CN113555229A - Graphene paper current collector, preparation method and supercapacitor - Google Patents
Graphene paper current collector, preparation method and supercapacitor Download PDFInfo
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- CN113555229A CN113555229A CN202010338476.1A CN202010338476A CN113555229A CN 113555229 A CN113555229 A CN 113555229A CN 202010338476 A CN202010338476 A CN 202010338476A CN 113555229 A CN113555229 A CN 113555229A
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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
- H01G11/66—Current collectors
- H01G11/68—Current collectors 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
- H01G11/66—Current collectors
- H01G11/70—Current collectors characterised by their structure
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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
A method of making a graphene paper current collector, the method comprising the steps of: mixing expanded graphite and pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion; adding pure water into the mixture for dilution, adding an active agent, stirring, and mechanically stripping through primary shearing and secondary shearing to obtain mixed slurry; crushing the mixed slurry through a high-pressure homogenization process, and then performing ultrasonic oscillation treatment to obtain graphene mixed slurry; carrying out solid-liquid separation treatment on the graphene mixed slurry by adopting a freeze drying process to obtain graphene powder; and carrying out mould pressing treatment on the graphene powder to obtain the graphene paper current collector. The preparation method of the graphene paper current collector has the advantages that the technological process is simple to operate, the chemical reaction process is avoided, the environment pollution is avoided in green production, the prepared graphene paper current collector has a large specific surface area, the storage capacity of active substances is increased, and the capacity and performance of the super capacitor are greatly improved.
Description
Technical Field
The application relates to the field of electrode materials, in particular to a graphene paper current collector, a preparation method and a super capacitor.
Background
Generally, a supercapacitor is mainly assembled by an electrode active material layer, an electrolyte, a separator, a current collector, a case, and the like. The current collector is a structure or a part for collecting current, and has the main functions of collecting the current generated by the active material of the battery, providing an electronic channel, accelerating charge transfer and improving the coulomb charging and discharging efficiency. The graphene is used as a current collector and has the characteristics of high conductivity, good mechanical property, light weight and the like, and due to the excellent optical, electrical and mechanical properties of graphene, people apply graphene to the current collector. At present, graphene paper on the market is mainly prepared by a chemical method, chemical reagents such as concentrated acid, potassium permanganate, a reducing agent, various organic solvents and the like need to be introduced, the preparation process is complex and has defects, and on one hand, graphene oxide can destroy the conjugated structure of graphene, so that the conductivity and the mechanical property of graphene are greatly reduced; on the other hand, the problem of waste pollution of chemical reagents is involved, and waste acid and alkali in the process can cause environmental pollution and have potential safety hazards.
Disclosure of Invention
In view of this, there is a need to provide a graphene paper current collector, a preparation method thereof, and a supercapacitor, wherein the preparation method is simple, a chemical reaction process is not required, and the prepared graphene paper has excellent electrical and mechanical properties.
The embodiment of the application provides a preparation method of a graphene paper current collector, which comprises the following steps:
mixing expanded graphite and pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion;
adding pure water into the mixture for dilution, adding an active agent, stirring, and mechanically stripping through primary shearing and secondary shearing to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenization process, and then performing ultrasonic oscillation treatment to obtain graphene mixed slurry;
carrying out solid-liquid separation treatment on the graphene mixed slurry by adopting a freeze drying process to obtain graphene powder;
and carrying out mould pressing treatment on the graphene powder to obtain the graphene paper current collector.
Further, in some embodiments of the present application, the predetermined ratio is 1:2 to 1: 3.
Further, in some embodiments herein, the active agent is a combination of polyvinylpyrrolidone and sodium cholate, with the polyvinylpyrrolidone and sodium cholate added in a 2:1 ratio.
Further, in some embodiments of the present application, the total amount of the active agent added is 1% o to 1.5% o.
Further, in some embodiments of the present application, pure water is added to the mixture for dilution, wherein the concentration of the mixture is 7.5% to 12%.
Further, in some embodiments of the present application, the rotation speed of the low-speed stirring is 40-80 rpm, the rotation speed of the high-speed dispersing is 1500-4000 rpm, the rotation speed of the primary shearing is 3000-6000 rpm, the shearing time is 2-3 h, the rotation speed of the secondary shearing is 8000-14000 rpm, and the shearing time is 8-20 h.
Further, in some embodiments of the present application, the pressure of the high-pressure homogenization treatment is 750 to 1800bar, and the number of cycles is 15 to 25.
Further, in some embodiments of the present application, the freeze-drying process comprises:
freezing the graphene mixed slurry subjected to ultrasonic oscillation treatment to below-45 ℃, heating and sublimating, raising the temperature to 5-8 ℃ per hour, and preserving the temperature for 2 hours after the temperature reaches 35 ℃ to obtain graphene powder.
The embodiment of the application also provides the graphene paper current collector prepared by the preparation method of the graphene paper current collector, wherein the specific surface area of the graphene paper current collector is 1450-1500 square meters per gram.
The embodiment of the application also provides a super capacitor, adopts the aforesaid graphite alkene paper mass flow body to make, super capacitor's voltage is 2.7-4V, and volume energy density is 16 ~ 25 Wh/L.
According to the preparation method of the graphene paper current collector, the technical process is simple to operate, a chemical reaction process is avoided, the conjugate structure of graphene is prevented from being damaged by chemical reagents, the conductivity and the mechanical property of graphene are greatly reduced, pollutants such as waste acid and alkali do not need to be treated, environmental pollution is avoided in green production, the prepared graphene paper current collector has a large specific surface area, the storage capacity of active substances is increased, and the capacity and the performance of the supercapacitor are greatly improved.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "or/and" includes any and all combinations of one or more of the associated listed items.
The embodiment of the application provides a preparation method of a graphene paper current collector, which comprises the following steps:
mixing expanded graphite and pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion;
adding pure water into the mixture for dilution, adding an active agent, stirring, and mechanically stripping through primary shearing and secondary shearing to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenization process, and then performing ultrasonic oscillation treatment to obtain graphene mixed slurry;
carrying out solid-liquid separation treatment on the graphene mixed slurry by adopting a freeze drying process to obtain graphene powder;
and carrying out mould pressing treatment on the graphene powder to obtain the graphene paper current collector.
The embodiment of the application also provides the graphene paper current collector prepared by the preparation method of the graphene paper current collector, wherein the specific surface area of the graphene paper current collector is 1450-1500 square meters per gram.
The embodiment of the application also provides a super capacitor, adopts the aforesaid graphite alkene paper mass flow body to make, super capacitor's voltage is 2.7-4V, and volume energy density is 16 ~ 25 Wh/L.
According to the preparation method of the graphene paper current collector, the technical process is simple to operate, a chemical reaction process is avoided, the conjugate structure of graphene is prevented from being damaged by chemical reagents, the conductivity and the mechanical property of graphene are greatly reduced, pollutants such as waste acid and alkali do not need to be treated, environmental pollution is avoided in green production, the prepared graphene paper current collector has a large specific surface area, the storage capacity of active substances is increased, and the capacity and the performance of the supercapacitor are greatly improved.
Some embodiments of the present application will be described in detail below.
The preparation method of the graphene paper current collector in an embodiment of the application specifically includes the following steps:
s11, mixing the expanded graphite with pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion;
s12, adding pure water into the mixture for dilution, adding an active agent, stirring, and mechanically stripping through primary shearing and secondary shearing to obtain mixed slurry;
s13, crushing the mixed slurry through a high-pressure homogenization process, and then performing ultrasonic oscillation treatment to obtain graphene mixed slurry;
s14, performing solid-liquid separation treatment on the graphene mixed slurry by adopting a freeze drying process to obtain graphene powder;
and S15, carrying out mould pressing treatment on the graphene powder to obtain the graphene paper current collector. In one embodiment, the graphene paper current collector has a specific surface area of 1450-1500 square meters per gram.
In one embodiment, the predetermined ratio in step S11 is 1:2 to 1:3, preferably 1: 2.
In one embodiment, the low-speed stirring in step S11 is performed at a rotation speed of 40 to 80rpm, the high-speed dispersing is performed at a rotation speed of 1500 to 4000rpm, and the stirring and dispersing are performed simultaneously for at least two hours, so as to prepare a uniformly mixed high-concentration material. In one embodiment, the expanded graphite has a mesh size of 1500 to facilitate mechanical exfoliation.
In one embodiment, pure water is added to the mixture to dilute the mixture to 7.5% to 12% in the step S12. The rotating speed of the primary shearing is 3000-6000 rpm, the rotating speed of the secondary shearing is 8000-14000 rpm, the shearing time is 2-3 h, and the shearing time is 8-20 h. In the mixed slurry after mechanical stripping, the solid phase volume rapidly expands and has higher surface energy. Due to the fact that agglomeration can occur in the mixture under a stable state, the agglomeration of graphene can be avoided by adding a proper amount of active agent. In one embodiment, the active agent is a combination of polyvinylpyrrolidone and sodium cholate, the total addition amount is 1-1.5%, and the addition ratio of the polyvinylpyrrolidone to the sodium cholate is 2: 1.
In one embodiment, in step S13, the high-pressure homogenizing process is performed by a high-pressure homogenizer, the high-pressure homogenizing process is composed of an external circulation pipeline, and the homogenizing process result can be controlled by the number of cycles. The high-pressure homogenization can improve the liquid phase stability of the mixed slurry, further reduce the distribution width of the sheet diameter size of the graphene, and is beneficial to preparing the graphene current collector with excellent electrical and mechanical properties. In one embodiment, the homogenization treatment pressure is 750-1800 bar, and the cycle time is 15-25 times, so that the comprehensive efficiency of the uniformity degree and the treatment time of the graphene slurry can achieve the best effect.
In one embodiment, the power of the ultrasonic oscillation treatment in step S13 is 15 to 24kw, and the temperature control is paid attention to the ultrasonic process to avoid high-temperature graphene agglomeration. And the ultrasonic vibration treatment is used for dispersing and crushing, so that the graphite sheet layer is further opened, and more single-layer graphene is produced. In one embodiment, the sonication process control temperature is not higher than 38 ℃.
And the step S14 of freeze-drying specifically comprises the steps of freezing the graphene mixed slurry subjected to ultrasonic oscillation treatment to a temperature below-45 ℃, heating and sublimating, raising the temperature by 5-8 ℃ per hour, keeping the temperature for 2 hours when the temperature reaches 35-37 ℃, obtaining graphene powder, and drying and storing. The freezing temperature is preferably-46 ℃ and the warming temperature is preferably 35 ℃.
In one embodiment, the pressure of the compression molding process in the step S15 is 10 to 35 MP.
In one embodiment, the specific surface area of the obtained graphene paper current collector is 1450-1500 square meters per gram, the voltage of a super capacitor prepared from the graphene paper current collector is 2.7-4V, and the volume energy density is 16-25 Wh/L.
The present application will be further described with reference to specific examples. It should be understood that the detailed description and specific examples, while indicating the present application, are given by way of illustration and explanation only, and are not intended to limit the present application.
Example 1
Mixing 3kg of 1500-mesh expanded graphite with 6L of pure water, and stirring at a low speed of 60rpm and a high speed of 2000rpm to obtain a mixture;
adding pure water into the mixture for dilution to reach a concentration of 7.5%, adding 48g of polyvinylpyrrolidone and sodium cholate in total, wherein the amount of polyvinylpyrrolidone is 32g, and the amount of sodium cholate is 16g, stirring, and then performing primary shearing and secondary shearing, wherein the primary shearing rotation speed is 5000rpm, the shearing time is 2h, the secondary shearing rotation speed is 12000rpm, and the shearing time is 3h, so as to perform mechanical stripping to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, wherein the homogenizing pressure is 1500bar, performing cyclic treatment for 18 times, then performing ultrasonic oscillation treatment to obtain graphene mixed slurry, performing solid-liquid separation treatment on the graphene mixed slurry through a freeze drying process to obtain graphene powder, and performing mould pressing treatment on the graphene powder under 18Mpa to obtain a graphene paper current collector, wherein the specific surface area of the graphene paper current collector is 1480 square meter/g, the voltage of the prepared super capacitor is 4.0V, and the volume energy density is 25 Wh/L.
Example 2
Mixing 3kg of 1500-mesh expanded graphite with 6L of pure water, and stirring at a low speed of 60rpm and a high speed of 2000rpm to obtain a mixture;
adding pure water into the mixture for dilution, diluting to 10% concentration, adding 37.5g of polyvinylpyrrolidone and sodium cholate in total, wherein the amount of polyvinylpyrrolidone is 25g, and the amount of sodium cholate is 12.5g, stirring, and then performing primary shearing and secondary shearing, wherein the primary shearing rotation speed is 5000rpm, the shearing time is 2.5h, the secondary shearing rotation speed is 12000rpm, and the shearing time is 4h, so as to perform mechanical stripping to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, performing cyclic treatment for 18 times under the homogenizing pressure of 1300bar, performing ultrasonic oscillation treatment to obtain graphene mixed slurry, performing solid-liquid separation treatment on the graphene mixed slurry through a freeze drying process to obtain graphene powder, and performing mould pressing treatment on the graphene powder under 18Mpa to obtain a graphene paper current collector, wherein the specific surface area of the graphene paper current collector is 1460 square meters per gram, the voltage of the prepared super capacitor is 3.8V, and the volume energy density is 22 Wh/L.
Example 3
Mixing 3kg of 1500-mesh expanded graphite with 6L of pure water, and stirring at a low speed of 60rpm and a high speed of 2000rpm to obtain a mixture;
adding pure water into the mixture for dilution, diluting to 12% concentration, adding 30g of polyvinylpyrrolidone and sodium cholate in total, wherein the amount of polyvinylpyrrolidone is 20g, and the amount of sodium cholate is 10g, stirring, and then performing primary shearing and secondary shearing, wherein the primary shearing rotation speed is 5000rpm, the shearing time is 3h, the secondary shearing rotation speed is 12000rpm, and the shearing time is 4h, so as to perform mechanical stripping to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, performing cyclic treatment for 15 times at a homogenizing pressure of 1600bar, performing ultrasonic oscillation treatment to obtain graphene mixed slurry, performing solid-liquid separation treatment on the graphene mixed slurry through a freeze drying process to obtain graphene powder, and performing mould pressing treatment on the graphene powder under 18Mpa to obtain a graphene paper current collector, wherein the specific surface area of the graphene paper current collector is 1450 square meters per gram, the voltage of the prepared super capacitor is 3.7V, and the volume energy density is 20 Wh/L.
The preparation method of the graphene paper current collector has the advantages that the technological process is simple to operate, no chemical reaction process exists, the yield is high, chemical reagents are prevented from damaging the conjugated structure of graphene, the conductivity and the mechanical property of the graphene are greatly reduced, pollutants such as waste acid and alkali do not need to be treated, the green production is free of environmental pollution, the prepared graphene paper current collector has a large specific surface area, the storage capacity of active substances is increased, and the capacity and the performance of the super capacitor are greatly improved.
It should be understood by those skilled in the art that the above embodiments are only for illustrating the present application and are not used as limitations of the present application, and that suitable changes and modifications of the above embodiments are within the scope of the present application as claimed.
Claims (10)
1. A preparation method of a graphene paper current collector is characterized by comprising the following steps: the method comprises the following steps:
mixing expanded graphite and pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion;
adding pure water into the mixture for dilution, adding an active agent, stirring, and mechanically stripping through primary shearing and secondary shearing to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenization process, and then performing ultrasonic oscillation treatment to obtain graphene mixed slurry;
carrying out solid-liquid separation treatment on the graphene mixed slurry by adopting a freeze drying process to obtain graphene powder;
and carrying out mould pressing treatment on the graphene powder to obtain the graphene paper current collector.
2. The method of preparing a graphene paper current collector of claim 1, wherein: the predetermined ratio is 1: 2-1: 3.
3. The method of preparing a graphene paper current collector of claim 1, wherein: the active agent is a combination of polyvinylpyrrolidone and sodium cholate, and the adding ratio of the polyvinylpyrrolidone to the sodium cholate is 2: 1.
4. The method of preparing a graphene paper current collector of claim 1, wherein: the total addition amount of the active agent is 1-1.5 per mill.
5. The method of preparing a graphene paper current collector of claim 1, wherein: and adding pure water into the mixture for dilution, wherein the concentration of the mixture is 7.5-12%.
6. The method of preparing a graphene paper current collector of claim 1, wherein: the low-speed stirring rotating speed is 40-80 rpm, the high-speed dispersing rotating speed is 1500-4000 rpm, the primary shearing rotating speed is 3000-6000 rpm, the shearing time is 2-3 h, the secondary shearing rotating speed is 8000-14000 rpm, and the shearing time is 8-20 h.
7. The method of preparing a graphene paper current collector of claim 1, wherein: the pressure of the high-pressure homogenizing treatment is 750-1800 bar, and the circulation times are 15-25 times.
8. The method of preparing a graphene paper current collector of claim 1, wherein: the freeze drying process comprises the following steps:
and (3) freezing the graphene mixed slurry subjected to ultrasonic oscillation treatment to at least-45 ℃, heating and sublimating, raising the temperature to 5-8 ℃ per hour, keeping the temperature for 2 hours after the temperature reaches 35-37 ℃, and obtaining the graphene powder.
9. A graphene paper current collector prepared by the method for preparing a graphene paper current collector according to any one of claims 1 to 8, wherein: the specific surface area of the graphene paper current collector is 1450-1500 square meters per gram.
10. A supercapacitor, characterized by: the graphene paper current collector is prepared by adopting the graphene paper current collector as claimed in claim 9, the voltage of the super capacitor is 2.7-4V, and the volume energy density is 16-25 Wh/L.
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