CN112635746A - Preparation method and application of water-based zinc ion battery vanadium-based positive electrode material - Google Patents
Preparation method and application of water-based zinc ion battery vanadium-based positive electrode material Download PDFInfo
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Abstract
The invention discloses a preparation method of a vanadium-based cathode material of a water-based zinc ion battery, which comprises the following steps: 1) ammonium metavanadate, 2-methylimidazole zinc salt and absolute ethyl alcohol according to a mass ratio of 10 (2-5): (3-10) uniformly mixing, and stirring to obtain a solid product; 2) and putting the solid product into a magnetic boat, putting the magnetic boat in a tubular furnace, heating to 400-600 ℃ at the heating rate of 1-3 ℃/min in the air or nitrogen atmosphere, preserving the heat for 1-3h, naturally cooling to room temperature, and uniformly grinding the obtained product to obtain the vanadium-based oxide electrode material. The invention takes ammonium metavanadate as a raw material to prepare the anode material of the water-based zinc ion battery. The preparation method has simple steps, is suitable for mass production, uses the ammonium metavanadate as the raw material with low price, and is expected to realize industrial application. In addition, electrochemical tests show that the zinc ion battery formed by taking the vanadium-based oxide as the positive electrode and the zinc sheet as the negative electrode shows excellent electrochemical performance when being charged and discharged under different current densities.
Description
The technical field is as follows:
the invention belongs to the field of water-system zinc ion batteries, and particularly relates to a preparation method and application of a water-system zinc ion battery vanadium-based cathode material.
Background art:
fossil fuels, which are the main energy source for the development of the current society, face the problems of limited resources, non-regeneration, environmental pollution caused by improper use, and the like. The rechargeable battery as a clean electrochemical energy storage device has the advantages of high charging and discharging efficiency, high energy density/power density and the like, and has wide application prospect no matter the rechargeable battery is used in a portable or large-scale fixed mode. Under the background that the applications of current electronic products and electric vehicles are more and more extensive, the research and development of rechargeable secondary batteries with high energy density, high rate performance, safety, low cost and long cycle life is one of the key technologies. The organic electrolyte used in the lithium ion battery widely used at present has potential safety hazards such as flammability, toxicity and the like, and the problems of limited lithium metal storage capacity and high price are faced. The water-based zinc ion battery draws wide attention as a novel energy storage system with low price, safety and environmental protection, and the zinc sheet cathode of the water-based zinc ion battery has higher specific mass capacity (819mAh/g) and high specific volume capacity (5855 mAh/cm)3) And the oxidation-reduction potential is lower (-0.76V, relative to a standard hydrogen electrode), and in addition, the aqueous electrolyte is safe and environment-friendly, is convenient for the assembly of the battery, and greatly reduces the production cost.
At present, the cathode materials of the water-based zinc ion battery are various, such as Prussian Blue Analogues (PBAs), manganese-based materials, vanadium-based materials, conductive polymers and the like. Compared with positive electrode materials such as manganese-based oxides, Prussian blue analogues and the like, the vanadium-based materials tend to have higher reversible capacity, excellent rate characteristics and long cycle life. In the prior art, application number CN111640921A discloses a preparation method of a vanadium-based compound electrode material and application of the vanadium-based compound electrode material in a water-based zinc ion battery.
The invention content is as follows:
the invention aims to provide a preparation method and application of a vanadium-based positive electrode material of a water-based zinc ion battery, which is used as a positive electrode material of the water-based zinc ion battery. The method has the characteristics of simple preparation process, easy realization of large-scale production of products, low production cost and low raw material price, and the prepared material has excellent electrochemical performance when being used as a cathode material of a water-system zinc ion battery.
The invention is implemented by the following technical scheme: a preparation method of a water-based zinc ion battery vanadium-based positive electrode material comprises the following steps:
1) ammonium metavanadate, 2-methylimidazole zinc salt and absolute ethyl alcohol according to a mass ratio of 10 (2-5): (3-10) uniformly mixing and stirring to finally obtain a solid product;
2) and (3) heating the solid product to 400-600 ℃ at the heating rate of 1-3 ℃/min in the air or nitrogen atmosphere, preserving the heat for 1-3h, naturally cooling to room temperature, and uniformly grinding the obtained product to obtain the vanadium-based oxide electrode material.
Further, in the step 1), after mixing the ammonium metavanadate, the 2-methylimidazole zinc salt and the absolute ethyl alcohol, stirring the mixture by a magnetic stirrer at normal temperature or carrying out ultrasonic treatment by an ultrasonic instrument to uniformly disperse the mixture, and obtaining a solid product after the absolute ethyl alcohol is completely volatilized.
Further, in the step 1), after mixing ammonium metavanadate, 2-methylimidazole zinc salt solution and absolute ethyl alcohol, uniformly stirring by using a magnetic stirrer, putting the mixture into a reaction kettle, reacting for 24 hours in an oven at 180 ℃, washing a product by using the absolute ethyl alcohol, and drying to obtain a solid product.
The invention also discloses an application of the water-based zinc ion battery vanadium-based positive electrode material, the prepared vanadium-based oxide positive electrode material is mixed with conductive carbon powder and a binder according to the mass ratio of (7-8): 1-2):1, ethanol is used as a dispersing agent, the mixture is stirred for 12 to 24 hours by a magnetic stirrer, the prepared electrode slurry is uniformly coated on carbon paper to construct a zinc ion battery positive electrode, and then the zinc ion battery positive electrode, a glass fiber diaphragm, a water-based electrolyte and a zinc sheet negative electrode are assembled in the air to form the water-based zinc ion battery button battery.
Further, the binder is polyvinylidene fluoride or polytetrafluoroethylene, and the water system electrolyte is 3mol/L zinc trifluoromethanesulfonate.
The invention has the advantages that: the invention takes ammonium metavanadate as a main raw material to prepare the vanadium-based cathode material of the water-based zinc ion battery. The method has simple synthesis steps, can realize mass production, uses low-price raw materials, and is expected to realize industrial application. Electrochemical tests show that the zinc ion battery formed by taking the vanadium-based oxide as the anode and the zinc sheet as the cathode shows excellent electrochemical performance when being charged and discharged under different current densities, and the discharge specific capacity of 205mAh/g can still be kept after 2000 times of charge and discharge cycles under the heavy current density of 10A/g.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an XRD pattern of a vanadium-based oxide produced in example 1 of the present invention.
FIG. 2 is a graph showing the cycle characteristics of an aqueous zinc-ion battery having a vanadium-based oxide as a positive electrode, which was produced in example 1 of the present invention, at a current density of 10A/g.
FIG. 3 is an XRD pattern of the vanadium-based oxide produced in example 2 of the present invention.
FIG. 4 is a graph showing the cycle characteristics of an aqueous zinc-ion battery having a vanadium-based oxide as a positive electrode, which was produced in example 2 of the present invention, at a current density of 10A/g.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 invention.
Example 1
Dispersing 100mg of ammonium metavanadate in 30mL of absolute ethanol, adding 50mg of 2-methylimidazole zinc salt (ZIF-8, Adv. Mater.2019,31,1903404 prepared according to a literature report method), stirring at normal temperature by a magnetic stirrer until the ethanol is completely volatilized, putting the obtained solid product into a magnetic boat, putting the magnetic boat in a tube furnace, heating to 450 ℃ at a heating rate of 2 ℃/min in an air atmosphere, keeping for 2h, and after naturally cooling to room temperature, uniformly grinding the prepared product to obtain orange-yellow powder. It can be seen from the XRD test of FIG. 1 that the prepared vanadium-based oxide is V2O5。
Example 2
Dispersing 20mg of 2-methylimidazolium zinc salt in 30mL of absolute ethyl alcohol, adding 10mL of 0.1M ammonium metavanadate aqueous solution, uniformly stirring by using a magnetic stirrer, placing the mixture into a reaction kettle, placing the reaction kettle into an oven, reacting for 24 hours at 180 ℃, washing the obtained product for three times by using the absolute ethyl alcohol, drying the product, placing the product into a tubular furnace, heating the product to 450 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2 hours, and grinding the product uniformly to obtain orange powder after the product is naturally cooled to room temperature. It can be seen from the XRD test of FIG. 3 that the prepared vanadium-based oxide is V2O5。
Mixing the vanadium-based oxide prepared in example 1-2 with conductive carbon powder (Ketjen black, EC-300J) and PVDF (polyvinylidene fluoride) as binder at a mass ratio of 7:2:1, adding absolute ethyl alcohol as dispersant, stirring for 12h with a magnetic stirrer to obtain electrode slurry, uniformly coating the slurry on carbon paper (type HCP020N) to construct a zinc ion battery anode, and mixing the anode, a glass fiber diaphragm (type GF/D) and a water-based electrolyte (3MZn (CF MZn)3SO3)2) And assembling the zinc sheet cathode into a water system zinc ion battery button cell, standing for 24 hours, and then carrying out electrochemical performance test: the constant current charge and discharge test was performed on the battery fabricated above, and the current density was set to 10A/g, and the test results are shown in fig. 2 and 4.
And (4) analyzing electrochemical performance results:
in the aqueous zinc ion battery using the vanadium-based oxide as the positive electrode in example 1, the specific discharge capacity after 2000 charge-discharge cycles in the constant current charge-discharge test with the current density of 10A/g was 205 mAh/g. In the aqueous zinc ion battery using the vanadium-based oxide as the positive electrode in the embodiment 2, after 2000 charge-discharge cycles in the constant current charge-discharge test with the current density of 10A/g, the specific discharge capacity is 263 mAh/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A preparation method of a water-based zinc ion battery vanadium-based positive electrode material is characterized by comprising the following steps:
1) ammonium metavanadate, 2-methylimidazole zinc salt and absolute ethyl alcohol according to a mass ratio of 10 (2-5): (3-10) uniformly mixing and stirring to finally obtain a solid product;
2) and (3) heating the solid product to 400-600 ℃ at the heating rate of 1-3 ℃/min in the air or nitrogen atmosphere, preserving the heat for 1-3h, naturally cooling to room temperature, and uniformly grinding the obtained product to obtain the vanadium-based oxide electrode material.
2. The preparation method of the water-based zinc-ion battery vanadium-based positive electrode material according to claim 1, characterized in that in the step 1), after the ammonium metavanadate, the 2-methylimidazole zinc salt and the absolute ethyl alcohol are mixed, the mixture is stirred by a magnetic stirrer at normal temperature or is subjected to ultrasonic treatment by an ultrasonic instrument, so that the mixture is uniformly dispersed, and a solid product is obtained after the absolute ethyl alcohol is completely volatilized.
3. The preparation method of the aqueous zinc-ion battery vanadium-based positive electrode material according to claim 1, characterized in that in step 1), ammonium metavanadate, 2-methylimidazole zinc salt and absolute ethyl alcohol are mixed, stirred uniformly by a magnetic stirrer, placed in a reaction kettle, placed in an oven to react for 24 hours at 180 ℃, and the product is washed by absolute ethyl alcohol and dried to obtain a solid product.
4. The application of the vanadium-based oxide electrode material prepared by the method according to any one of claims 1 to 3, characterized in that the vanadium-based oxide positive electrode material is mixed with conductive carbon powder and a binder according to the mass ratio of (7-8): 1-2):1, ethanol is used as a dispersing agent, the mixture is stirred by a magnetic stirrer for 12 to 24 hours, the prepared electrode slurry is uniformly coated on carbon paper to construct a zinc ion battery positive electrode, and then the zinc ion battery positive electrode, a glass fiber diaphragm, an aqueous electrolyte and a zinc sheet negative electrode are assembled into an aqueous zinc ion battery button cell in the air.
5. The preparation method of the water-based zinc ion battery vanadium-based positive electrode material as claimed in claim 4, wherein the binder is polyvinylidene fluoride or polytetrafluoroethylene, and the water-based electrolyte is 3mol/L zinc trifluoromethanesulfonate.
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| CN113422048A (en) * | 2021-06-23 | 2021-09-21 | 上海电力大学 | Preparation method and application of novel water-based zinc ion battery positive electrode material |
| CN113937264A (en) * | 2021-09-28 | 2022-01-14 | 桂林理工大学 | Preparation method of nitrogen compound modified manganese vanadate at normal temperature and application of nitrogen compound modified manganese vanadate in water-based zinc ion battery |
| CN115472815A (en) * | 2022-09-23 | 2022-12-13 | 天津大学 | Vanadium-based cathode material and preparation method and application thereof |
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| CN113135586A (en) * | 2021-04-21 | 2021-07-20 | 内蒙古大学 | Zinc oxide micron ball, electrode and preparation method thereof |
| CN113422048A (en) * | 2021-06-23 | 2021-09-21 | 上海电力大学 | Preparation method and application of novel water-based zinc ion battery positive electrode material |
| CN113937264A (en) * | 2021-09-28 | 2022-01-14 | 桂林理工大学 | Preparation method of nitrogen compound modified manganese vanadate at normal temperature and application of nitrogen compound modified manganese vanadate in water-based zinc ion battery |
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