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Method for low temperature preparing lithium ion battery positive pole material phosphoric acid vanadium lithium

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: 2008-08-27
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 low temperature preparing lithium ion battery positive pole material phosphoric acid vanadium lithium
  • Method for low temperature preparing lithium ion battery positive pole material phosphoric acid vanadium lithium
  • Method for low temperature preparing lithium ion battery positive pole material phosphoric acid vanadium lithium

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Effect test

Embodiment 1

[0016] Heat 0.1mol vanadium pentoxide powder to 600°C, keep the temperature for 4 hours to make it melt, and then quickly pour it into a container filled with water to form a brownish red solution, which can be formed after standing for 16 hours. 2 o 5 ·nH 2 O wet gel. The wet gel was washed to remove most of the moisture, then vacuum-dried at 70° C. for 16 hours, and ground to obtain vanadium pentoxide gel powder. Mix the prepared vanadium pentoxide gel powder with 0.3mol lithium acetate, 0.3mol diammonium hydrogen phosphate and 0.36mol acetylene black, and then sinter at 500°C, 600°C, 700°C, and 800°C under nitrogen protection 10h, after cooling, it is the finished product 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, the particle size of the product obtained by SEM is about 1 μm. The obtained product was assembled into an experimental button battery to measure ...

Embodiment 2

[0020] Heat 0.1mol vanadium pentoxide powder to 900°C, keep the temperature constant for 1 hour to melt the vanadium pentoxide, then quickly pour it into a container filled with water to form a brownish-red solution, and leave the solution for 12 hours to form V 2 o 5 ·nH 2 O wet gel. Wash the wet gel to remove most of the moisture, then vacuum-dry it at 90° C. for 12 hours, and grind it to obtain vanadium pentoxide gel powder. After mixing the prepared vanadium pentoxide gel powder with 0.3mol lithium fluoride, 0.3mol ammonium dihydrogen phosphate and 0.36mol acetylene black, they were sintered at 700°C under the protection of argon for 10, 20, 30 and 40 hours respectively. , after cooling, the finished product 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, the particle size of the product obtained by SEM is about 1 μm. The obtained product was assembled into an e...

Embodiment 3

[0024] Heat 0.1mol vanadium pentoxide powder to 800°C, keep the temperature constant for 2 hours to melt it, then quickly pour it into a container filled with water to form a brown-red solution, and the solution can be formed after standing for 4 hours. 2 o 5 ·nH 2 O wet gel. The wet gel was washed to remove most of the water, then vacuum-dried at 100° C. for 8 hours, and ground to obtain vanadium pentoxide gel powder. Mix the prepared vanadium pentoxide gel powder with 0.3mol of lithium chloride, 0.3mol of potassium phosphate and 0.36mol of acetylene black, and heat them at 550°C, 650°C, 750°C, and 800°C under the protection of argon. After sintering for 40 hours, the finished product 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, the particle size of the product obtained by SEM is about 1 μm. The obtained product was assembled into an e...

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Abstract

The invention discloses a method for preparing anode material vanadium lithium phosphate of a lithium-ion cell at low temperature, comprising the steps of: (1) heating vanadic oxide powder to six hundred to nine hundred DEG C; allowing to melt at a constant temperature for one to four hours and pouring into a container with water rapidly to form a brown-red solution; letting the solution stand for four to sixteen hours to form wet gel V2O5.nH2O; washing the wet gel, removing most of moisture, keeping drying for four to sixteen hours in a vacuum ambient of seventy to one hundred DEG C and grinding to obtain vanadic oxide powder. (2) Mixing the vanadic oxide powder obtained through the preparation method with lithium, phosphates and acetylene black evenly at mol ratio of one to three to three to three point six, sintering for ten to forty hours at temperature between four hundred to seven hundred DEG C under the protection of an inert gas and cooling to obtain a finished product of Li3V2 (PO4)3.The preparation method solves the problem that vanadium ion is easy to be oxidized, reduces sintering temperature and cost, improves the charging and discharging performance and cycle performance of samples.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium phosphate lithium ion battery cathode material at low temperature. 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): H01M4/58H01M4/48H01M4/04C01B25/45
CPCY02E60/10
Inventor 钟胜奎刘长久王健
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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