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Preparation method of ammonium oxovanadium phosphate crystals

A technology of ammonium vanadyl phosphate and crystals, which is applied in the field of preparation of positive electrode materials, can solve problems such as difficult process control, difficulty in preparing precursors, and cumbersome preparation steps, and achieve the effects of improving conductivity, reducing agglomeration, and having a wide range of sources

Active Publication Date: 2015-05-06
固安锋行科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few relevant reports on the preparation method of lithium vanadium phosphate material precursor. It is generally believed that the preparation steps of lithium vanadium phosphate precursor are cumbersome and the process is difficult to control, and it is difficult to prepare the precursor.

Method used

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  • Preparation method of ammonium oxovanadium phosphate crystals
  • Preparation method of ammonium oxovanadium phosphate crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Dissolve 0.05mol (5.85g) of ammonium metavanadate, 0.20mol (19.60g) of phosphoric acid, and 0.10mol (19.21g) of citric acid in 100mL of deionized water, and mechanically stir in a water bath at 60°C until Uniform blue solution;

[0034] (2) Regulate pH with ammoniacal liquor (concentration is 20wt%), pH value adjusts pH=7;

[0035] (3) Then transfer it to a polytetrafluoroethylene-lined reactor (Shandong Weihai Self-Control Reactor Co., Ltd., WHFS-10 type reactor) and heat at 280°C for 30 hours, cool to room temperature, take out and filter;

[0036] (4) transfer the filtered product to a vacuum oven at 110° C. for 7 hours to obtain amorphous ammonium vanadyl phosphate powder;

[0037] (5) The amorphous ammonium vanadyl phosphate powder is fully ground in an agate mortar, placed in an air atmosphere muffle furnace, sintered at 550°C for 6h, and then cooled down to room temperature naturally to obtain vanadyl phosphate ammonium crystals. The particle size of the o...

Embodiment 2

[0040] (1) Dissolve 0.05mol (12.25g) of vanadyl oxalate, 0.20mol (26.41g) of diammonium hydrogen phosphate, and 0.50mol (87.00g) of oxalic acid in 500mL of deionized water, and mechanically stir in a water bath at 70°C until A uniform blue solution is formed;

[0041] (2) Regulate pH with ammoniacal liquor (concentration is 20%), pH value adjusts pH=10;

[0042] (3) Then transfer it to a polytetrafluoroethylene-lined reactor at 300°C for heating and reaction for 25 hours, cool to room temperature, take out and filter;

[0043] (4), then transfer the filtered product to a vacuum oven at 110° C. for drying for 9 hours to obtain amorphous ammonium vanadyl phosphate powder;

[0044] (5) The amorphous ammonium vanadyl phosphate powder is fully ground in an agate mortar and evenly placed in a muffle furnace filled with an air atmosphere and sintered at 600 ° C for 5 hours, and then naturally cooled to room temperature to obtain vanadyl phosphate ammonium crystals. The particle si...

Embodiment 3

[0047] (1) Dissolve 0.05mol (9.1g) of vanadium pentoxide, 0.8mol (78.4g) of phosphoric acid, and 0.1mol (17.61g) of ascorbic acid in 1000mL of deionized water, and mechanically stir in a water bath at 80°C until a uniform blue solution;

[0048] (2) Regulate pH with ammoniacal liquor (concentration is 25%), pH value adjusts pH=8;

[0049] (3) Then transfer it to a polytetrafluoroethylene-lined reaction kettle, heat and react at 250°C for 35h, cool to room temperature, take out and filter;

[0050] (4) transfer the filtered product to a vacuum oven at 110° C. for 9 hours to obtain amorphous ammonium vanadyl phosphate powder;

[0051] (5) The amorphous ammonium vanadyl phosphate powder is fully ground in an agate mortar and evenly placed in a muffle furnace filled with an air atmosphere and sintered at 650 ° C for 4 hours, and then naturally cooled to room temperature to obtain vanadyl phosphate ammonium crystals. The particle size of the ammonium vanadyl phosphate material o...

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Abstract

The invention belongs to the field of battery materials, and provides a preparation method of ammonium oxovanadium phosphate crystals. The preparation method comprises the following steps of: (1) dissolving a vanadium source, a phosphorus source and a carbonaceous organic material into water to obtain a solution; (2) stirring in a 20-100 DEG C constant-temperature water bath; (3) adjusting the pH value to 3-14; (4) heating and reacting for 1-72h to obtain gel; (5) drying under a vacuum condition to form an amorphous-state ammonium oxovanadium phosphate precursor; and (6) sintering for 2-20h at 300-750 DEG C in an oxidizing atmosphere, cooling to room temperature. The invention provides a simple method for preparing ammonium oxovanadium phosphate crystals, the reaction process is easy to control, the requirement of green chemistry is met, the method is applicable to industrial mass production; the used raw materials are easily available and the cost is low; the carbonaceous organic material can effectively improve the dispersibility of vanadium ions and phosphate radicals in the solution, so as to reduce the occurrence of agglomeration phenomenon. Furthermore, a coating carbon source is provided for the ammonium oxovanadium phosphate material, and the electrical conductivity of the material is improved.

Description

technical field [0001] The invention belongs to the field of battery materials, and in particular relates to a preparation method of a positive electrode material of a lithium ion battery. Background technique [0002] The progress and development of mankind is also accompanied by the rapid depletion of fossil energy; the burning of fossil energy also leads to inevitable environmental pollution. Among them, the exhaust gas emitted by automobiles is the main cause of air pollution. Therefore, the development and application of electric vehicles (EV) or hybrid electric vehicles (HEV) and corresponding power sources have been rapidly developed. In the existing power battery system, the lithium-ion secondary battery has the advantages of high volume energy ratio and weight energy ratio, high voltage, low self-discharge rate, no memory effect, long cycle life, etc., as EV and HEV power energy. Absolute advantage. [0003] Lithium-ion battery cathode material is the key and cor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCC01B25/26C01B25/45H01M4/1397H01M4/58H01M10/0525Y02E60/10
Inventor 郑淑芬贾跃祥赵南南
Owner 固安锋行科技有限公司
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