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Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery

A lithium-ion battery, sodium vanadium fluorophosphate technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of not too large input of one-time raw materials, difficult to achieve large-scale production, environmental pollution, etc. Chemical properties, convenient for large-scale production, and the effect of simple and easy methods

Inactive Publication Date: 2012-06-20
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using this synthesis method, although it is a one-step synthesis, due to the sol-gel processing, the raw materials are required to be soluble, and the one-time raw material input should not be too large, the operation is inconvenient, and a large amount of organic matter is decomposed to cause waste of resources. and environmental pollution, the cost is high, and it is difficult to achieve large-scale production

Method used

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  • Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery
  • Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery
  • Method for preparing positive material fluorine-doped sodium vanadium phosphate of sodium-containing lithium ion battery

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Embodiment 1

[0032] 0.052mol vanadium pentoxide, 0.156mol ammonium fluoride, 0.156mol sodium bicarbonate, 0.104mol ammonium dihydrogen phosphate and 6g glucose were mixed and dispersed in ethanol, placed in a ball mill, and mechanically Activation for 8h. The mechanically activated material is roasted at 600°C for 24 hours under the protection of argon, and the product Na 3 V 2 (PO 4 ) 2 f 3 / C. The X-ray diffraction analysis of the obtained product is as follows: figure 1 As shown, the analysis shows that the product prepared by this formula also has a small amount of Na 3 V 2 (PO 4 ) 3 In the heterogeneous phase, there is no carbon peak in the spectrum, which shows that glucose is decomposed into amorphous carbon at high temperature. The obtained product was assembled into an experimental button battery, and the electrochemical performance of charge and discharge was tested. The test results showed that the first discharge specific capacity of the material at the rate of 0.5C, ...

Embodiment 2

[0034] 0.052mol vanadium pentoxide, 0.156mol ammonium dihydrogen phosphate, 0.156mol sodium hydroxide and 6g glucose were mixed and dispersed in ethanol, placed in a ball mill, and mechanically activated at 800 rpm for 8 hours. The mechanically activated material was roasted at 900°C for 8 hours under the protection of argon, and the product Na was obtained after cooling. 3 V 2 (PO 4 ) 3 / C. SEM analysis of materials such as image 3 As shown, the analysis showed that the particle size of the product was around 1 μm. The obtained product was assembled into an experimental button battery, and its charge-discharge electrochemical performance was tested at a rate of 0.1C. The test results showed that the first discharge specific capacity was 109mAh·g -1 , and a constant voltage platform appears near the 3.7V voltage, and there is no obvious constant voltage platform near the 4.2V voltage. The first charge and discharge curve of the material at 0.1C is as follows Figure 4 ...

Embodiment 3

[0036] 0.052mol vanadium pentoxide, 0.13mol ammonium dihydrogen phosphate, 0.156mol sodium hydroxide, 0.075mol ammonium fluoride and 6g glucose were mixed and dispersed in ethanol, placed in a ball mill, and mechanically Activate for 10h. The mechanically activated material was roasted at 700°C for 12 hours under the protection of argon, and the product Na was obtained after cooling. 3 V 2 (PO 4 ) 2.5 f 1.5 / C. The obtained product was assembled into an experimental button battery, and the electrochemical performance of the material was tested. The results showed that the material material not only appeared a constant voltage platform near a voltage of 3.7V, but also appeared a constant voltage platform near a voltage of 4.2V. The first charge and discharge curve of the material at 0.5C rate is as follows Figure 5 As shown, the cycle curve of the material at 5C rate is as follows Image 6 shown.

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Abstract

The invention relates to a method for preparing positive material fluorine-doped sodium vanadium phosphate of a sodium-containing lithium ion battery, and particularly relates to a method for preparing Na3V2(PO4)3-x / 3Fx (x is not smaller than 0 and not less than 6) by mechanical activation-assisted one-step high-temperature solid state reaction. The method comprises the following steps: dispersing sodium (Na) source, vanadium (V) source, phosphorus (P) source, fluorine (F) source, and carbon (C) source with reducing and conductive effect in a certain amount of liquid dispersion medium; high-speed ball milling the blended materials for mechanical activation; calcining the activated material at 450 to 1000 DEG C for 1 to 72 hours in an inert or reducing atmosphere; and cooling to obtain the final product. The positive material Na3V2(PO4)3-x / 3Fx prepared by the method has good electrochemical property. The method provided by the invention has the advantages of simple and convenient process, easy control, low cost, and friendly environment, and the synthesis process is simplified so as to facilitate large-scale production.

Description

technical field [0001] The invention relates to a method for preparing a positive electrode material of a sodium-containing lithium ion battery, that is, a method for preparing a sodium-containing lithium ion battery positive electrode material by a one-step high-temperature solid-phase method assisted by mechanical activation, which belongs to the preparation of new energy materials technology field. Background technique [0002] With the continuous development of the lithium-ion battery industry, especially the rise of electric vehicles, the market demand for lithium-ion batteries is constantly increasing, which brings a strong demand for lithium resources. However, at present, lithium resources are mostly stored in salt lakes, and extracting lithium from salt lakes is still a high-cost process, which has become a bottleneck restricting the rapid development of the lithium-ion battery industry. If we can consider replacing lithium with other cheaper elements, it will brea...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 杜柯郭宏伟胡国荣彭忠东曹雁冰张罗虎
Owner CENT SOUTH UNIV
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