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Method for preparing spherical composite anode material fluorine lithium vanadium phosphate-lithium vanadium phosphate of lithium ion battery

A composite cathode material, lithium-ion battery technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of cycle performance and rate performance need to be further improved, and achieve easy oxidation, fine particles, and excellent electrochemical performance. Effect

Active Publication Date: 2012-07-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its cycle performance and rate performance still need to be further improved.

Method used

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  • Method for preparing spherical composite anode material fluorine lithium vanadium phosphate-lithium vanadium phosphate of lithium ion battery
  • Method for preparing spherical composite anode material fluorine lithium vanadium phosphate-lithium vanadium phosphate of lithium ion battery
  • Method for preparing spherical composite anode material fluorine lithium vanadium phosphate-lithium vanadium phosphate of lithium ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Using lithium hydroxide, lithium fluoride, vanadium pentoxide, and ammonium dihydrogen phosphate as raw materials, press 0.5LiVPO 4 F. Li 3 V 2 (PO 4 ) 3 The stoichiometric ratio of the ingredients, adding oxalic acid (added by 2 times the theoretical amount), ball milling until the pentavalent vanadium is completely reduced to trivalent vanadium, adding water to dissolve and disperse, and then spray-dry the resulting suspension, the air inlet temperature 110°C, the air outlet temperature is 100°C, and finally in an argon atmosphere at 500°C, 600°C, 700°C, 800°C and 900°C for 24 hours to obtain a spherical composite cathode material 0.5LiVPO 4 F. Li 3 V 2 (PO 4 ) 3 , The resulting product was assembled into a button battery and its charge and discharge capacity and rate performance were measured within the voltage range of 3.0-4.5V. Charge and discharge at different rates, the first discharge specific capacity is shown in Table 1.

[0031] Experimental conditio...

Embodiment 2

[0034] Using lithium carbonate, vanadium trifluoride, ammonium metavanadate, and diammonium hydrogen phosphate as raw materials, press 5LiVPO 4 F. Li 3 V 2 (PO 4 ) 3 The stoichiometric ratio of ingredients, adding ascorbic acid (adding 5 times the theoretical amount), then adding water, and mixing evenly, stirring at a constant temperature in a water bath at 50 ° C until the pentavalent vanadium is completely reduced to trivalent vanadium and a uniform solution is generated. Then the resulting solution was spray-dried, the air inlet temperature was 250°C, the air outlet temperature was 130°C, and finally kept at 700°C in a nitrogen atmosphere for 2, 6, 12, and 18 hours to obtain the spherical composite cathode material 5LiVPO 4 F. Li 3 V 2 (PO 4 ) 3 , the resulting product was assembled into a button battery, and its charge and discharge capacity and rate performance were measured within the voltage range of 3.0 to 4.5V. The charge and discharge were carried out at diff...

Embodiment 3

[0038] Using lithium hydrogen fluoride, ammonium fluoride, vanadium dioxide, and triammonium phosphate as raw materials, press 50LiVPO 4 F. Li 3 V 2 (PO 4 ) 3Add hydrazine hydrate (according to 3 times the theoretical amount) and water, keep the temperature in a water bath at 20°C until the tetravalent vanadium is completely reduced to trivalent vanadium and form a uniform solution, and then the resulting solution is spray-dried , the air inlet temperature is 300°C, the air outlet temperature is 180°C, and finally kept at 650°C for 10 hours in a nitrogen atmosphere to obtain a spherical composite cathode material 20LiVPO 4 F. Li 3 V 2 (PO 4 ) 3 , the resulting product was assembled into a button battery, and its charge and discharge capacity and rate performance were measured within the voltage range of 3.0 to 4.5V. The charge and discharge were carried out at different rates, and its first discharge ratio at 0.5C, 2C, 5C and 10C rates The capacity is 150.7mAh·g -1 , ...

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Abstract

The invention discloses a method for preparing a spherical composite anode material, i.e. fluorine lithium vanadium phosphate-lithium vanadium phosphate, of a lithium ion battery. The method is characterized by preparing the spherical composite anode material, i.e. the fluorine lithium vanadium phosphate-lithium vanadium phosphate, of the lithium ion battery by adopting a chemical reduction-spray drying method and specifically comprises the following steps of: mixing a lithium source, a vanadium source, a fluorine source and a phosphorus source according to the ratio of xLiVPO4F.Li3V2(PO4)3, adding a reductant to carry out chemical reduction so as to reduce the high-valent vanadium to three-valent vanadium and obtain a homogeneous solution, sol or suspension; carrying out spray drying to obtain a product; and heating the product to the temperature of 500-900 DEG C in a non-oxidizing atmosphere, carrying out constant temperature for 2-24 hours, and then, obtaining the fluorine lithium vanadium phosphate-lithium vanadium phosphate, i.e. the spherical composite anode material. The fluorine lithium vanadium phosphate-lithium vanadium phosphate, i.e. the spherical composite anode material prepared by the method has excellent magnification performance and cycling performance.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials and preparation methods thereof, and relates to a preparation method of lithium vanadium phosphate-lithium vanadium phosphate, a composite positive electrode material of a spherical lithium ion battery. Background technique [0002] Lithium vanadium phosphate (Li vanadium phosphate) as a positive electrode material for phosphate-based lithium-ion batteries with a three-dimensional spatial structure 3 V 2 (PO 4 ) 3 ), is considered to be a reliable cathode material for power vehicles due to its advantages of low cost, good reversibility of lithium deintercalation, and good thermal stability. However, its poor electronic conductivity limits its application. [0003] Lithium vanadium fluorophosphate (LiVPO 4 F) is a new type of polyanion material, its structure is a PO 4 Tetrahedron and VO 4 f 2 A three-dimensional framework network constructed by octahedra, where PO 4 Tetrahedro...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 王志兴王接喜李新海郭华军彭文杰胡启阳张云河黄思林肖玮
Owner CENT SOUTH UNIV