A method for preparing nanoscale lithium iron phosphate by self-sacrificing template method

A technology of lithium iron phosphate and sacrificial templates, which is applied in the field of electrochemistry, can solve the problems of difficult control of particle shape, complicated preparation process, narrow size distribution range, etc., and achieve good reversibility of lithium deintercalation, uniform chemical composition, The effect of uniform mixing of reactants

Active Publication Date: 2011-12-07
DONGFANG ELECTRIC CORP LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, based on the limitation of the high-temperature solid-state reaction itself, due to the long-term heat treatment at high temperature, the LiFePO prepared by the high-temperature solid-state method 4 Large particle size, uneven distribution, and difficult to control particle shape
Preparation of LiFePO by liquid phase methods such as hydrothermal method 4 The advantages and disadvantages of the method are obvious: the advantages are that the raw materials are mixed between molecules, the mixing u...

Method used

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  • A method for preparing nanoscale lithium iron phosphate by self-sacrificing template method
  • A method for preparing nanoscale lithium iron phosphate by self-sacrificing template method
  • A method for preparing nanoscale lithium iron phosphate by self-sacrificing template method

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Embodiment 1

[0037] 1. With FeCl 3 and NH 4 h 2 PO 4 The raw materials are respectively prepared into aqueous solutions with a concentration of 0.1mol / L; according to Fe 3+ :PO 4 3+ The molar ratio is 1:1.1, weighed and placed in the reaction container, and stirred at a speed of 30 r / min, then added ammonia water to adjust the pH of the solution to 4, and reacted at 80°C for 5 hours to obtain amorphous iron phosphate precipitation ; After the precipitate is filtered, it is washed with deionized water and alcohol until the washing liquid is neutral to remove impurity ions, and then the precipitate is dried in an oven at 60°C for 10 hours to obtain nano-scale FePO 4 . wxya 2 O, then calcined in an air atmosphere at 550°C for 8 hours, then slowly cooled to room temperature with the furnace, and then ground and pulverized to obtain a crystalline nano-iron phosphate template; weigh lithium hydroxide and the prepared iron phosphate template in a molar ratio of 1.01:1 At the same time, af...

Embodiment 2

[0043] with FeCl 3 and (NH 4 ) 2 HPO 4 The raw materials are respectively prepared into aqueous solutions with a concentration of 1mol / L; according to Fe 3+ :PO 4 3+ The molar ratio is 1:1.2, weighed and placed in the reaction container, and stirred at a speed of 40 r / min, then added ammonia water to adjust the pH of the solution to 6, and reacted at 90°C for 5 hours to obtain amorphous iron phosphate precipitation ; After filtering the precipitate, wash it with deionized water and alcohol until the washing liquid is neutral to remove impurity ions, and then dry the precipitate in an oven at 70°C for 10 hours to obtain nano-scale FePO 4 . wxya 2 O, then calcined in an air atmosphere at 600°C for 8 hours, then slowly cooled to room temperature with the furnace, and then ground and pulverized to obtain a crystalline nano-iron phosphate template; weigh lithium carbonate and the prepared iron phosphate template at a molar ratio of 0.51:1 At the same time, after adding 45g ...

Embodiment 3

[0047] With Fe(NO 3 ) 3 and NH 4 h 2 PO 4 The raw materials are respectively prepared into aqueous solutions with a concentration of 4mol / L; according to Fe 3+ :PO 4 3+ The molar ratio is 1:1.3, weighed and placed in a reaction container, and stirred at a speed of 40 r / min, then added ammonia water to adjust the pH of the solution to 3, and reacted at 70°C for 6 hours to obtain amorphous iron phosphate precipitation ; After the precipitate is filtered, it is washed with deionized water and alcohol until the washing liquid is neutral to remove impurity ions, and then the precipitate is dried in an oven at 90°C for 6 hours to obtain nano-scale FePO 4 . wxya 2 O, then calcined in an air atmosphere at 650°C for 12 hours, then slowly cooled to room temperature with the furnace, and then ground and pulverized to obtain a crystalline nano-iron phosphate template; weigh lithium acetate and the prepared iron phosphate template at a molar ratio of 1.03:1 At the same time, after...

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Abstract

The invention relates to a self-sacrificing template method for preparing nanoscale lithium ferrous phosphate used as a cell cathode material and belongs to the field of electrochemistry. The method comprises the following specific steps: dissolving inorganic compound raw materials containing Fe<3+> and PO4<3+> in an aqueous solution, adjusting the pH value of the solution to 1-6, reacting at thetemperature of 60-150 DEG C for 3-10 hours, filtering, washing to obtain amorphous nano iron phosphate, and then baking at the temperature of 450-750 DEG C in air atmosphere for 4-16 hours to obtain a crystalline nano iron phosphate template; and on the basis of utilizing crystalline nano iron phosphate as a template, dissolving iron phosphate, a Li<+>-containing compound and a carbon-containing organic matter in water, stirring and mixing uniformly, after spray-drying, and baking at the temperature of 450-800 DEG C in a/an nitrogen/argon protective atmosphere furnace to prepare a grey-black lithium ferrous phosphate (LiFePO4)/C material. The preparation method provided by the invention is simple and low in cost; and the prepared lithium ferrous phosphate material has the advantages of high purity, good consistency, integral crystal structure, small and uniform particles and excellent electrochemical performance.

Description

technical field [0001] The invention relates to a preparation method of lithium ferrous phosphate, a positive electrode material of a lithium ion battery, in particular to a method for preparing nanoscale lithium ferrous phosphate by a self-sacrificing template method, which belongs to the field of electrochemistry. Background technique [0002] The continuous deterioration of the global environment and the continuous shortage of energy supply are two major problems that mankind must face in the 21st century. The development and application of new energy and renewable clean energy has become an urgent task. Renewable resources such as wind energy, solar energy, and tidal energy are increasingly being used for power generation by humans, and green and environmentally friendly batteries as storage units for electric energy have also become research hotspots at home and abroad. Lithium-ion secondary battery, as a new type of green battery, has developed quite rapidly since it c...

Claims

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Application Information

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IPC IPC(8): C01B25/45B82Y40/00
Inventor 郑威王瑨梁孜谢皎李玉龙王睿
Owner DONGFANG ELECTRIC CORP LTD
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