Preparation method of hollow spherical negative electrode material vanadium phosphate/carbon for lithium ion battery

A technology for lithium ion batteries and negative electrode materials, which is applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of difficulty in controlling the morphology and characteristics of vanadium phosphate materials, influence on the electrochemical performance of materials, and low industrialization prospects, and achieve Coulomb efficiency. Stable, good cycle stability, strong controllability

Active Publication Date: 2018-07-13
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the vanadium phosphate material prepared by this method is in block shape, its fluidity is poor, its tap density is low, and its industrialization prospect is lower than that of spherical particles.
[0006] At present, the preparation of negative vanadium phosphate materials mainly adopts methods such as ball milling. However, the morphology and characteristics of the prepared vanadium phosphate materials are difficult to control, which is not conducive to subsequent processing. At the same time, the uneven morphology will also affect the electrochemical performance of the material.

Method used

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  • Preparation method of hollow spherical negative electrode material vanadium phosphate/carbon for lithium ion battery
  • Preparation method of hollow spherical negative electrode material vanadium phosphate/carbon for lithium ion battery
  • Preparation method of hollow spherical negative electrode material vanadium phosphate/carbon for lithium ion battery

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Experimental program
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Effect test

Embodiment 1

[0036] (1) Add 10mmol (1169.8mg) ammonium metavanadate to 250mL ultrapure water, heat to 60°C, and keep stirring at 400 rpm until dissolved, then add 10mmol (1150.3mg) ammonium dihydrogen phosphate, Heat to 70°C and keep stirring at 500 rpm until dissolved, finally add 0.5mmol (4000mg) polyvinylpyrrolidone, heat to 70°C, and keep stirring at 400 rpm until dissolved to obtain the precursor solution;

[0037] (2) Spray-dry the precursor solution obtained in step (1), wherein the inlet temperature is 220°C and the flow rate of the liquid is 600mL / h to obtain the precursor of vanadium phosphate / carbon material;

[0038] (3) The vanadium phosphate / carbon material precursor obtained in step (2) was heated to 750°C at a rate of 5°C / min under high-purity argon gas, and kept for 8 hours to obtain a hollow spherical lithium-ion battery negative electrode material vanadium phosphate / carbon.

[0039] Such as figure 1 As shown, the peak value of vanadium phosphate / carbon of the hollow ...

Embodiment 2

[0047] (1) Add 5mmol (584.9mg) ammonium metavanadate to 250mL ultrapure water, heat to 55°C, and keep stirring at 300 rpm until dissolved, then add 5mmol (660.28mg) diammonium hydrogen phosphate, Heat to 65°C and keep stirring at 600 rpm until dissolved, finally add 0.05mmol (400mg) polyvinylpyrrolidone, heat to 70°C, and keep stirring at 400 rpm until dissolved to obtain the precursor solution;

[0048] (2) Spray-dry the precursor solution obtained in step (1), wherein the inlet temperature is 210°C and the flow rate of the liquid is 700mL / h to obtain the precursor of vanadium phosphate / carbon material;

[0049] (3) The precursor of the vanadium phosphate / carbon material obtained in step (2) was heated up to 800°C at a rate of 3°C / min under high-purity helium gas, and kept for 6 hours to obtain a hollow spherical lithium-ion battery negative electrode material vanadium phosphate / carbon.

[0050] After testing, the XRD peaks of the vanadium phosphate / carbon anode material f...

Embodiment 3

[0058] (1) Add 30mmol (3509.4mg) ammonium metavanadate to 600mL ultrapure water, heat to 45°C, and keep stirring at 280 rpm until dissolved, then add 30mmol (3450.9mg) ammonium dihydrogen phosphate, Heat to 65°C and keep stirring at 350 rpm until dissolved, finally add 3mmol (1093.35mg) hexadecyltrimethylammonium bromide, heat to 70°C and keep stirring at 400 rpm , until dissolved to obtain a precursor solution;

[0059] (2) Spray-dry the precursor solution obtained in step (1), wherein the inlet temperature is 210°C and the flow rate of the liquid is 500mL / h to obtain the precursor of vanadium phosphate / carbon material;

[0060] (3) The precursor of the vanadium phosphate / carbon material obtained in step (2) was heated up to 700°C at a rate of 3°C / min under high-purity argon, and kept for 16 hours to obtain a hollow spherical lithium-ion battery negative electrode material vanadium phosphate / carbon.

[0061] After testing, the XRD peaks of the vanadium phosphate / carbon ano...

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Abstract

The invention discloses a preparation method of hollow spherical negative electrode material vanadium phosphate/carbon for a lithium ion battery. The preparation method comprises the following steps:(1) adding a vanadium source into water, heating and stirring, then adding a high molecular surfactant, heating and stirring to obtain a precursor solution; (2) carrying out spray drying to obtain a precursor of a vanadium phosphate/carbon material; and (3) carrying out heat treatment under an inert atmosphere to obtain the material. In the hollow spherical vanadium phosphate/carbon obtained by the method, vanadium phosphate is a pure phase, the particle morphology is uniform, and the particles are spherical; according to the assembled lithium ion battery, under 0 to 3 V and 100 mA/g, the first discharge gram volume reaches up to 1073.47 mAh/g, and the coulombic efficiency is high; the first reversible specific capacity reaches 551.41 mAh/g, and the capacity retention ratio after 83 timesof circulations is 80.0%; and the method is simple in operation and low in cost, and is applicable to industrial production.

Description

technical field [0001] The invention relates to a preparation method of vanadium phosphate / carbon, a negative electrode material of a lithium ion battery, in particular to a preparation method of a hollow spherical lithium ion battery negative electrode material, vanadium phosphate / carbon. Background technique [0002] The oil crisis forces people to look for new alternative energy sources. Lithium-ion battery research began in the 1980s. It has the advantages of high discharge voltage, high capacity, no memory effect, small size and excellent cycle performance, so it is widely used in mobile phones, digital cameras, notebook computers, electronic instruments, etc. Many civilian and military fields. Among them, the negative electrode material is one of the main factors affecting the cost and performance of the battery. Therefore, improving its electrochemical performance has become a research hotspot of many scholars. [0003] Among many negative electrode materials to be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/362H01M4/5825H01M4/62H01M10/0525Y02E60/10
Inventor 郑俊超肖彬汤林波王鹏博张宝童汇喻万景
Owner CENT SOUTH UNIV
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