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Graded porous vanadium oxide microspheres and preparation method and application thereof

A vanadium oxide, graded porous technology, applied in vanadium oxide, electrical components, battery electrodes, etc., can solve the problems of decreased electrode cycle stability, unfavorable large-scale application, and high temperature required for the reaction, and achieves enhanced cycle stability, The effect of improving charge transport efficiency and reaction safety and stability

Inactive Publication Date: 2014-12-03
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of the above reports use the hydrothermal method, which requires high reaction temperature, long time, and low yield, and the prepared vanadium oxide is nano-sized. In the process of highly deintercalating lithium, there is a serious volume effect, and particle agglomeration occurs, resulting in The cycle stability of the electrode decreases, which is not conducive to large-scale application in actual production

Method used

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  • Graded porous vanadium oxide microspheres and preparation method and application thereof
  • Graded porous vanadium oxide microspheres and preparation method and application thereof
  • Graded porous vanadium oxide microspheres and preparation method and application thereof

Examples

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Embodiment 1

[0035] A method for synthesizing porous vanadium oxide microspheres, comprising the following steps:

[0036] (1) Add 0.5g of ammonium metavanadate to 200mL of ethylene glycol, place it on a water bath at 80°C and stir for 1 hour to form a uniform and transparent bright yellow liquid;

[0037] (2) continue to place the mixed solution described in step (1) on the oil bath, raise the temperature to 170°C, then react at a constant temperature of 170°C for 2 hours, condense and reflux during the reaction, and then cool naturally to obtain a blue-purple precipitate;

[0038] (3) Place the precipitate obtained in step (2) on a centrifuge and wash it six times with ethanol, the centrifuge speed is 6000r / min, and then dry the powder obtained by centrifugation in an oven at 60°C;

[0039] (4) Place the powder dried in step (3) in a tube furnace, start from room temperature, raise the temperature to 300°C at a rate of 1°C / min, and keep it at 300°C for 5 hours, the porous vanadium oxide ...

Embodiment 2

[0043] A method for synthesizing porous vanadium oxide microspheres, comprising the following steps:

[0044] (1) Add 0.5g of ammonium metavanadate to 400mL of ethylene glycol, place it on a water bath at 60°C and stir for 30min to form a uniform and transparent bright yellow liquid;

[0045] (2) continue to place the mixed solution described in step (1) on the oil bath, heat up to 170°C, then react at a constant temperature of 170°C for 1 hour, condense and reflux during the reaction, and then cool naturally to obtain a blue-purple precipitate;

[0046] (3) Place the precipitate obtained in step (2) on a centrifuge and wash it six times with ethanol, the centrifuge speed is 6000r / min, and then dry the powder obtained by centrifugation in an oven at 60°C;

[0047] (4) Place the powder dried in step (3) in a tube furnace, start from room temperature, raise the temperature to 500°C at a rate of 1°C / min, and keep it at 500°C for 4 hours, the porous vanadium oxide microspheres . ...

Embodiment 3

[0051] A method for synthesizing porous vanadium oxide microspheres, comprising the following steps:

[0052] (1) Add 0.25g of ammonium metavanadate to 200mL of ethylene glycol, place it on a water bath at 80°C and stir for 2 hours to form a uniform and transparent bright yellow liquid;

[0053] (2) continue to place the mixed solution described in step (1) on an oil bath, heat up to 180°C, then react at a constant temperature of 180°C for 2 hours, condense and reflux during the reaction, and then cool naturally to obtain a blue-purple precipitate;

[0054] (3) Place the precipitate obtained in step (2) on a centrifuge and wash it six times with ethanol, the centrifuge speed is 6000r / min, and then dry the powder obtained by centrifugation in an oven at 60°C;

[0055] (4) Place the powder dried in step (3) in a tube furnace, start from room temperature, raise the temperature to 600°C at a rate of 1°C / min, and keep it at 600°C for 5 hours, the porous vanadium oxide microspheres ...

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Abstract

The invention relates to graded porous vanadium oxide microspheres and a preparation method and application thereof. The size of the graded porous vanadium oxide microsphere is 4-10 micrometers, and the graded porous vanadium oxide microspheres are structurally formed by stacking a plurality of nano particles in a staggered way. The preparation method of the graded porous vanadium oxide microspheres comprises the following steps of: dissolving ammonium metavanadate in an organic solvent, carrying out condensation refluxing for 1-4 hours at constant temperature of 150-190 DEG C so that ammonium metavanadate has a reduction reaction to obtain bluish violet vanadium alkoxide precipitate; placing the bluish violet vanadium alkoxide precipitate in an argon atmosphere and calcining at 200-700 DEG C for 3-6 hours to obtain the graded porous vanadium oxide microspheres. According to the preparation method, the graded porous vanadium oxide microspheres are prepared by adopting constant-temperature liquid-phase reaction, related raw materials are common and nontoxic, the used process is simple and easy to operate, and high output is achieved; and the obtained graded porous vanadium oxide microsphere has important application value in the field of electrodes of lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials and electrochemical devices, and specifically relates to a hierarchical porous vanadium oxide microsphere and a preparation method thereof. The material can be used as a material in lithium ions or other electrochemical devices. Background technique [0002] With the increasing consumption of irreversible energy such as petroleum, portable energy systems are facing increasingly severe challenges. Because of its high energy density, excellent cycle performance and strong charge retention ability, lithium-ion batteries are expected to replace petroleum and are widely used in portable electronic devices. However, most of the cathode materials currently commercialized and about to enter developmental research are lithium-intercalated transition metal oxides. These cathode materials have fatal intrinsic constraints-low specific capacity, and it is difficult to achieve fast charge and discha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02H01M4/48
CPCY02E60/10
Inventor 王洪恩蔡祎黄绍专李昱苏宝连
Owner WUHAN UNIV OF TECH
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