CN113555229B - Graphene paper current collector, preparation method and supercapacitor - Google Patents
Graphene paper current collector, preparation method and supercapacitor Download PDFInfo
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- CN113555229B CN113555229B CN202010338476.1A CN202010338476A CN113555229B CN 113555229 B CN113555229 B CN 113555229B CN 202010338476 A CN202010338476 A CN 202010338476A CN 113555229 B CN113555229 B CN 113555229B
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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 for preparing a graphene paper current collector, the method comprising the steps of: mixing the expanded graphite with 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 homogenizing process, and then performing ultrasonic vibration 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. According to the preparation method of the graphene paper current collector, the technological process is simple to operate, the chemical reaction process is avoided, the environment-friendly production is realized, 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 supercapacitor 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 supercapacitor.
Background
Generally, the super capacitor is mainly assembled by an electrode active material layer, an electrolyte, a separator film, a current collector, a shell and the like. The current collector is a structure or part for collecting current, and has the main functions of collecting the current generated by the active substances of the battery, providing an electronic channel, accelerating charge transfer and improving charge-discharge coulomb efficiency. As a current collector, the characteristics of high conductivity, good mechanical properties, light weight and the like need to be satisfied, and due to the excellent optical, electrical and mechanical properties of graphene, graphene is applied to the current collector. At present, the graphene paper on the market mainly adopts a chemical method preparation route, chemical reagents such as concentrated acid, potassium permanganate, reducing agents, various organic solvents and the like are required to be introduced, the preparation link is complex, and defects exist, on one hand, graphene oxide can damage the conjugated structure of the graphene, so that the conductivity and mechanical properties of the graphene are greatly reduced; on the other hand, the problems of chemical reagent waste pollution are related, waste acid and alkali in the process can cause environmental pollution, and potential safety hazards exist at the same time.
Disclosure of Invention
In view of the above, it is necessary to provide a graphene paper current collector, a preparation method thereof and a supercapacitor, wherein the preparation method is simple, no chemical reaction process exists, 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 the expanded graphite with 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 homogenizing process, and then performing ultrasonic vibration 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 of the present application, the active agent is a combination of polyvinylpyrrolidone and sodium cholate, and the addition ratio of polyvinylpyrrolidone to sodium cholate is 2:1.
Further, in some embodiments of the present application, the total amount of the active agent added is 1 to 1.5%.
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% -12%.
Further, in some embodiments of the present application, the low speed stirring is at a speed of 40 to 80rpm, the high speed dispersing is at a speed of 1500 to 4000rpm, the primary shearing is at a speed of 3000 to 6000rpm, the shearing time is 2 to 3 hours, the secondary shearing is at a speed of 8000 to 14000rpm, and the shearing time is 8 to 20 hours.
Further, in some embodiments of the present application, the high pressure homogenization treatment is performed at a pressure of 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 vibration treatment to below-45 ℃, heating and sublimating, heating to 5-8 ℃ per hour, and preserving heat for 2 hours after reaching 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, and 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 which is manufactured by adopting the graphene paper current collector, wherein the voltage of the super capacitor is 2.7-4V, and the volume energy density is 16-25 Wh/L.
According to the preparation method of the graphene paper current collector, the technological process is simple to operate, the chemical reaction process is avoided, the chemical reagent is prevented from damaging the conjugated structure of graphene, the conductivity and mechanical property of graphene are greatly reduced, and pollutants such as waste acid and alkali are not required to be treated, so that environment-friendly production is realized, 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 supercapacitor are greatly improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
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 application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "or/and" as used herein 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 the expanded graphite with 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 homogenizing process, and then performing ultrasonic vibration 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, and 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 which is manufactured by adopting the graphene paper current collector, wherein the voltage of the super capacitor is 2.7-4V, and the volume energy density is 16-25 Wh/L.
According to the preparation method of the graphene paper current collector, the technological process is simple to operate, the chemical reaction process is avoided, the chemical reagent is prevented from damaging the conjugated structure of graphene, the conductivity and mechanical property of graphene are greatly reduced, and pollutants such as waste acid and alkali are not required to be treated, so that environment-friendly production is realized, 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 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 the embodiment of the application specifically comprises the following steps:
s11, mixing the expanded graphite and 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 homogenizing process, and then performing ultrasonic vibration treatment to obtain graphene mixed slurry;
s14, carrying out 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 specific surface area of the graphene paper current collector is 1450-1500 square meters per gram.
In one embodiment, the predetermined ratio in the step S11 is 1:2 to 1:3, preferably 1:2.
In one embodiment, the low-speed stirring in the step S11 is performed at a rotation speed of 40-80 rpm, the high-speed dispersing is performed at a rotation speed of 1500-4000 rpm, and the stirring and dispersing are performed simultaneously for at least two hours, so as to prepare the uniformly mixed high-concentration material. In one embodiment, the expanded graphite has a mesh number of 1500, facilitating mechanical exfoliation.
In one embodiment, in the step S12, pure water is added into the mixture to dilute the mixture to 7.5% -12%. 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. In the mixed slurry after mechanical stripping, the solid phase volume is rapidly expanded, and the surface energy is higher. Because the aggregation phenomenon can occur under the steady state of the mixture, the aggregation phenomenon of graphene can be avoided by adding a proper active agent. In one embodiment, the active agent is a combination of polyvinylpyrrolidone and sodium cholate, the total addition amount is 1 to 1.5 per mill, and the addition ratio of polyvinylpyrrolidone to sodium cholate is 2:1.
In one embodiment, in the step S13, a 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 result can be controlled by the circulation times. The high-pressure homogenization can improve the liquid phase stability of the mixed slurry, and further reduce the distribution width of the graphene sheet diameter size, thereby being beneficial to preparing the graphene current collector with excellent electrical and mechanical properties. In one embodiment, the homogenizing treatment pressure is 750-1800 bar, and the circulation times are 15-25 times, so that the comprehensive efficiency of the uniformity degree and the treatment times of the graphene slurry can achieve the best effect.
In an embodiment, the power of the ultrasonic vibration treatment in the step S13 is 15-24 kw, and the temperature control is paid attention to in the ultrasonic process, so that the high-temperature graphene agglomeration is avoided. The ultrasonic vibration treatment is used for dispersing and crushing, and further opens the graphite sheet layer to produce more single-layer graphene. In one embodiment, the ultrasonic process control temperature is no greater than 38 ℃.
And in the step S14, the freeze-drying is specifically implemented by freezing the graphene mixed slurry subjected to ultrasonic vibration treatment to a temperature below minus 45 ℃, heating and sublimating, heating to 5-8 ℃ per hour, and preserving heat for 2 hours at 35-37 ℃ to obtain graphene powder, and drying and storing. The freezing temperature is preferably-46℃and the heating temperature is preferably 35 ℃.
In one embodiment, the pressure of the compression process in the step S15 is 10 to 35MP.
In one embodiment, the graphene paper current collector has a specific surface area of 1450-1500 square meters per gram, and the supercapacitor prepared by using the graphene paper current collector has a voltage of 2.7-4V and a volume energy density of 16-25 Wh/L.
The present application will be further described with reference to specific examples. It should be understood that the detailed description is presented herein for purposes of illustration and explanation only and is not intended to limit the present application.
Example 1
3kg of 1500 mesh expanded graphite is mixed with 6L of pure water, and the mixture is obtained by low-speed stirring, high-speed dispersion and 2000rpm of rotation speed;
adding pure water into the mixture for dilution to 7.5%, and adding 48g of polyvinylpyrrolidone and sodium cholate, wherein the amount of polyvinylpyrrolidone is 32g, the amount of sodium cholate is 16g, stirring, and then performing primary shearing and secondary shearing, wherein the primary shearing rotating speed is 5000rpm, the shearing time is 2h, the secondary shearing rotating speed is 12000rpm, and the shearing time is 3h, so as to perform mechanical stripping, thereby obtaining mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, circularly treating the mixed slurry for 18 times under the homogenizing pressure of 1500bar, then performing ultrasonic vibration 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, 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 supercapacitor is 4.0V, and the volume energy density is 25Wh/L.
Example 2
3kg of 1500 mesh expanded graphite is mixed with 6L of pure water, and the mixture is obtained by low-speed stirring, high-speed dispersion and 2000rpm of rotation speed;
adding pure water into the mixture for dilution to 10 percent concentration, and adding 37.5g of polyvinylpyrrolidone and sodium cholate in total, wherein the amount of polyvinylpyrrolidone is 25g, the amount of sodium cholate is 12.5g, stirring, and then carrying out primary shearing and secondary shearing, wherein the primary shearing rotating speed is 5000rpm, the shearing time is 2.5h, the secondary shearing rotating speed is 12000rpm, and the shearing time is 4h, so as to obtain mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, circularly treating the mixed slurry for 18 times under the homogenizing pressure of 1300bar, then performing ultrasonic vibration 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, 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 supercapacitor is 3.8V, and the volume energy density is 22Wh/L.
Example 3
3kg of 1500 mesh expanded graphite is mixed with 6L of pure water, and the mixture is obtained by low-speed stirring, high-speed dispersion and 2000rpm of rotation speed;
adding pure water into the mixture for dilution to a concentration of 12%, and adding polyvinylpyrrolidone and sodium cholate with a total amount of 30g, wherein the amount of polyvinylpyrrolidone is 20g, the amount of sodium cholate is 10g, stirring, and then carrying out primary shearing and secondary shearing, wherein the primary shearing rotating speed is 5000rpm, the shearing time is 3h, the secondary shearing rotating speed is 12000rpm, and the shearing time is 4h, so as to carry out mechanical stripping, thereby obtaining mixed slurry;
crushing the mixed slurry through a high-pressure homogenizing process, circularly treating the mixed slurry for 15 times under the homogenizing pressure of 1600bar, then performing ultrasonic vibration 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, 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 supercapacitor is 3.7V, and the volume energy density is 20Wh/L.
The preparation method of the graphene paper current collector has the advantages of simple technological process operation, no chemical reaction process, high yield, capability of avoiding the chemical reagent from damaging the conjugated structure of graphene, capability of greatly reducing the conductivity and mechanical property of graphene, no need of treating pollutants such as waste acid and alkali, environment-friendly production, no environmental pollution, large specific surface area, capability of increasing the storage capacity of active substances and capability of greatly improving the capacity and performance of the supercapacitor.
It will be appreciated by persons skilled in the art that the above embodiments are provided for illustration only and not as limitations of the present application, and that suitable modifications and variations of the above embodiments are within the scope of the application as claimed.
Claims (8)
1. A preparation method of a graphene paper current collector is characterized by comprising the following steps: the method comprises the following steps:
mixing the expanded graphite with pure water according to a preset proportion, and obtaining a mixture through low-speed stirring and high-speed dispersion, wherein the preset proportion is 1:2-1:3;
adding pure water into the mixture for dilution and adding an active agent, and mechanically stripping through primary shearing and secondary shearing after stirring to obtain mixed slurry, wherein the concentration of the mixed slurry is 7.5-12%;
crushing the mixed slurry through a high-pressure homogenizing process, and then performing ultrasonic vibration 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 for preparing the graphene paper current collector according to claim 1, wherein: the active agent is the combination of polyvinylpyrrolidone and sodium cholate, and the adding ratio of polyvinylpyrrolidone to sodium cholate is 2:1.
3. The method for preparing the graphene paper current collector according to claim 1, wherein: the total addition amount of the active agent is 1 to 1.5 per mill.
4. The method for preparing the graphene paper current collector according to claim 1, wherein: 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.
5. The method for preparing the graphene paper current collector according to claim 1, wherein: the pressure of the high-pressure homogenizing treatment is 750-1800 bar, and the number of times of circulation is 15-25 times.
6. The method for preparing the graphene paper current collector according to claim 1, wherein: the freeze-drying process comprises the following steps:
and freezing the graphene mixed slurry subjected to ultrasonic vibration treatment at least to-45 ℃, heating and sublimating, heating to 5-8 ℃ per hour, and preserving heat for 2 hours after reaching 35-37 ℃ to obtain graphene powder.
7. A graphene paper current collector prepared by the preparation method of the graphene paper current collector according to any one of claims 1 to 6, characterized in that: the specific surface area of the graphene paper current collector is 1450-1500 square meters per gram.
8. A supercapacitor, characterized in that: the graphene paper current collector is adopted to manufacture the supercapacitor, wherein the voltage of the supercapacitor is 2.7-4V, and the volume energy density is 16-25 Wh/L.
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