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Preparation method of lithium vanadium phosphate (Li3V2(PO4)3)/graphene composite material for positive electrode of lithium ion battery

A lithium-ion battery, lithium vanadium phosphate technology, applied in battery electrodes, circuits, electrical components and other directions, can solve the problems of poor electrochemical performance, complicated operation, low synthesis temperature, etc., to improve electronic conductivity, simple preparation process, The effect of suppressing excessive growth

Inactive Publication Date: 2012-08-01
SHANGHAI ZHIRONG TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the carbothermal reduction method can reduce costs and improve material properties, the use of carbothermal solid phase reduction still inevitably mixes uneven raw materials, which affects the tap density of positive electrode materials.
The microwave method has the advantages of short reaction time and low energy consumption, but the heating time is not easy to control
Although the sol-gel method has low synthesis temperature, small product particle size, good electrochemical performance, and good cycle stability, the operation is complicated and the reaction conditions are harsh.
The advantage of the high-temperature solid-phase method is that the process is simple and easy to realize industrialization, but the purity of the synthesized sample is not high, the particle size is large, and the electrochemical performance is poor. In addition, the traditional high-temperature solid-phase method uses pure H2 as the reducing agent, which has the disadvantage of high cost. , unsafe shortcomings

Method used

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  • Preparation method of lithium vanadium phosphate (Li3V2(PO4)3)/graphene composite material for positive electrode of lithium ion battery
  • Preparation method of lithium vanadium phosphate (Li3V2(PO4)3)/graphene composite material for positive electrode of lithium ion battery
  • Preparation method of lithium vanadium phosphate (Li3V2(PO4)3)/graphene composite material for positive electrode of lithium ion battery

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh LiNO according to the stoichiometric ratio of Li:V:P molar ratio of 3:2:33 , V 2 o 5 and NH 4 h 2 PO 4 A total of 20g, uniformly mixed with 2.5g graphene oxide precursor by magnetic stirring, stirred for 2h, continued to stir for 0.5h after adding 2.5g citric acid, then sprayed dry by spray dryer to obtain powder material, then transferred the gained material to Into a tube furnace, in an argon atmosphere, heated at a heating rate of 30°C / min, with an argon flow rate of 100mL / min, and calcined at a constant temperature of 200°C for 1h. After natural cooling, the obtained precursor powder was ground for 50 minutes, then transferred to a tube furnace, heated at a heating rate of 30°C / min, with a gas flow rate of 100mL / min, and calcined at a constant temperature of 850°C for 10 hours to obtain a lithium-ion battery lithium vanadium phosphate positive electrode Material. It is measured that the primary particle diameter of the material obtained by spray granulati...

Embodiment 2

[0032] Weigh CH according to the stoichiometric ratio of Li:V:P=3:2:3 3 COOLi, NH 4 VO 3 and (NH 4 ) 2 HPO 4 A total of 20g, mixed uniformly with an aqueous solution containing 1.5g graphite oxide (3mg / mL) by magnetic stirring, stirred for 3h, continued to stir for 1h after adding 2.8g sucrose, then spray-dried by a spray dryer to obtain a powder material, and then The obtained material was transferred into a tube furnace, heated at a heating rate of 20°C / min in a hydrogen atmosphere, the hydrogen flow rate was 80mL / min, and calcined at a constant temperature of 250°C for 2h. After natural cooling, the obtained precursor powder was ground for 30 minutes, then transferred to a tube furnace, heated at a heating rate of 20°C / min, with a gas flow rate of 80mL / min, and calcined at a constant temperature of 800°C for 8 hours to obtain a lithium-ion battery lithium vanadium phosphate positive electrode Material.

[0033] The XRD of the product see figure 1 As shown in the midd...

Embodiment 3

[0035] Weigh LiOH·H according to the stoichiometric ratio of Li:V:P=3:2:3 2 O, NaVO 3 and H 3 PO 4 A total of 25g, mixed uniformly with 3.7g pyrolytic graphene (400°C×2h) precursor by magnetic stirring, stirred for 3h, added 2.6g polyvinyl alcohol and continued to stir for 1.5h, and then spray dried by a spray dryer to obtain The powder material was then transferred to a tube furnace, heated in an ethylene atmosphere at a heating rate of 20°C / min, with an ethylene flow rate of 60mL / min, and calcined at a constant temperature of 350°C for 3h. After natural cooling, the obtained precursor powder was ground for 20 minutes, then transferred to a tube furnace, heated at a heating rate of 25°C / min, with a gas flow rate of 60mL / min, and calcined at a constant temperature of 700°C for 6 hours to obtain a lithium-ion battery lithium vanadium phosphate positive electrode Material. The average particle size of the material is measured to be 100-200nm, and the tap density is 1.60g / cm ...

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Abstract

The invention relates to a preparation method of a lithium vanadium phosphate (Li3V2(PO4)3) / graphene composite material for a positive electrode of a lithium ion battery. The method comprises the steps that firstly, a mixed precursor solution is prepared; pretreatment of spray drying is conducted and a precursor is obtained; and then the lithium vanadium phosphate positive electrode material of the lithium ion battery is prepared through a calcination reaction under an inert atmosphere condition. Compared with the prior art, the preparation method has the advantages that the combination mode of the Li3V2(PO4)3 and the graphene, the contents of carbon and the graphene, and the particle size of the material are effectively controlled, thereby improving the stability and the electrical conductive performance of the material.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a preparation method of a positive electrode material of a lithium ion battery. The key point is a method for assisting the synthesis of lithium vanadium phosphate / graphene composite material by spray drying. Background technique [0002] Lithium-ion battery is a new generation of green high-energy battery, which has many advantages such as high voltage, high energy density, good cycle performance, small self-discharge, no memory effect, and wide operating temperature range. At present, the application fields of lithium-ion batteries continue to expand, and have become an important part of high-tech products that are of great significance to the national economy and people's livelihood. [0003] Cathode materials determine the performance of lithium-ion batteries to a large extent, so they have always been a research hotspot in the field of lithium-ion bat...

Claims

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Application Information

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IPC IPC(8): H01M4/62H01M4/38H01M4/58
CPCY02E60/12Y02E60/10
Inventor 赵兵蒋永徐为文
Owner SHANGHAI ZHIRONG TECH
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