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Preparation method of lithium-rich manganese-based positive electrode material precursor

A positive electrode material, lithium-rich manganese-based technology, applied in chemical instruments and methods, battery electrodes, inorganic chemistry, etc., can solve the problems of precursor difficulties, cation mixing, and capacity retention rate reduction, so as to reduce Li/Ni mixing Discharge, reduce irreversible phase transition, reduce the effect of development cost

Active Publication Date: 2021-01-01
JINGMEN GEM NEW MATERIAL
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Problems solved by technology

[0004] Lithium-rich manganese-based cathode materials have attracted much attention due to their high specific capacity and high safety, but due to the presence of Li 2 MnO 3 and LiTMO 2 (TM=Ni, Co, Mn) (NCM) two materials, which belong to a composite material, are prone to cation mixing during the electrochemical cycle, resulting in a phase change, some of which are reversible and some are irreversible , so "voltage decay" is prone to occur during cycling, and the capacity retention rate decreases. These defects have seriously hindered the wide application of lithium-rich manganese-based cathode materials in vehicle power batteries.
The complex structure of lithium-rich manganese-based materials is a big challenge to improve the electrochemical performance of lithium-rich manganese-based materials.
In the preparation process of lithium-rich manganese-based precursors, due to the high content of Mn, oxidation easily occurs during the reaction process, which affects the morphology and growth rate of the precursors. At the same time, the particle size of the high-manganese precursors is not easy to grow, making It is difficult to prepare precursors with large particle sizes

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  • Preparation method of lithium-rich manganese-based positive electrode material precursor

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preparation example Construction

[0027] A method for preparing a lithium-rich manganese-based cathode material precursor, the steps comprising:

[0028] (1) Nickel sulfate, manganese sulfate are x according to the molar ratio 1 :1-x 1 Mix and prepare a mixed salt solution A with a metal ion concentration of 2.5-4.5mol / L, where 0.10≤x 1 ≤0.20; the molar ratio of manganese sulfate, nickel sulfate and cobalt sulfate is x 2 :y 2 :z 2 Configure mixed salt solution B with a metal ion concentration of 2.5-4.5mol / L, where 0.10≤x 2 ≤0.20, 0.20≤y 2 ≤0.30, 0.50≤z 2 ≤0.70,x 2 +y 2 +z 2 = 1;

[0029] (2) Pass inert gas 1h-5h into the reaction kettle containing the bottom liquid earlier as protective gas to prevent the oxidation of Mn in the reaction process, when the pH of the bottom liquid is 9.0-10.5 and the ammonia concentration is 8-10g / L, Add mixed salt solution A, ammonia water with a concentration of 7-14g / L and 3mol / L alkaline solution into the reaction kettle and stir, control the pH of the reaction sy...

Embodiment 1

[0035] Step 1, nickel sulfate and manganese sulfate are configured as nickel-manganese metal mixed salt solution A of 15:85 by metal molar ratio, and manganese sulfate, nickel sulfate and cobalt sulfate are configured as 10:20:70 by molar ratio of nickel, cobalt and manganese to mix Salt solution B, the concentration of metal ions is 2.5mol / L, add 500L of pure water, 1kg of sodium carbonate and 40kg of ammonia as the bottom liquid in a 1 cubic reaction kettle, the pH is 9.5, and the ammonia concentration is 8g / L, 3 hours before the reaction, 1m 3 The inert protective gas of / h, then stably add nickel-manganese metal mixed salt solution A in the reactor with the flow rate of 30kg / h with metering pump, add the ammoniacal liquor that concentration is 12g / L and 3mol / L in reactor simultaneously Sodium carbonate solution, the flow rate is 5kg / h and 10kg / h respectively, by controlling the flow rate of ammonia water and sodium carbonate solution during the reaction, the pH of the adju...

Embodiment 2

[0040] Step 1, nickel sulfate and manganese sulfate are configured nickel-manganese mixed salt solution A of 20:80 by metal molar ratio, and manganese sulfate, nickel sulfate and cobalt sulfate are configured mixed salt solution B according to molar ratio of 20:20:60, The concentration of metal ions is 3.0mol / L. Add 300L of pure water, 3kg of sodium hydroxide and 50kg of ammonia water into a 1 cubic reaction kettle as the bottom liquid. The pH is 10.0 and the ammonia concentration is 9g / L. Medium access 5h 1m 3 / h of inert gas to prevent the oxidation of Mn in the reaction process, then use a metering pump to stably add nickel-manganese metal mixed salt solution A to the reactor at a flow rate of 40kg / h, and add a concentration of 14g / L to the reactor at the same time ammonia water and 3mol / L sodium hydroxide solution, the flow rates are 7kg / h and 15kg / h respectively, during the reaction process, the pH of the system is adjusted by controlling the flow rate of ammonia water an...

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Abstract

The invention discloses a preparation method of a lithium-rich manganese-based positive electrode material precursor. The preparation method comprises the following steps: preparing a mixed salt solution A of nickel and manganese and a mixed salt solution B of nickel, cobalt and manganese, introducing inert gas into a reaction kettle containing a base solution, respectively adding the mixed salt solution A, ammonia water and an alkaline solution into the reaction kettle, stirring, adding the mixed salt solution B, ammonia water and the alkaline solution, and controlling the pH, the ammonia-alkali concentration, the reaction temperature, the reaction time, the stirring speed and the like in the reaction process to obtain the precursor with the particle size of 13-18 [mu]m. According to theinvention, the problems of voltage attenuation and poor cycle performance of the lithium-rich manganese-based material are solved, and the rate capability of the material can be improved through uniform pores.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a preparation method of a lithium-rich manganese-based cathode material precursor. Background technique [0002] Lithium-rich manganese-based cathode materials have attracted the attention of scientists in the industry due to their advantages such as ultra-high specific capacity (>250mAh g-1) and low cost. This cathode material can be regarded as a special kind of nickel-cobalt-manganese Lithium acid ternary material, the general formula can be expressed as Li1+xM1-xO2 (M=Ni, Co, Mn). Although the lithium-rich manganese-based cathode materials have great potential, the instability of the crystal structure of the lithium-rich manganese-based cathode materials will cause the material to transform from a layered phase to a spinel phase structure during cycling, resulting in the electrochemical degradation of the material. Severe voltage attenuation occurs during cycling, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/36H01M4/505H01M4/52
CPCC01G53/006C01G53/44C01G53/50H01M4/366H01M4/505H01M4/523C01P2006/40C01P2004/61C01P2004/03Y02E60/10
Inventor 薛晓斐张坤许开华李聪陈康黎俊孙海波范亮姣
Owner JINGMEN GEM NEW MATERIAL