Method for preparing cathode material lithium vanadium phosphate of lithium ion battery by using fast sol-gel method

A technology of lithium ion battery and sol-gel method, which is applied in the field of lithium vanadium phosphate preparation lithium ion battery positive electrode material, can solve the problems of high equipment requirements, lower product roasting temperature, large material particles, etc., and achieve simplified synthesis process, roasting The effect of shortening the time and uniform material particles

Inactive Publication Date: 2010-09-22
NANCHANG UNIV
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Problems solved by technology

The traditional solid-phase method requires repeated grinding, a calcination temperature greater than 900°C, and a calcination time of more than 16 hours. The obtained material particles are large, uneven, and prone to impurities; hydrothermal synthesis and rheological phase synthesis. The requirements for synthetic equipment are high, and it is difficult to apply to industrial production. Compared with these methods, the sol-gel method can not only realize the mixing of reactants at the molecular level, reduce the particle size of the material, but also reduce the temperature of product roasting. Also easy to operate
However, the traditional sol-gel method usually takes several days to obtain the precursor, resulting in too long a time to produce the product, which is not conducive to the realization of industrialization

Method used

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  • Method for preparing cathode material lithium vanadium phosphate of lithium ion battery by using fast sol-gel method
  • Method for preparing cathode material lithium vanadium phosphate of lithium ion battery by using fast sol-gel method
  • Method for preparing cathode material lithium vanadium phosphate of lithium ion battery by using fast sol-gel method

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Experimental program
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Effect test

Embodiment 1

[0019] Dissolve 0.03 mol of vanadium pentoxide powder in a saturated solution of 0.1 mol of citric acid, stir at 60°C for 15 min, then add 0.093 mol of lithium acetate, 0.09 mol of diammonium hydrogen phosphate and 0.2 g of glucose, and continue stirring for 4 h. After drying at 100°C, pre-decompose at 300°C for 4 hours under the protection of argon, then mix 0.2g of polyaniline and grind for 2 hours, and then bake at 750°C for 4 hours under the protection of argon, and the finished Li is obtained after cooling. 3 V 2 (PO 4 ) 3 / C. The obtained product shows through X-ray diffraction analysis, see figure 1 As shown in b, without any impurities, it is pure phase Li 3 V 2 (PO 4 ) 3 . figure 2 It is the scanning electron microscope picture of the product. It can be seen from the picture that the size of the prepared product is at the nanometer level, the size is about 500-600nm, and the surface is covered with a layer of uniform nano-carbon particles.

Embodiment 2

[0021] Dissolve 0.02 mol of vanadium pentoxide powder in a solution containing 0.06 mol of oxalic acid, stir at 80°C for 20 min, then add 0.06 mol of lithium chloride, 0.061 mol of ammonium dihydrogen phosphate and 0.25 g of glucose and continue stirring for 2 h, 100 After drying at ℃, pre-decompose at 350℃ for 3h under the protection of nitrogen, then mix 0.25g of acetylene black and grind for 1h, then roast at 800℃ for 3h under the protection of nitrogen, and the finished Li 3 V 2 (PO 4 ) 3 / C. The obtained product shows through X-ray diffraction analysis, see figure 1 As shown in c, without any impurities, it is pure phase Li 3 V 2 (PO 4 ) 3 . The first charge and discharge curve of the lithium vanadium phosphate positive electrode material is as follows: image 3 As shown, the discharge specific capacity can reach 158mAh / g in the range of 3.0-4.8V, and the charge-discharge voltage platform is consistent, indicating that the material has good reversibility.

Embodiment 3

[0023] Dissolve 0.05 mol of vanadium pentoxide powder in a solution containing 0.15 mol of oxalic acid, stir at 65°C for 30 min, then add 0.0765 mol of lithium carbonate, 0.145 mol of sodium phosphate and 1 g of polyethylene glycol (molecular formula 300) , continue to stir for 3 hours, after drying at 100°C, pre-decompose at 400°C for 2 hours under the protection of argon-hydrogen mixture gas, then mix Super P and grind for 2 hours, and then roast at 850°C for 2 hours under the protection of argon-hydrogen mixture gas, and after cooling, the finished Li 3 V 2 (PO 4 ) 3 / C. The obtained product shows through X-ray diffraction analysis, see figure 1 As shown in d, without any impurities, it is pure phase Li 3 V 2 (PO 4 ) 3 . The lithium vanadium phosphate positive electrode material is charged and discharged in the range of 3.0-4.8V, and the rate of 0.1C is as follows: Figure 4 As shown, the highest discharge capacity can reach 173mAh / g, and after 50 cycles, the capac...

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Abstract

The invention discloses a method for preparing a cathode material lithium vanadium phosphate of a lithium ion battery by using a fast sol-gel method, which specifically comprises the following steps of: (1) adding vanadic oxide into the solution of a reducing acid, heating the mixed solution to 60 to 80 DEG C and stirring the mixed solution for 10 to 50 minutes at a constant temperature to obtain blue solution; (2) adding lithium salts into the blue solution, wherein a stoichiometric ratio of the lithium salts to the vanadic oxide is 3-3.2: 2.9-3.05: 0.95-1.05; (3) treating an obtained powder material in an inert atmosphere at 200 to 400 DEG C for 2 to 4 hours to obtain a precursor; and (4) mixing and grinding uniformly the obtained precursor and another carbon source and cooling the mixture to obtain the cathode material lithium vanadium phosphate of the lithium ion battery. The method has the advantages that: (1) a synthesis process is simplified, the cost is reduced and the method is applied to industrial production; (2) the baking time is greatly shortened, the granularity of the product is reduced and the synthesized material has a nano-size; and (3) the carbon source is mixed before baking, carbon granules also can prohibit the growth of material granules and the synthesized material granules are uniform and fine.

Description

technical field [0001] The invention relates to a method for preparing lithium vanadium phosphate, a positive electrode material of a lithium ion battery, in particular to a method for preparing lithium vanadium phosphate, a positive electrode material for a lithium ion battery, by a rapid sol-gel method. Background technique [0002] As a technology that can safely and effectively realize the conversion and storage of chemical energy and electrical energy, chemical power technology has set off a research boom in the world. Lithium-ion batteries are regarded as one of the most potential chemical power sources because of their small size, light weight, high working voltage, high specific energy, long cycle life, no memory effect, and small self-discharge. At present, lithium-ion batteries have played their unique advantages in some markets in the fields of electric vehicles (EV), hybrid electric vehicles (HEV), electric bicycles (EB), and power tools (PT). As the most critic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397H01M4/58
Inventor 张宁程睿杨震宇张荣斌古宁宇
Owner NANCHANG UNIV
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