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Preparation method of lithium iron phosphate cathode material with high rate, high capacity and low temperature performance by reverse salting out method

A low temperature performance, lithium iron phosphate technology, applied in chemical instruments and methods, battery electrodes, phosphorus compounds, etc., can solve the problems of poor low temperature performance, poor rate performance, poor conductivity of lithium iron phosphate, etc., and achieve a small specific surface area. Effect

Active Publication Date: 2020-02-14
SHANDONG GOLDENCELL ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this material also has some shortcomings, which hinder its practical application. First, the low temperature performance is poor; second, lithium iron phosphate (LiFePO 4 ) poor conductivity,
[0004] Therefore, the rate performance is not good

Method used

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  • Preparation method of lithium iron phosphate cathode material with high rate, high capacity and low temperature performance by reverse salting out method
  • Preparation method of lithium iron phosphate cathode material with high rate, high capacity and low temperature performance by reverse salting out method
  • Preparation method of lithium iron phosphate cathode material with high rate, high capacity and low temperature performance by reverse salting out method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Ferric phosphate and glucose are mixed at a mass ratio of 12:1, and the solid content is controlled at 45%. After mechanical mixing and stirring, microwave drying is performed to control the water content at 20%. Then, the material was sintered at 325° C. under nitrogen and maintained at a pressure of 0.8 MPa for 3 hours.

[0026] (2) Cyclic salting-out crystallization: the product in (1), lithium acetate, glucose in a mass ratio of 13:10.5:0.5, with deionized water as a solvent, with a solid content of 72%, first mechanically stirred at 65°C until When the solid content is below 50%, stand still until the slurry is dry and crystallized; then continue to add deionized water until the solid content is 72%, and repeat salting out until the surface distribution is relatively uniform.

[0027] (3) Tablet shaping: the product in step (2) is mixed with glucose at a mass ratio of 14:0.5, the solid content is controlled at 30%, mechanically stirred, and microwave-dried. Th...

Embodiment 2

[0030] (1) Iron phosphate and sucrose are mixed according to a mass ratio of 12:1, and the solid content is controlled at 45%. After mechanical mixing and stirring, microwave drying is performed to control the water content at 25%. The material was then placed under nitrogen conditions at 325°C,

[0031] And keep the pressure of 0.7MPa for sintering for 3h.

[0032] (2) Cyclic salting out crystallization: mix the product in (1), lithium hydroxide, and sucrose at a mass ratio of 13:5:0.5, use deionized water as a solvent, and have a solid content of 80%, and mechanically stir at 50°C Until the solid content is below 45%, stand still until the slurry is dry and crystallized; then continue to add deionized water until the solid content is 80%, and repeatedly carry out salting out until the surface distribution is relatively uniform.

[0033] (3) Tablet shaping: the product in step (2) is mixed with soluble carbohydrates at a mass ratio of 7:0.5, the solid content is controlled a...

Embodiment 3

[0036] (1) Ferric phosphate and citric acid are mixed at a mass ratio of 12:1, and the solid content is controlled at 45%. After mechanical mixing and stirring, microwave drying is performed to control the water content at 25%. Then the material was sintered at 325° C. under nitrogen and maintained at a pressure of 0.7 MPa for 3 hours.

[0037] (2) Cyclic salting out crystallization: the product in (1), lithium carbonate, and sucrose in a mass ratio of 13:5:10:0.5, using deionized water as a solvent, with a solid content of 65%, first mechanically at 50°C Stir until the solid content is below 30%, stand still until the slurry is dry and crystallized; then continue to add deionized water until the solid content is 65%, and repeat salting out until the surface distribution is relatively uniform.

[0038] (3) Tablet shaping: the product in step (2) is mixed with citric acid in a mass ratio of 7:0.5, the solid content is controlled at 30%, mechanically stirred, and microwave-dried...

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Abstract

The invention discloses a preparation method for a lithium iron phosphate positive electrode material with high rate, high capacity and excellent low-temperature performance by a reverse salting out method. The preparation method aims to synthesize a lithium iron phosphate material by a novel method which is relatively easy to implement, and the electrical conductivity of the material is improved.The preparation method comprises the steps of (1) performing high-pressure permeation; (2) performing salting out and crystallization in a circulation way; (3) tabletting and shaping; and (4) performing high-temperature sintering to form a three-dimensional structure, in which heat preservation is performed on a material of the step (3) for 4-12 hours at 600-800 DEG C, nitrogen is needed to be introduced during the whole sintering process, and the pressure is maintained at 0.1-1MPa. The preparation method has the advantages that a few amount of raw materials for synthesis are used, the process is simple and is easy to operate, the electrical conductivity of the synthesized lithium iron phosphate material reaches 10<-2>s / cm under the condition that other additives are not added, the specific area is small and can reach 10m<2> / g, half-cell test shows that the discharging capacity retention rate is 90.9% after circulation for 1,000 periods at 1C, the initial discharging specific capacityis 200.0mAh / g at 0.2C, and the capacity is 125mAh / g or above at 5C.

Description

technical field [0001] The invention belongs to the battery cathode material in the field of materials, and in particular relates to a method for preparing a lithium iron phosphate cathode material by a reverse salting-out method. Background technique [0002] Lithium-ion batteries are the necessary power sources for mobile electronic devices in today's society, and are composed of positive electrodes, negative electrodes, separators, and electrolytes. Its key performance indicators such as: rate performance and cycle life, [0003] It is determined by the electrochemical performance of the cathode material. Lithium iron phosphate (LiFePO 4 ) The theoretical specific capacity is 170mAh / g, the discharge platform is 3.4V, it has good cycle performance and thermal stability, and its non-toxic, cheap and other characteristics make it expected to become a new generation of lithium-ion battery cathode materials. However, this material also has some shortcomings, which hinder it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M10/0525C01B25/45
CPCY02E60/10
Inventor 薛娟娟孟博杜显振
Owner SHANDONG GOLDENCELL ELECTRONICS TECH