Improved method for preparing layered enriched lithium-manganese-nickel oxide by low-heat solid-phase reaction

A nickel oxide, low thermal solid phase technology, applied in manganese oxide/manganese hydroxide, electrical components, battery electrodes, etc., can solve the problem that the microscopic morphology and particle size distribution cannot be effectively controlled, and achieve accelerated reaction - nucleation ―Growth process, simplify the operation process, overcome the effect of severe oxidation

Active Publication Date: 2011-10-19
湖南金富力新能源股份有限公司
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  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a method for preparing layered lithium-rich manganese-nickel oxide material by improving low-heat solid-state reaction, the preparation process is simplified, and the process is improved according to the characteristics of the initial slurry prepared by low-heat solid-state reaction, Solve the problem that the microscopic appearance and particle size distribution of materials cannot be effectively controlled, and synthesize materials with typical layered structure characteristics whose particle size meets the requirements of engineering indicators

Method used

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  • Improved method for preparing layered enriched lithium-manganese-nickel oxide by low-heat solid-phase reaction
  • Improved method for preparing layered enriched lithium-manganese-nickel oxide by low-heat solid-phase reaction
  • Improved method for preparing layered enriched lithium-manganese-nickel oxide by low-heat solid-phase reaction

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Embodiment 1

[0025] 1) Lithium hydroxide monohydrate LiOH·H 2 O, dihydrate oxalic acid C 2 h 2 o 4 2H 2 O, nickel acetate and manganese acetate were added to the ball mill at the same time, in which LiOH·H 2 O:C 2 h 2 o 4 2H 2 The molar ratio of O is 1:1, the molar ratio of lithium hydroxide monohydrate to manganese acetate and nickel acetate is 1.2:0.6:0.2, and the ball mill is mixed for 1 hour;

[0026] 2) Add deionized water to the obtained slurry, adjust the concentration to 280g / l, carry out spray drying, and control the temperature of fluid heating at 120°C to obtain dry powder;

[0027] 3) The powder is roasted at 450°C for 3 hours, ball milled and put into a corundum saggar, and then heated to 600°C and roasted for 12 hours. Lithium manganese nickel oxide Li 1.2 mn 0.6 Ni 0.2 o 2 (Li 1+x mn y Ni 1-x-y o 2， where x=0.2, y=0.6).

Embodiment 2

[0029] 1) Lithium hydroxide monohydrate LiOH·H 2 O, dihydrate oxalic acid C 2 h 2 o 4 2H 2 O, nickel acetate and manganese acetate were added to the ball mill at the same time, in which LiOH·H 2 O:C 2 h 2 o 4 2H 2 The molar ratio of O is 1:1.2, the molar ratio of lithium hydroxide monohydrate to manganese acetate and nickel acetate is 1.3:0.01:0.69, and the ball mill is mixed for 0.8h;

[0030] 2) Add deionized water to the obtained slurry, adjust the concentration to 250g / l, carry out spray drying, and control the temperature of fluid heating at 115°C to obtain dry powder;

[0031] 3) The powder is roasted at 500°C for 6 hours, ball milled, put into a corundum sagger, and then heated to 750°C for 15 hours after pressing. It has high fluidity and a layered lithium-rich particle size composition controlled at 4-12 μm. Manganese Nickel Oxide Li 1.3 mn 0.01 Ni 0.69 o 2 (Li 1+x mn y Ni 1-x-y o 2， where x=0.3, y=0.01).

Embodiment 3

[0033] 1) Lithium hydroxide monohydrate LiOH·H 2 O, dihydrate oxalic acid C 2 h 2 o 4 2H 2 O, nickel acetate and manganese acetate were added to the ball mill at the same time, in which LiOH·H 2 O:C 2 h 2 o 4 2H 2 The molar ratio of O is 1:1.15, the molar ratio of lithium hydroxide monohydrate to manganese acetate and nickel acetate is 1.11:0.56:0.33, and the ball mill is mixed for 2 hours;

[0034] 2) Add deionized water to the obtained slurry, adjust the concentration to 220g / l, carry out spray drying, and control the temperature of fluid heating within the range of 110°C to obtain dry powder;

[0035] 3) The powder is calcined at 480°C for 4 hours, ball-milled, put into a corundum sagger, and then heated to 850°C for 13 hours after pressing. It has high fluidity and a layered lithium-rich particle size composition controlled at 3-10 μm. Manganese Nickel Oxide Li 1.11 mn 0.56 Ni 0.33 o 2 (Li 1+x mn y Ni 1-x-y o 2， where x=0.11, y=0.56).

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Abstract

The invention provides an improved method for preparing layered enriched lithium-manganese-nickel oxide by low-heat solid-phase reaction. The method comprises the following steps: weighing lithium hydroxide monohydrate, nickel acetate and manganese acetate, and oxalic acid dihydrate according to the stoichiometry as follows: Li1+xMnyNi1-x-yO2, x being more than 0 and less than or equal to 1 / 3, y being more than 0 and less than 1, and x+y being more than 0 and less than 1 (wherein the mole ratio of LiOH.H2O to C2H2O4.2H2O is 1:1-1.2), and adding into a ball milling tank together for balling milling for 0.5-2h; obtaining slurry, adding deionized water in the slurry to adjust concentration, spraying and drying the slurry, and roasting the dried powder to obtain the final product -Li1+xMnyNil-x-yO2. The improved method has the following advantages: the process flow is short, the component of the material can be accurately controlled, the problems of material loss and inaccurate stoichiometry caused by repeatedly washing the product in a liquid phase method are overcome, the generation of a large quantity of waste water is avoided; simultaneously, the shape and particle size of a synthesized material can be controlled, the engineering index requirement can be achieved, the impurity pollution caused by dependence of a synthetic material by a solid phase method on crushing process can be overcome, the enriched lithium-manganese-nickel oxide has typical layered structure property, the particle size is 3-12mum, the specific capacity is high, and the cyclic performance is stable.

Description

technical field [0001] The invention belongs to the technical field of preparation of cathode materials for lithium ion batteries, and in particular relates to an improved method for preparing a layered lithium-rich manganese nickel oxide material by an improved low-heat solid-state reaction. Background technique [0002] Lithium-ion batteries have outstanding advantages such as high working voltage, high energy density, high specific capacity, wide working temperature range, small self-discharge, long cycle life, no memory effect, fast charging and discharging, and no environmental pollution. Ideal power supplies for small and lightweight electronic devices such as telephones, notebook computers, and portable testers. At the same time, lithium-ion batteries will also become an ideal light-duty high-energy power source for electric vehicles and a safe and efficient energy storage power source. The promotion and application of lithium-ion batteries, especially large-scale li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02H01M4/1391
CPCY02E60/10
Inventor 连芳李栋仇卫华李福燊周国治
Owner 湖南金富力新能源股份有限公司
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