CN115417455A - Vanadium pentoxide intercalation material, preparation method thereof and application thereof in water-based zinc ion battery - Google Patents

Vanadium pentoxide intercalation material, preparation method thereof and application thereof in water-based zinc ion battery Download PDF

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Publication number
CN115417455A
CN115417455A CN202211228051.0A CN202211228051A CN115417455A CN 115417455 A CN115417455 A CN 115417455A CN 202211228051 A CN202211228051 A CN 202211228051A CN 115417455 A CN115417455 A CN 115417455A
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China
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vanadium pentoxide
ion battery
intercalation
zinc ion
preparation
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陈双明
王一琇
魏世强
宋礼
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/38—Construction or manufacture
    • 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
    • H01M4/36—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

A vanadium pentoxide intercalation material, a preparation method thereof and application thereof in a water system zinc ion battery. The invention provides a method for preparing an ammonium intercalation vanadium pentoxide material, and the material is applied as a positive electrode material of a water system zinc ion battery. The invention uses ammonium metavanadate as a precursor and obtains NH by a one-step calcination method 4 + ‑V 2 O 5 A material. NH prepared by the invention 4 + ‑V 2 O 5 The material shows higher capacity and better rate performance in the water-based zinc ion battery. And compared with the existing preparation method of vanadium pentoxide intercalation material, the method for preparing NH 4 + ‑V 2 O 5 The material has simple synthesis method and is easy to grow on a large scaleAnd the method has considerable application prospect.

Description

Vanadium pentoxide intercalation material, preparation method thereof and application thereof in water-based zinc ion battery
Technical Field
The invention belongs to the technical field of zinc ion batteries, and particularly relates to a vanadium pentoxide intercalation material, a preparation method thereof and application thereof in a water-system zinc ion battery.
Background
V 2 O 5 Is one of the important materials for the anode material of the water-based zinc ion battery. To enter intoThe battery capacity is improved, and the insertion layer type vanadium-based oxide is widely researched. NH (NH) 4 +-V 2 O 5 Is an ammonium radical intercalation V 2 O 5 The material of (1). Ammonium radical entering V 2 O 5 The interlayer has the function of expanding the interlayer spacing, further promotes the zinc ions to be embedded and separated in the charging and discharging process, and has practical significance in the aspect of improving the capacity and the rate capability of the zinc ion battery. However, the existing synthesis method is mostly limited to hydrothermal synthesis method, and has the problems of harsh conditions, low yield and the like.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a vanadium pentoxide intercalation material, a preparation method thereof, and an application thereof in a water-based zinc ion battery. And under the premise of uniform heating, the one-step calcining method has less limitation on the quality of the used raw materials, and the yield can reach 80 percent, so the yield is also improved.
The invention provides a preparation method of a vanadium pentoxide intercalation material, which comprises the following steps:
and calcining the ammonium metavanadate under the inert atmosphere condition to obtain the ammonium intercalation vanadium pentoxide material.
Preferably, the calcining temperature is 300-500 ℃ and the time is 2-3 h.
Preferably, the calcining temperature is 300 ℃ and the calcining time is 2h.
Preferably, the inert atmosphere condition is an argon atmosphere condition.
The invention also provides a vanadium pentoxide intercalation material prepared by the preparation method.
The invention also provides an application of the vanadium pentoxide intercalation material in a water-based zinc ion battery.
The invention also provides an application of the vanadium pentoxide intercalation material as a catalyst.
Compared with the prior art, the invention provides a preparation method of a vanadium pentoxide intercalation materialThe method comprises the following steps: and calcining the ammonium metavanadate under the inert atmosphere condition to obtain the ammonium intercalation vanadium pentoxide material. The production process is simple in flow and controllable in yield. The raw materials used in the invention have wide sources, low price and low production cost. The production process is safe, and the annealing is carried out under the protection of inert gas, so that the method is safe and harmless. The invention is harmless to environment, does not produce waste liquid and waste material, and produces NH 4 +-V 2 O 5 The material has wide application, not only can be used as an electrode material in the field of energy storage, but also can be used in the fields of catalysis and the like.
Drawings
FIG. 1 shows NH product of example 1 4 +-V 2 O 5 Scanning electron microscope pictures of the materials;
FIG. 2 shows NH product of example 1 4 +-V 2 O 5 Material transmission electron microscope photographs;
FIG. 3 shows NH product of example 1 4 +-V 2 O 5 A material X-ray diffraction pattern;
FIG. 4 shows NH product of example 2 4 +-V 2 O 5 A material X-ray diffraction pattern;
FIG. 5 shows NH product of example 3 4 +-V 2 O 5 A material X-ray diffraction pattern;
FIG. 6 shows NH product of example 4 4 +-V 2 O 5 A material X-ray diffraction pattern;
FIG. 7 shows NH product of example 3 4 +-V 2 O 5 Scanning electron microscope pictures of the materials;
FIG. 8 shows NH product of example 4 4 +-V 2 O 5 Scanning electron microscope pictures of the materials;
FIG. 9 shows NH product of example 1 4 +-V 2 O 5 A material zinc ion battery multiplying power performance diagram;
FIG. 10 shows NH product of example 4 3 H 2 O-V 2 O 5 The material zinc ion battery multiplying power performance diagram.
Detailed Description
The invention provides a preparation method of a vanadium pentoxide intercalation material, which comprises the following steps:
and calcining the ammonium metavanadate under the inert atmosphere condition to obtain the ammonium intercalation vanadium pentoxide material.
Specifically, the ammonium metavanadate is firstly placed in a quartz tube. Before the calcination and temperature rise, inert gas needs to be introduced for 5-10 min in advance, and oxygen in the quartz tube is removed.
Then calcining the mixture under the inert atmosphere condition to obtain the ammonium intercalation vanadium pentoxide material.
Wherein, the inert atmosphere condition is preferably an argon atmosphere condition.
The calcination temperature is 300-500 ℃, preferably 300, 400, 500, or any value between 300-500 ℃, and the time is 2-3 h, preferably 2h.
In some embodiments of the invention, the calcination temperature is 300 ℃ and the time is 2 hours. The temperature is too high, the obtained sample has high crystallinity and the main body is V 2 O 5 When the zinc ion battery is used as a positive electrode material of a zinc ion battery, the performance is poor, and the practical application is not facilitated.
The invention also provides an ammonium intercalation vanadium pentoxide material (NH) prepared by the preparation method 4 +-V 2 O 5 Material).
In the present invention, the NH 4 +-V 2 O 5 The particle size of the material is 1-10 μm.
The invention also provides an application of the vanadium pentoxide intercalation material in a water-based zinc ion battery.
The vanadium pentoxide intercalation material is used as a positive active material of a positive electrode of the water-based zinc ion battery. The present invention is not particularly limited to the preparation of the positive electrode, and may be prepared by a method known to those skilled in the art.
NH prepared by the invention 4 +-V 2 O 5 The material shows higher capacity and better rate performance in the water-based zinc ion battery.
The invention also provides an application of the vanadium pentoxide intercalation material as a catalyst.
The production process is simple and controllable in yield. The raw materials used in the invention have wide sources, low price and low production cost. The production process is safe, and the annealing is carried out under the protection of inert gas, so that the method is safe and harmless. The invention is harmless to environment, does not produce waste liquid and waste material, and produces NH 4 +-V 2 O 5 The material has wide application, not only can be used as an electrode material in the field of energy storage, but also can be used in the fields of catalysis and the like.
For further understanding of the present invention, the following description is given to the vanadium pentoxide intercalation material provided by the present invention and its preparation and application in water-based zinc-ion battery with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
1g of ammonium metavanadate is evenly placed in a porcelain boat and annealed for 2 hours at 300 ℃ under the protection of argon atmosphere, thus obtaining NH 4 +-V 2 O 5 A material.
Referring to FIGS. 1-3, FIG. 1 shows NH as a product of example 1 4 +-V 2 O 5 Scanning electron microscope pictures of the materials; FIG. 2 shows NH product of example 1 4 +-V 2 O 5 Transmission electron micrograph of the material; FIG. 3 shows NH product of example 1 4 +-V 2 O 5 Material X-ray diffraction pattern. As can be seen from FIGS. 1 to 3, NH was obtained 4 +-V 2 O 5 Obvious nanosheet structure appears on the surface. The shift of (001) crystal plane in XRD shows the intercalation of ammonium group to make V 2 O 5 The interlayer spacing increases. This is also further reflected in the lattice fringes of the (001) plane shown in the TEM images. .
Preparation of an aqueous zinc ion battery: reacting NH 4 +-V 2 O 5 The material, the conductive carbon black Super P and the binder PVDF are uniformly mixed according to the proportion of 7. And (3) assembling the button cell by taking the electrode plate as a positive electrode, a zinc metal plate as a negative electrode, filter paper with the radius of 10mm as a diaphragm and 3M zinc trifluoromethanesulfonate solution as electrolyte.
The performance of the prepared water-based zinc ion battery is measured, and the specific method comprises the following steps: and (4) carrying out performance test on the battery by using a Land CT2001A battery test system at room temperature. The voltage range is 0.2-1.8V, and the current density of the multiplying power performance test is 0.1-5 Ag- 1 In between.
The results are shown in FIG. 9, FIG. 9 is NH-product of example 1 4 +V 2 O 5 The material zinc ion battery multiplying power performance diagram. As can be seen from FIG. 9, NH 4 +-V 2 O 5 The anode material has better rate capability. At 5Ag- 1 The battery capacity can still reach 250.0mA h g- 1 And the coulombic efficiency approaches 100%.
Example 2
This embodiment differs from example 1 in that: the annealing temperature in step a was 400 ℃ and the rest was the same as in example 1. Referring to FIG. 4, FIG. 4 shows the NH product of example 2 4 +-V 2 O 5 Material X-ray diffraction pattern.
Example 3
This embodiment differs from example 1 in that: the annealing temperature in step a was 500 ℃ and the rest was the same as in example 1. Referring to FIGS. 5 and 7, FIG. 5 shows the NH product of example 3 4 +-V 2 O 5 X-ray diffraction pattern of material, FIG. 7 is NH product of example 3 4 +-V 2 O 5 Scanning electron microscope photograph of the material.
Example 4
This embodiment differs from example 1 in that: the precursor ammonium metavanadate is changed into ammonia water and V 2 O 5 And evaporating to dryness by magnetic stirring and heating at the rotating speed of 80 ℃ and 400rmp to obtain a gel-like precursor, and drying the precursor in a 50 ℃ oven for 12 hours under the same annealing condition as that of the embodiment 1.
Referring to fig. 6, 8 and 10, fig. 6 is the product NH of example 4 3 H 2 O-V 2 O 5 X-ray diffraction pattern of material, FIG. 8 is NH product of example 4 3 H 2 O-V 2 O 5 Scanning electron micrograph of the material, and FIG. 10 shows NH which is the product of example 4 3 H 2 O-V 2 O 5 The material zinc ion battery multiplying power performance diagram. As can be seen from FIGS. 6 and 8, the (001) peak in XRD is weak, and NH in SEM image is weak 3 H 2 O-V 2 O 5 The shape of the material is relatively fragmentary. This indicates that the use of ammonia as a precursor for intercalation can result in incomplete intercalation. As can be seen from FIG. 10, the ratio is compared with NH 4 +-V 2 O 5 Material, such incompletely intercalated NH 3 H 2 O-V 2 O 5 The material properties are relatively poor.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (7)

1. A preparation method of a vanadium pentoxide intercalation material is characterized by comprising the following steps:
and calcining the ammonium metavanadate under the inert atmosphere condition to obtain the ammonium intercalation vanadium pentoxide material.
2. The method according to claim 1, wherein the calcination is carried out at a temperature of 300 to 500 ℃ for 2 to 3 hours.
3. The method according to claim 1, wherein the calcination is carried out at a temperature of 300 ℃ for a period of 2 hours.
4. The method of claim 1, wherein the inert atmosphere condition is an argon atmosphere condition.
5. A vanadium pentoxide intercalation material prepared by the preparation method according to any one of claims 1 to 4.
6. Use of a vanadium pentoxide intercalation material according to claim 5 in an aqueous zinc-ion battery.
7. Use of a vanadium pentoxide intercalation material according to claim 5 as a catalyst.
CN202211228051.0A 2022-10-09 2022-10-09 Vanadium pentoxide intercalation material, preparation method thereof and application thereof in water-based zinc ion battery Pending CN115417455A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116135788A (en) * 2023-03-13 2023-05-19 浙江师范大学 Preparation method, product and application of halogen intercalation vanadium pentoxide nanoflower

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CN103531764A (en) * 2013-10-29 2014-01-22 福州大学 Sodium-ion battery positive material spherical ammonium vanadium oxide and preparation method therefor
CN105457665A (en) * 2014-09-09 2016-04-06 中国石油化工股份有限公司 Preparation method for vanadium-phosphorus catalyst with high specific surface area
CN107170967A (en) * 2017-05-05 2017-09-15 武汉理工大学 Pre- intercalated layered barium oxide nano material of bivalent metal ion and its preparation method and application
CN112194181A (en) * 2020-09-01 2021-01-08 河钢承德钒钛新材料有限公司 Method for preparing vanadium pentoxide by utilizing ammonium metavanadate
CN114988471A (en) * 2022-05-18 2022-09-02 北京大学深圳研究生院 Preparation method of vanadium-based positive electrode material, vanadium-based positive electrode material and positive plate

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CN103531764A (en) * 2013-10-29 2014-01-22 福州大学 Sodium-ion battery positive material spherical ammonium vanadium oxide and preparation method therefor
CN105457665A (en) * 2014-09-09 2016-04-06 中国石油化工股份有限公司 Preparation method for vanadium-phosphorus catalyst with high specific surface area
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116135788A (en) * 2023-03-13 2023-05-19 浙江师范大学 Preparation method, product and application of halogen intercalation vanadium pentoxide nanoflower
CN116135788B (en) * 2023-03-13 2023-11-14 浙江师范大学 Preparation method, product and application of halogen intercalation vanadium pentoxide nanoflower

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