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Method for producing lithium ion battery anode material vanadium lithium phosphate by sol-gel method

A technology for lithium-ion batteries and positive electrode materials, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve poor conductivity and cycle performance, uneven particle size distribution of synthetic materials, uneven particle size distribution of materials, etc. problems, to achieve the effect of easy control, inhibition of excessive growth, and simple and convenient methods

Inactive Publication Date: 2008-12-03
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The hydrogen reduction method uses pure H 2 As a reducing agent, due to the H 2 It is very dangerous due to its flammable and explosive properties, which is not conducive to industrial production
Moreover, the particle size distribution of the synthesized material is not uniform, and the electrical conductivity is low.
Due to the relatively high reaction temperature required by the high-temperature carbothermal reduction method, the particle size distribution of the synthesized material is uneven, and the electrical conductivity and cycle performance are not good.

Method used

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  • Method for producing lithium ion battery anode material vanadium lithium phosphate by sol-gel method
  • Method for producing lithium ion battery anode material vanadium lithium phosphate by sol-gel method
  • Method for producing lithium ion battery anode material vanadium lithium phosphate by sol-gel method

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Experimental program
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Effect test

Embodiment 1

[0017] Heat 0.095mol of vanadium pentoxide powder to 600°C, keep it at constant temperature for 4 hours to make it melt, then quickly pour it into a container filled with water to form a brownish-red solution, then add 0.31mol of lithium acetate and 0.305mol of diammonium hydrogen phosphate to the solution and 0.105mol ascorbic acid, after mixing evenly, sintering at 400°C, 500°C, 600°C, and 700°C for 5 hours under the protection of nitrogen, and the finished Li 3 V 2 (PO 4 ) 3 . The obtained products were analyzed by X-ray diffraction, showing that they were all Li 3 V 2 (PO 4 ) 3 , without any impurity phase, the particle size of the product obtained by SEM is about 0.5 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles are shown in Table 1.

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Embodiment 2

[0021] Heat 0.10mol of vanadium pentoxide powder to 900°C and keep the temperature constant for 1 hour to melt the vanadium pentoxide and quickly pour it into a container filled with water to form a brown-red solution, then add 0.30mol of lithium fluoride and 0.30mol of Ammonium dihydrogen phosphate and 0.10 mol of adipic acid are mixed evenly, and then sintered at 600°C under the protection of argon for 5, 10, 15 and 20 hours respectively, and the finished Li is obtained after cooling. 3 V 2 (PO 4 ) 3 . The obtained products were analyzed by X-ray diffraction, showing that they were all Li 3 V 2 (PO 4 ) 3 , without any impurity phase, the particle size of the product obtained by SEM is about 0.5 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles ar...

Embodiment 3

[0025] Heat 0.105mol of vanadium pentoxide powder to 800°C, keep it at constant temperature for 2 hours to make it melt, then quickly pour it into a container filled with water to form a brownish red solution, then add 0.305mol of lithium chloride, 0.31mol of potassium phosphate and 0.105mol of malonic acid, mixed evenly, sintered at 450°C, 550°C, 650°C, and 700°C for 20h under the protection of argon, and the finished Li 3 V 2 (PO 4 ) 3 . The obtained products were analyzed by X-ray diffraction, showing that they were all Li 3 V 2 (PO 4 ) 3 , without any impurity phase, the particle size of the product obtained by SEM is about 0.5 μm. The obtained product was assembled into an experimental button battery to measure its charge-discharge specific capacity and cycle performance. The charge-discharge was carried out at a rate of 1C. The initial discharge capacity and the discharge capacity after 30 cycles are shown in Table 3.

[0026] Experimental condition and result of...

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Abstract

The invention discloses a method for preparing lithium ion battery anode material vanadium lithium phosphoric acid by a sol-gel method. The method of the invention comprises the following steps: the vanadium pentoxide powder is heated to 600-900 DEG C and the temperature is kept for 1-4 hours till the power is melted; the melted powder is rapidly dumped into a container with water to form a brownish red solution; subsequently, lithium salt, phosphate and organic acid are added into the solution; the solution is uniformly mixed and then sintered for 5-20 hours under the protection of inert gas so as to form a finished product LI3V2(PO4)3 after being cooled. The method of the invention solves the problem that the vanadium ion is easy to be oxidated, the sintering temperature and the cost are reduced, and the charging and discharging performance and the circulation performance of the samples are improved.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium phosphate lithium ion battery cathode material by a sol-gel method. Background technique [0002] Li 3 V 2 (PO 4 ) 3 The material has the advantages of good reversible performance, abundant raw materials, and high specific capacity (theoretical capacity is 197mAh / g). But it has the following disadvantages that hinder its practical application: (1) V in synthesis 3+ easily oxidized to V 5+ , it is not easy to obtain single-phase Li 3 V 2 (PO 4 ) 3 (2) Lithium ions in Li 3 V 2 (PO 4 ) 3 Diffusion is difficult in medium, resulting in low utilization of active materials; (3) Li 3 V 2 (PO 4 ) 3 The conductivity itself is also very low, resulting in poor high-current discharge performance. Existing research improves Li through the following aspects 3 V 2 (PO 4 ) 3 Performance: (1) Use an inert atmosphere to protect V 3+ ; (2) Synthesize Li with small particle size 3 V 2...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/48H01M4/04C01B25/45C04B35/624
CPCY02E60/10
Inventor 钟胜奎王健刘乐通刘洁群姜吉琼
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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