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Porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and preparation method thereof

A technology of carbon-coated sodium vanadium phosphate and composite positive electrode materials, which is applied in nanotechnology for materials and surface science, battery electrodes, electrical components, etc., can solve the problems of poor performance of synthetic materials, long production operation time, and preparation process Complicated problems, to achieve excellent electrochemical performance, short cycle, low reaction temperature effect

Active Publication Date: 2018-01-19
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the synthesis temperature of this method is low, the steps are simple, and it is convenient for industrialization, the performance of the obtained material is not good.
[0008] CN105161688A discloses a carbon-coated sodium iron phosphate composite material and its preparation method. Although its synthesis method is simple, it has the disadvantage of poor performance of the composite material; and CN104733731 A discloses a method for preparing uniform carbon-coated sodium vanadium phosphate The method of materials, CN106058202 A discloses a carbon-coated metal ion-doped sodium vanadium phosphate composite positive electrode material prepared by freeze-drying method and its preparation method and application. Their preparation process is complicated and the production operation time is long

Method used

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  • Porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and preparation method thereof
  • Porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and preparation method thereof
  • Porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and preparation method thereof

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Embodiment 1

[0046] (1) Dissolve 4mmol (0.4679g) of ammonium metavanadate and 6mmol (0.7564g) of oxalic acid dihydrate in 20mL of deionized water, heat and stir at 80°C until the solution turns blue, then add 6mmol (0.7199g) Sodium dihydrogen phosphate, stirred and dissolved to obtain 20mL blue mixed solution;

[0047] (2) Add 30 mL of N,N-dimethylformamide (the volume after mixing is 50 mL) to 20 mL of the blue mixed solution obtained in step (1), and place it in a 100 mL polytetrafluoroethylene-lined stainless steel sealed reaction kettle , at 180°C, react for 20h, cool, centrifuge, wash the cross-precipitate with ethanol and water for 3 times, and then dry at 80°C for 24h to obtain the precursor powder;

[0048] (3) Mix the precursor powder obtained in step (2) with 0.1982g glucose evenly, then place it in a high-purity argon atmosphere, sinter at 750°C for 10h, then cool to room temperature with the furnace, and coat it with porous spherical carbon Sodium vanadium phosphate composite ...

Embodiment 2

[0057] (1) Dissolve 1mmol (0.1820g) vanadium pentoxide and 1mmol (0.1921g) citric acid in 30mL deionized water, heat and stir at 70°C until the solution turns blue, then add 3mmol (0.395g) phosphoric acid (mass fraction 74.4%) and 4mmol (0.16g) sodium hydroxide, stirred and dissolved to obtain 30mL blue mixed solution;

[0058] (2) Add 30mL of n-propanol (60mL volume after mixing) to the 30mL blue mixed solution obtained in step (1), place it in a 100mL polytetrafluoroethylene-lined stainless steel sealed reaction vessel, and react at 160°C 20h, cooling, centrifuging, washing the cross-precipitation with ethanol and water for 4 times, and then drying at 80°C for 20h to obtain the precursor powder;

[0059] (3) Mix the precursor powder obtained in step (2) with 0.0991g of glucose evenly, then place it in a high-purity nitrogen atmosphere, sinter at 750°C for 10h, and then cool to room temperature with the furnace to form a porous spherical carbon-coated phosphoric acid Vanadiu...

Embodiment 3

[0067] (1) Dissolve 4mmol (0.4679g) of ammonium metavanadate and 3mmol (0.1875g) of hydrazine hydrate (mass fraction 80%) in 10mL of deionized water, heat and stir at 90°C until the solution turns green, then add 6mmol (0.7199g) sodium dihydrogen phosphate, stirred and dissolved to obtain 10mL green mixed solution;

[0068] (2) Add 50 mL of N,N-dimethylformamide to 10 mL of the blue mixed solution obtained in step (1) (the volume after mixing is 60 mL), and place it in a 100 mL polytetrafluoroethylene-lined stainless steel sealed reaction kettle, React at 230°C for 48h, cool, centrifuge, wash the cross-precipitate with ethanol and water for 5 times, and then dry at 100°C for 12h to obtain the precursor powder;

[0069] (3) Mix the precursor powder obtained in step (2) with 0.3964g glucose evenly, then place it in a hydrogen / argon gas mixture (the volume concentration of hydrogen is 5%), sinter at 800°C for 12h, and then After cooling to room temperature, the porous spherical ...

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Abstract

Disclosed are a porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and a preparation method thereof. The composite positive electrode material is prepared by the steps of (1) dissolving a vanadium source compound and a reducing agent into water, performing heating and then adding a phosphorus source compound and a sodium source compound to obtain a mixedsolution; (2) adding an organic solvent, wherein the polarity of the organic solvent is greater than that of water, and putting into a sealed container to be subjected to a heating reaction, and next, performing cooling, centrifuging, washing, depositing and drying to obtain precursor powder; and (3) performing mixing with glucose, and performing sintering and cooling on the mixture in protectiveatmosphere. The positive electrode material is spherical and has the primary granular diameter of 50-200nm; when the composite positive electrode material is assembled into a battery, the initial discharge capacity per gram at 0.2C and 10C within a voltage range of 2.0-3.8V can reach 110 mAh.g<-1> and 95 mAh.g<-1> respectively; the capacity retention rate can reach 99.47% at 10C rate after 100 cycles; and the method is simple and low in reaction temperature.

Description

technical field [0001] The invention relates to a sodium vanadium phosphate composite positive electrode material and a preparation method thereof, in particular to a porous spherical carbon-coated sodium vanadium phosphate composite positive electrode material and a preparation method thereof. Background technique [0002] With the consumption of non-renewable fossil energy such as oil and natural gas, the arrival of the energy crisis has attracted more and more attention. In this context, green and non-polluting new high-energy chemical power sources have become a hot spot in the development of countries all over the world. [0003] Lithium-ion battery is a new type of chemical power source, which is composed of two compounds that can reversibly insert and extract lithium ions as positive and negative electrodes. However, with the rapid development of lithium-ion batteries, the demand for metal lithium is increasing, but lithium resources are limited. Therefore, the cost ...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054B82Y30/00B82Y40/00
CPCY02E60/10
Inventor 童汇陈核章张宝姚赢赢王旭董鹏远郑俊超喻万景张佳峰
Owner CENT SOUTH UNIV
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