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Preparation method for fluorine-doped nickel-cobalt-manganese system ternary positive electrode material and prepared material

A cathode material, nickel-cobalt-manganese technology, which is applied in the field of preparing fluorine-doped nickel-cobalt-manganese-based ternary cathode materials by molten salt method, can solve the problems of high reaction time and reaction temperature, reduced battery performance, uneven heating, and the like. Achieve the effect of low production cost, good consistency and large diffusion rate

Inactive Publication Date: 2017-04-26
HUBEI JINQUAN NEW MATERIALS CO LTD
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  • Application Information

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Problems solved by technology

[0012] Aiming at the problems of non-uniform heating, high reaction time and high reaction temperature in the existing preparation method of nickel-cobalt-manganese series positive electrode materials, thereby reducing the performance of the battery, the present invention provides a molten salt method for preparing fluorine-doped nickel-cobalt Manganese-based ternary cathode material, method and prepared material

Method used

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  • Preparation method for fluorine-doped nickel-cobalt-manganese system ternary positive electrode material and prepared material
  • Preparation method for fluorine-doped nickel-cobalt-manganese system ternary positive electrode material and prepared material
  • Preparation method for fluorine-doped nickel-cobalt-manganese system ternary positive electrode material and prepared material

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preparation example Construction

[0070] The specific embodiment of the present invention provides a method for preparing a fluorine-doped nickel-cobalt-manganese ternary cathode material. The method includes the following steps:

[0071] (1) Mixing the transition metal source aqueous solution, lye and ammonia, stirring and heating for reaction, the precipitate obtained from the reaction is aged, filtered, washed and dried to obtain a nickel, cobalt and manganese composite precursor;

[0072] (2) The nickel-cobalt-manganese composite precursor obtained in step (1) is heat-treated at 500°C to 550°C, and then mixed with a lithium source and a fluorine source, and then a flux is added, mixed and made into a green body;

[0073] (3) Place the green body described in step (2) in a reaction furnace at a constant temperature of 700°C to 1000°C for constant temperature calcination, and then cool, wash and dry to obtain a fluorine-doped nickel-cobalt-manganese ternary cathode material.

Embodiment 1

[0076] This embodiment provides a method for preparing a fluorine-doped nickel-cobalt-manganese ternary positive electrode material. The method includes the following steps:

[0077] (1) Take 100 mL of a mixed aqueous solution of nickel, cobalt and manganese sulfate with an ion concentration of 2.5 mol / L (the molar ratio of nickel ions, manganese ions and cobalt ions is 5:2:3), and add them to a stirring device In the reactor, argon gas was added while slowly adding 5mol / L sodium hydroxide solution and 5mol / L ammonia solution, reacting at 55℃ for 20h under an inert atmosphere, adjusting the pH to stabilize at 12, and filtering and After ultrasonic washing, Ni is obtained 0.5 Co 0.2 Mn 0.3 (OH) 2 Precursor slurry;

[0078] (2) The Ni obtained in step (1) 0.5 Co 0.2 Mn 0.3 (OH) 2 The precursor slurry is heat treated at 500℃ for 6h, and then press LiNi 0.5 Co 0.2 Mn 0.3 O 1.85 F 0.15 Weigh the lithium hydroxide and lithium fluoride (the molar ratio is 25:3) and mix them, then add 10 t...

Embodiment 2

[0083] This embodiment provides a method for preparing a fluorine-doped nickel-cobalt-manganese ternary positive electrode material. The method includes the following steps:

[0084] (1) Take 200 mL of a mixed aqueous solution of nickel, cobalt, and manganese sulfate with an ion concentration of 2mol / L (the molar ratio of nickel, manganese, and cobalt ions is 1:1:1) and add it to the reaction with a stirring device In the vessel, argon gas, while slowly adding 10mol / L sodium hydroxide solution and 5mol / L ammonia aqueous solution, react at 50℃ for 24h under inert atmosphere, adjust the pH to stabilize at 11.5, filter and ultrasonically wash , Get Ni 1 / 3 Co 1 / 3 Mn 1 / 3 (OH) 2 Precursor slurry;

[0085] (2) The Ni obtained in step (1) 1 / 3 Co 1 / 3 Mn 1 / 3 (OH) 2 The precursor slurry is heat treated at 550℃ for 7h, then press LiNi 1 / 3 Co 1 / 3 Mn 1 / 3 O 1.9 F 0.1 Weigh the lithium hydroxide and lithium fluoride (the molar ratio is 9:1) and mix them, and then add the nickel-cobalt-manganese co...

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Abstract

The invention provides a preparation method for a fluorine-doped nickel-cobalt-manganese system ternary positive electrode material. The preparation method comprises the following steps of mixing a transitional metal source water solution, an alkali liquid and ammonium hydroxide, stirring and heating to perform a reaction, and performing aging, filtering, washing and drying on sediments obtained in the reaction to obtain a nickel-cobalt-manganese composite precursor; performing heat treatment on the precursor at a temperature of 500-550 DEG C, then mixing with a lithium source and a fluorine source, then adding a fluxing agent, and mixing and preparing into a blank; and putting the blank into a reaction furnace to be subjected to constant-temperature calcining at a temperature of 700-1,000 DEG C, and then cooling, washing and drying to obtain the fluorine-doped nickel-cobalt-manganese system ternary positive electrode material. The fluorine-doped ternary positive electrode material prepared by the preparation method is uniform in average grain diameter and excellent in cycle performance; and in addition, the preparation method is simple in process, low in production cost, energy-saving and efficient, and suitable for industrial production.

Description

Technical field [0001] The invention belongs to the field of battery material preparation, and relates to a method for preparing a fluorine-doped nickel-cobalt-manganese ternary cathode material and the prepared material, in particular to a molten salt method for preparing fluorine-doped nickel-cobalt-manganese ternary The method of positive electrode material and the material obtained. Background technique [0002] In the cathode material of lithium ion batteries, the layered structure of lithium cobalt oxide (LiCoO 2 ), due to the scarcity of cobalt resources, high prices, and its toxicity to the environment, limit its development potential. Another layered structure cathode material lithium nickel oxide (LiNiO 2 ) Although the price is lower and the performance is better, the preparation is complicated and there are high-temperature safety problems. In contrast, spinel’s lithium manganate (LiMn 2 O 4 ) Due to its abundant manganese materials, low price, non-toxicity, low poll...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/505H01M4/525H01M10/0525
CPCH01M4/362H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 谭明胜邹友生吕正中刘金成
Owner HUBEI JINQUAN NEW MATERIALS CO LTD
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