CN111640921A - Preparation method of vanadium compound electrode material and application of vanadium compound electrode material in water-based zinc ion battery - Google Patents
Preparation method of vanadium compound electrode material and application of vanadium compound electrode material in water-based zinc ion battery Download PDFInfo
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- CN111640921A CN111640921A CN202010444234.0A CN202010444234A CN111640921A CN 111640921 A CN111640921 A CN 111640921A CN 202010444234 A CN202010444234 A CN 202010444234A CN 111640921 A CN111640921 A CN 111640921A
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- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
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Abstract
The invention discloses a preparation method of a vanadium compound electrode material and application of the vanadium compound electrode material in a water-based zinc ion battery, which comprises the following steps: dispersing a vanadium compound in a water solvent, keeping the solution at the temperature of 100-200 ℃ for 2-120 hours, cooling the solution to room temperature, washing and drying the solution to obtain a vanadium compound active material, and mixing the obtained vanadium compound active material and a conductive adhesive in a ratio of (6-9): (4-1) preparing slurry by mixing according to the mass ratio, immersing a current collector into the slurry, taking out and drying, and repeating the immersion and drying processes for 10-30 times to obtain a vanadium compound electrode material; and (3) preparing the aqueous zinc ion battery by using the obtained vanadium compound electrode material as a positive electrode material, using a Zn foil as a negative electrode and using the battery electrolyte. The invention utilizes the conductive adhesive and the three-dimensional current collector, improves the conductivity of the electrode, improves the unit area load capacity of the active material on the electrode, and is beneficial to improving the electrochemical performance of the water system zinc ion battery.
Description
Technical Field
The invention belongs to the field of electrochemical materials, and particularly relates to a preparation method of a vanadium compound electrode material and application of the vanadium compound electrode material in a water-based zinc ion battery.
Background
Along with the development and progress of society, the demand of people for energy in life is gradually increased. And non-renewable energy sources such as coal, petroleum, natural gas and the like are gradually exhausted, and the use of the non-renewable energy sources generates a large amount of pollution, so that the ecological environment is continuously deteriorated. In order to solve these problems, it is required to develop new clean energy sources such as wind energy, solar tidal energy, and the like. However, these energy sources are intermittent and cannot be directly used, and therefore, there is a need for a device that can store these energies on a large scale. The lithium ion battery is the most widely used secondary battery in the current life, can be recycled, and has the advantages of small volume, light weight, long service life, wide working temperature range, high specific power and working voltage, high energy density, quick charging, safety and the like. However, lithium batteries have some problems due to limited lithium resources: the organic electrolyte solution is adopted, so that the production cost is high, potential safety hazards exist, and the like, and the search for a new energy storage system which is rich in resource storage capacity and friendly to the environment becomes a new research hotspot at present.
The rechargeable aqueous battery adopts water-based electrolyte, has low production cost and good safety, and is expected to replace a lithium ion battery to become a new generation of electrochemical energy storage system. The ion conductivity of the battery is up to 1S/cm by using the water-containing electrolyte, and is much higher than that of a non-water-based electrolyte (10mS/cm), so that the quick charge and discharge capacity of the battery is favorably adapted to emerging applications, and a quick response balance system for frequency adjustment is particularly important for power grid storage. The metal zinc has high content in earth resources, large production scale, low cost and no toxicity, so that the water system zinc ion battery is unique in various water system metal ion batteries. In addition, zinc anodes have several advantages: low redox potential (relative toStandard hydrogen electrode of-0.76V), high theoretical capacity (820 mA. h.g)-1) Excellent chemical stability in water. Therefore, the water-based zinc ion battery is expected to be an ideal choice for the next generation of large-scale energy storage devices. However, in the construction of conventional water-based zinc-ion battery electrode materials, the active material and conductive agent (e.g., acetylene black) are combined with non-conductive binders (e.g., PVDF and CMC) and applied to a metal foil current collector. There is a problem in that the mass load of the active material in the positive electrode is insufficient, which greatly inhibits the effective utilization of the zinc-ion battery, and therefore, it is necessary to develop a new strategy for increasing the loading amount per unit area of the electrode material of the battery and improving the performance of the battery.
Disclosure of Invention
Aiming at the problems, the invention researches and designs a preparation method of a vanadium compound electrode material and application of the vanadium compound electrode material in a water-system zinc ion battery to solve the defects of insufficient load capacity per unit area and insufficient battery performance of a positive electrode active material of a traditional water-system zinc ion battery. The technical means adopted by the invention are as follows:
a preparation method of a vanadium compound electrode material comprises the following steps:
s1, dispersing the vanadium compound in a water solvent, keeping the solution at the temperature of 100-200 ℃ for 2-120 hours, cooling the solution to room temperature, washing and drying the solution to obtain the vanadium compound active material;
s2, mixing the obtained vanadium compound active material and the conductive adhesive in a ratio of (6-9): and (4-1) preparing slurry by mixing according to the mass ratio, immersing the three-dimensional current collector into the slurry, taking out and drying, and repeating the immersion and drying processes for 10-30 times to obtain the vanadium compound electrode material.
Preferably, in step S1, the vanadium compound is one or more of vanadium pentoxide, vanadium dioxide and a vanadium bronze compound.
Preferably, in step S1, the drying manner is freeze drying, air drying or natural drying.
Preferably, in step S2, the conductive binder is one or more of 3, 4-ethyldioxythiophene, styrene sulfonate, conductive poly (9, 9-dioctylfluorene-fluorenone-methyl benzoate), polyaniline, polypyrrole, and polyaniline-polyethylene oxide.
Preferably, in step S2, the current collector is a three-dimensional current collector.
Preferably, the three-dimensional current collector is a current collector of a carbon felt, a carbon cloth, a nickel foam, graphene or a carbon nanotube array.
A method for preparing an aqueous zinc ion battery by using the vanadium compound electrode material comprises the following steps: and (3) preparing the aqueous zinc ion battery by using the obtained vanadium compound electrode material as a positive electrode material, using a Zn foil as a negative electrode and using the battery electrolyte.
Preferably, the battery electrolyte is zinc trifluoromethanesulfonate or zinc sulfate aqueous solution.
Compared with the prior art, the preparation method of the vanadium compound electrode material and the application of the vanadium compound electrode material in the water-based zinc ion battery have the following beneficial effects:
1. the conductive adhesive is used for replacing the traditional non-conductive adhesive, so that the conductivity of the electrode material is improved, the transmission of electrons in the charging and discharging process is facilitated, and the rate capability and specific capacity of the battery are improved.
2. The invention utilizes the three-dimensional current collector to replace a metal foil current collector, can effectively avoid the stripping of thick active materials, improves the unit area load capacity of the active materials on the electrode, simultaneously reduces the electron and ion transmission resistance, and is beneficial to improving the electrochemical performance of the water system zinc ion battery.
3. According to the invention, the loading capacity of the active material can be conveniently adjusted by utilizing the frequency of immersing the three-dimensional current collector into the slurry and the concentration of the active material in the slurry.
4. The method provided by the invention provides a general way for constructing the high-quality load of the water-based zinc ion battery system, has the advantages of environmental friendliness, low cost and high safety, and can be used for manufacturing large-scale energy storage devices.
Drawings
Fig. 1 is an XRD pattern of the active material prepared in each example of the present invention.
Fig. 2 is an SEM image of the positive electrode of the aqueous battery prepared in example 1 of the present invention.
Fig. 3 is a charge and discharge curve of the positive electrode materials prepared in example 1 of the present invention and comparative example at a current density of 0.2A/g.
Fig. 4 is a charge-discharge curve diagram of different mass-loaded cathode materials prepared in example 1 of the present invention.
Detailed Description
A preparation method of a vanadium compound electrode material and an application of the vanadium compound electrode material in a water-based zinc ion battery comprise the following steps:
s1, preparation of an active material: dissolving the vanadium compound by using solvent water, sealing the mixed solution in a high-pressure kettle, keeping the mixed solution at the temperature of 100-200 ℃ for 2-120 hours, cooling to room temperature, washing the product by using deionized water for a plurality of times, and drying (freeze drying, blast drying, natural airing and the like) to obtain the required vanadium compound active material.
S2, preparing a high-load vanadium compound electrode slice: mixing the obtained vanadium compound with conductive carbon and a conductive adhesive in a specific weight ratio (6:3:1 or 7:2:1 or 8:1:1) to form uniform slurry, immersing a three-dimensional current collector into the slurry, taking out and airing, and repeating the immersion and drying processes for a plurality of times until the vanadium compound electrode plate with the required mass load is obtained.
S3, preparing a zinc ion battery with high area load: the prepared high-load vanadium compound electrode plate, the filter paper and the Zn foil are respectively used as a positive electrode, a diaphragm and a negative electrode, and the high-area-load aqueous zinc ion battery is prepared by taking zinc trifluoromethanesulfonate or zinc sulfate aqueous solution as battery electrolyte.
In step S2, the three-dimensional porous layered current collector may be made of a material with high conductivity and low density, such as carbon felt, and the pore size of the material is moderate, the pore directions of the material are parallel and three-dimensionally orthogonal. The three-dimensional porous layered current collector is used for replacing the traditional flat metal foil current collector, so that the defects of low specific surface area, easy aggregation of active materials, easy falling off after long-time circulation and the like can be overcome, and the energy storage performance of the battery can be improved.
Example 1:
preparing a vanadium dioxide active material: adding vanadium pentoxide solid into distilled water, adding a certain amount of oxalic acid, stirring in a water bath at 80 ℃ for 1 hour, converting the mixed solution into a dark blue solution, sealing the mixed solution in an autoclave, and keeping the mixed solution at 180 ℃ for 4 hours. And cooling to room temperature, and washing the product with deionized water for several times to obtain the vanadium dioxide nano rod.
Preparing a vanadium dioxide positive electrode on a three-dimensional current collector: 3 mg. about.mL-1Is mixed with the conductive carbon and the conductive binder in a weight ratio of 7:2:1 to form a uniform slurry. Immersing a carbon felt with the diameter of 10mm into the slurry as a three-dimensional current collector, taking out and airing, repeating the process for 10-30 times to obtain the mass load of 3-15mg/cm2The electrode sheet of (1).
Assembling an aqueous zinc ion battery: the prepared electrode plate, filter paper and Zn foil are respectively used as a positive electrode, a diaphragm and a negative electrode, and a 3M aqueous solution of zinc trifluoromethanesulfonate is used as an electrolyte to assemble the water-based zinc ion button cell. The electrochemical performance of the cell was then measured at an electrochemical workstation.
Example 2:
preparing a vanadium pentoxide active material: adding ammonium vanadate solid into distilled water, adding a certain amount of hydrochloric acid, converting the mixed solution into brown solution, sealing the mixed solution in an autoclave, and keeping the autoclave at 120 ℃ for 24 hours. And cooling to room temperature, and washing the product with deionized water for several times to obtain the vanadium pentoxide material.
Preparing a vanadium pentoxide positive electrode on a three-dimensional current collector: 3 mg. about.mL-1The vanadium pentoxide was mixed with the conductive carbon and the conductive binder at a weight ratio of 7:2:1 to form a uniform slurry. And (3) immersing a carbon felt with the diameter of 10mm serving as a three-dimensional current collector into the slurry, taking out and airing, and repeating the process for 10-30 times until an electrode plate with the required mass load is obtained.
Assembling an aqueous zinc ion battery: the prepared electrode plate, filter paper and Zn foil are respectively used as a positive electrode, a diaphragm and a negative electrode, and a 3M aqueous solution of zinc trifluoromethanesulfonate is used as an electrolyte to assemble the water-based zinc ion button cell. The electrochemical performance of the cell was then measured at an electrochemical workstation.
Comparative example:
the difference from the examples was that a comparative sample electrode sheet was obtained by replacing the conductive adhesive (PEDOT/PSS) with a non-conductive adhesive (PVDF).
As shown in fig. 1, XRD characterization of the vanadium dioxide active material prepared in example 1 was performed, consistent with JCPDS 81-2392. XRD characterization is carried out on the vanadium pentoxide active material prepared in the embodiment 2, and the vanadium pentoxide active material conforms to JCPDS 40-1296, which shows that the purity of vanadium dioxide and vanadium pentoxide is high.
Fig. 2 is an SEM image of the high-loading electrode material prepared in example 1, and it can be seen that the electrode material is uniformly loaded on the three-dimensional current collector, and the composite electrode still exhibits a porous structure, which is advantageous for the diffusion of the electrolyte.
Fig. 3 is a charge-discharge curve at a current density of 0.2A/g for the vanadium dioxide positive electrodes prepared in example 1 and comparative example. Fig. 3 shows that the specific capacity of the cathode material using the conductive binder reaches 332mAh/g, which is higher than that of the cathode material using the non-conductive binder, which indicates that the use of the conductive binder is beneficial to improving the conductivity of the electrode sheet and further improving the specific capacity. The unit area mass load of the water system zinc ion battery constructed by the invention is obviously improved and can reach 15mg/cm2(FIG. 4).
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (8)
1. A method for preparing a vanadium compound electrode material is characterized by comprising the following steps: the method comprises the following steps:
s1, dispersing the vanadium compound in a water solvent, keeping the solution at the temperature of 100-200 ℃ for 2-120 hours, cooling the solution to room temperature, washing and drying the solution to obtain the vanadium compound active material;
s2, mixing the obtained vanadium compound active material and the conductive adhesive in a ratio of (6-9): and (4-1) preparing slurry by mixing according to the mass ratio, immersing a current collector into the slurry, taking out and drying, and repeating the immersion and drying processes for 10-30 times to obtain the vanadium compound electrode material.
2. The method for preparing a vanadium compound electrode material according to claim 1, wherein: in step S1, the vanadium compound is one or more of vanadium pentoxide, vanadium dioxide, and a vanadium bronze compound.
3. The method for preparing a vanadium compound electrode material according to claim 1, wherein: in step S1, the drying method is freeze drying, air drying or natural drying.
4. The method for preparing a vanadium compound electrode material according to claim 1, wherein: in step S2, the conductive binder is one or more of 3, 4-ethyldioxythiophene, styrenesulfonate, conductive poly (9, 9-dioctylfluorene-fluorenone-methyl benzoate), polyaniline, polypyrrole, and polyaniline-polyethylene oxide.
5. The method for preparing a vanadium compound electrode material according to claim 1, wherein: in step S2, the current collector is a three-dimensional current collector.
6. The method for preparing a vanadium compound electrode material according to claim 5, wherein: the three-dimensional current collector is a current collector of a carbon felt, a carbon cloth, foamed nickel, graphene or a carbon nanotube array.
7. A method for preparing an aqueous zinc-ion battery using the vanadium compound electrode material according to any one of claims 1 to 6, wherein: the method comprises the following steps: and (3) preparing the aqueous zinc ion battery by using the obtained vanadium compound electrode material as a positive electrode material, using a Zn foil as a negative electrode and using the battery electrolyte.
8. The method for preparing the water-based zinc-ion battery by using the vanadium compound electrode material as claimed in claim 7, wherein the method comprises the following steps: the electrolyte of the battery is zinc trifluoromethanesulfonate or zinc sulfate aqueous solution.
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Cited By (5)
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| CN112357959A (en) * | 2020-10-19 | 2021-02-12 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of nano vanadium dioxide/reticular graphite-based composite electrode material |
| CN112421017A (en) * | 2020-10-29 | 2021-02-26 | 湘潭大学 | Preparation method of binder-free water-based zinc ion battery positive electrode composite material |
| CN112614985A (en) * | 2021-01-11 | 2021-04-06 | 江苏师范大学 | Aqueous zinc ion battery and preparation method of positive electrode |
| CN113651360A (en) * | 2021-08-18 | 2021-11-16 | 江南大学 | Synthesis method and application of vanadium oxide |
| CN114628672A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Organic-inorganic hybrid material based on vanadium pentoxide and preparation and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112357959A (en) * | 2020-10-19 | 2021-02-12 | 成都先进金属材料产业技术研究院有限公司 | Preparation method of nano vanadium dioxide/reticular graphite-based composite electrode material |
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| CN112421017A (en) * | 2020-10-29 | 2021-02-26 | 湘潭大学 | Preparation method of binder-free water-based zinc ion battery positive electrode composite material |
| CN112421017B (en) * | 2020-10-29 | 2022-02-18 | 湘潭大学 | Preparation method of binder-free water-based zinc ion battery positive electrode composite material |
| CN114628672A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Organic-inorganic hybrid material based on vanadium pentoxide and preparation and application thereof |
| CN114628672B (en) * | 2020-12-11 | 2023-11-21 | 中国科学院大连化学物理研究所 | Organic-inorganic hybrid material based on vanadium pentoxide, and preparation and application thereof |
| CN112614985A (en) * | 2021-01-11 | 2021-04-06 | 江苏师范大学 | Aqueous zinc ion battery and preparation method of positive electrode |
| CN112614985B (en) * | 2021-01-11 | 2022-05-24 | 江苏师范大学 | Aqueous zinc ion battery and preparation method of positive electrode |
| CN113651360A (en) * | 2021-08-18 | 2021-11-16 | 江南大学 | Synthesis method and application of vanadium oxide |
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Application publication date: 20200908 |