high power large capacity carbon aerogel electric double layer capacitor monomer as claimed in claim 1, wherein the pressure for rolling in step (1) is 100-300 MPa.
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