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Preparation method of vanadium sodium fluophosphate cathode material of hybrid ion battery

A technology of sodium vanadium fluorophosphate and positive electrode materials, applied in battery electrodes, circuits, electrical components, etc., can solve problems such as easy sintering of lithium ions, unsuitable for high-rate current charging and discharging, production and application restrictions, and achieve large-scale production. High stability, improved electrochemical performance, easy to control and realize the effect

Inactive Publication Date: 2012-01-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use and research of ion batteries are now dominated by phosphoric acid system transition metal materials, but there are also many problems: lithium ion batteries have low-temperature lithium precipitation phenomenon, which is easy to cause safety hazards; low conductivity, not suitable for high-rate current charging and discharging ;The tap density is low, and the material volume is large; Lithium ions are easy to sinter, resulting in the instability of the material
But its raw material cost is high, in the preparation process due to Decomposition releases a large amount of gas, the particle size distribution range of the product is difficult to control, and the production application is bound to be limited

Method used

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  • Preparation method of vanadium sodium fluophosphate cathode material of hybrid ion battery
  • Preparation method of vanadium sodium fluophosphate cathode material of hybrid ion battery
  • Preparation method of vanadium sodium fluophosphate cathode material of hybrid ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Firstly, accurately weigh 2.5g of raw materials and 0.125g of conductive agent acetylene black, the acetylene black as conductive agent is 5% of the total weight of raw materials, put them in a mortar and grind them for 2.5h to obtain a uniformly mixed precursor . The raw material part includes 0.567g NaF, 0.802g V 2 o 5 , 1.025g NH 4 h 2 PO 4 and 0.106g reducing agent acetylene black (V:P:F molar ratio is about 2:2:3). The well-ground precursor powder was placed in a tube furnace, and the temperature was gradually raised to 350°C at a rate of 3°C / min under an argon protective atmosphere, and kept at this temperature for 8 hours, and a solid mixture was obtained after natural cooling. After the solid powder is completely transferred to the mortar and fully ground again, the set temperature is reached at a heating rate of 3°C / min. Carry out calcination in the range of 550-750°C, keep warm in argon atmosphere for 8 hours, and cool naturally to obtain sodium vanadium...

Embodiment 2

[0031] Accurately weigh 2.5g of raw materials and 0.125g of conductive agent acetylene black. The acetylene black used as conductive agent is 5% of the total weight of the raw materials. They are placed in a mortar and ground for 2.5 hours to obtain a uniformly mixed precursor. The raw material part includes 0.567g NaF, 0.802g V 2 o 5 , 1.128g NH 4 h 2 PO 4 and 0.106g reducing agent acetylene black (V:P:F molar ratio is about 2:2.2:3). The well-ground precursor powder was placed in a tube furnace, and the temperature was gradually raised to 350°C at a rate of 3°C / min under an argon protective atmosphere, and kept at this temperature for 8 hours, and a solid mixture was obtained after natural cooling. Completely transfer the solid powder to a mortar and fully grind it again, then calcinate at 550-750°C with a heating rate of 3°C / min, keep it in an argon atmosphere for 8 hours, and cool naturally with the furnace to obtain sodium vanadium phosphate. Other steps are the same...

Embodiment 3

[0033] Accurately weigh 2.5g of raw materials and 0.075g of conductive agent acetylene black. The acetylene black used as conductive agent is 3% of the total weight of raw materials. They are placed in a mortar and thoroughly ground for 2.5 hours to obtain a uniformly mixed precursor. The raw material part includes 0.567g NaF, 0.802g V 2 o 5 , 1.025g NH 4 h 2 PO 4 and 0.106g reducing agent acetylene black (V:P:F molar ratio is about 2:2:3). The well-ground precursor powder was placed in a tube furnace, and the temperature was gradually raised to 350°C at a rate of 3°C / min under an argon protective atmosphere, and kept at this temperature for 8 hours, and a solid mixture was obtained after natural cooling. Completely transfer the solid powder to a mortar and fully grind it again, then calcinate at 550-750°C with a heating rate of 3°C / min, keep it in an argon atmosphere for 8 hours, and cool naturally with the furnace to obtain sodium vanadium phosphate. Other steps are the...

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Abstract

The invention provides a preparation method of a vanadium sodium fluophosphate cathode material of a hybrid ion battery. The method comprises the following steps: 1) grinding of a mixed material: taking trivalent or pentavalent vanadium oxide (V), ammonium dihydrogen phosphate (P), sodium fluoride (F) and a reducing agent carbon source (C) as raw materials, wherein the molar ratio of V to P to F is 2:(1.9-2.3):3, the molar ratio of V to C in the reducing agent carbon source is 1:(1-2), then weighing carbon source accounting for 3-5% of the total weight of the raw materials to serve as a conductive agent, and carrying out mixed grinding to obtain a precursor mixture; 2) precalcination: precalcinating the precursor mixture for 6-10 hours at the temperature of 300-400 DEG C at the warming speed of 3-5 DEG C per minute under the protection of inert gas, cooling the mixture to room temperature and taking out the mixture for secondary grinding; and 3) secondary calcination: carrying out the secondary calcination on the mixture ground in the step 2) for 6-10 hours at the temperature of 550-750 DEG C at the warming speed of 3-5 DEG C per minute under the protection of the inert gas, and naturally cooling to room temperature to obtain the vanadium sodium fluophosphate cathode material. The vanadium sodium fluophosphate cathode material has good electrochemical performance which is obviously improved.

Description

Technical field: [0001] The invention relates to the field of material chemistry and the technical field of high-energy battery materials, in particular to a mixed ion battery sodium vanadium fluorophosphate [Na 3 V 2 (PO 4 ) 2 f 3 ] The preparation method of cathode material. Background technique: [0002] Lithium-ion batteries have the advantages of small size, light weight, large specific capacity, long cycle life, small self-discharge, and no memory effect, and have been widely used, and are steadily developing towards the goals of safety, high capacity, and long life. The research, development and application of positive electrode active materials in batteries are quite active at home and abroad, and great progress has been made, but there are still many problems restricting the scale of use of ion batteries. The use and research of ion batteries are now dominated by phosphoric acid system transition metal materials, but there are also many problems: lithium ion ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 刘素琴宋维鑫黄承焕涂飞跃冯秋菊
Owner CENT SOUTH UNIV
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