Preparation method of submicron level LiniO.5MnO.5O2 cathode material

A cathode material, sub-micron technology, applied in battery electrodes, nickel oxide/nickel hydroxide, electrical components, etc., to achieve the effects of low production cost, easy process control, and excellent cycle stability.

Inactive Publication Date: 2010-09-15
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of submicron level LiniO.5MnO.5O2 cathode material
  • Preparation method of submicron level LiniO.5MnO.5O2 cathode material
  • Preparation method of submicron level LiniO.5MnO.5O2 cathode material

Examples

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Embodiment 1

[0020] Accurately weigh 2.8088g nickel sulfate heptahydrate (0.01mol) and 1.6901g manganese sulfate monohydrate (0.01mol), and dissolve them in a 100mL beaker successively to prepare 0.01mol / L Ni 2+ and Mn 2+ mixture. Prepare 100mL0.04mol / L NaOH solution, then add ammonia water at a molar ratio of 1:0.2 relative to NaOH, and the mixed solution of NaOH and ammonia water is used as the precipitant solution. Use a titration device to slowly drop the above metal ion mixed solution and precipitant solution into 100mL aqueous solution in which 14mg (0.14g / L) sodium lauryl sulfate is dissolved at a speed of 1.0mL / min and 1.2mL / min respectively . Before titration, sodium lauryl sulfate had been completely dissolved in the aqueous solution and kept stirring for 1 h, the stirring speed was 300 r / min, and the reaction temperature was 55°C. After the titration is complete, continue stirring at high speed for 5 h. After the precipitation was complete, the turbid solution wa...

Embodiment 2

[0025] Accurately weigh 2.8088g nickel sulfate heptahydrate (0.01mol) and 1.6901g manganese sulfate monohydrate (0.01mol), and dissolve them in a 100mL beaker successively to prepare 0.01mol / L Ni 2+ and Mn 2+ mixture. Prepare 100ml of 0.04mol / L NaOH solution, then add ammonia water at a molar ratio of 1:0.2 relative to NaOH, and a mixed solution of NaOH and ammonia water as a precipitant solution. Use a titration device to slowly drop the above metal ion mixed solution and precipitant solution into 100mL of 40mg (0.40g / L) sodium dodecylbenzenesulfonate solution at a speed of 1.0mL / min and 1.2mL / min respectively. in aqueous solution. Other steps are the same as in Example 1.

[0026] Figure 5 (a) The capacity retention diagram of the half-cell with the prepared material as the positive electrode in the first 20 cycles is recorded. It can be seen from the figure that the first discharge specific capacity of the prepared material at 0.2C rate is 158.3mAh / g, 20 cy...

Embodiment 3

[0028] Accurately weigh 2.4884g of nickel acetate tetrahydrate (0.01mol) and 2.6810g of manganese acetate dihydrate (0.01mol), and dissolve them in a 100mL beaker to prepare 0.01mol / L Ni 2+ and Mn 2+ mixture. Prepare 100ml of 0.04mol / L NaOH solution, then add ammonia water at a molar ratio of 1:0.2 relative to NaOH, and a mixed solution of NaOH and ammonia water as a precipitant solution. Use a titration device to slowly drop the above-mentioned metal ion mixed solution and precipitant solution into 100 mL of an aqueous solution in which 40 mg (0.40 g / L) of polyethylene glycol 2000 is dissolved at a speed of 1.0 mL / min and 1.2 mL / min, respectively. Other steps are the same as in Example 1.

[0029] Figure 5 (b) Recorded the capacity retention diagram of the half-battery with the prepared material as the positive electrode in the first 20 cycles. It can be seen from the figure that the first discharge specific capacity of the prepared material at 0.2C rate is 155....

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Abstract

The invention discloses a preparation method of a submicron level LiniO.5MnO.5O2 cathode material, which comprises the steps of: taking soluble nickel salt and manganese salt to prepare a nickel salt water solution and a manganese salt water solution respectively, and mixing the two solutions; preparing a sodium hydroxide solution isometric to a metal ion solution, and adding ammonia as a precipitator solution; dropwise adding the metal ion solution and the precipitator solution into a water solution of surface active agents in parallel flow, and stirring the mixed solution evenly; controlling the temperature of the precipitation reaction to be 55 DEG C, and stirring at high speed, standing, vacuum filtrating, flushing, drying and grinding after the metal ion solution and the precipitator solution are completely added to obtain the powder; adding lithium hydroxide, and carrying out ball grinding to obtain a precursor. The heat treatment for the precursor comprises the following processes of: heating the precursor at 2 to 12 DEG C /min to 350 to 450 DEG C for 2 to 6 h for pre-treatment, and then continuing to heat the precursor at the speed of 2 to 12 DEG C/min to 700 to 1000 DEG C; calcinating the precursor for 8 to 20 DEG C, cooling the precursor at the speed of 2 to 12 DEG C/min down to 300 to 500 DEG C, and annealing the precursor for 2 to 4 h. In the invention, the submicron level uniformly distributed near-spherical LiniO.5MnO.5O2 material with no obvious glomeration by introducing the surface active agent into the LiniO.5MnO.5O2 cathode material prepared by the optimized coprecipitation method. The grains of the material are distributed uniformly, and the grain diameter is about 80 to 200nm; the material is in a near-spherical shape, and has higher specific discharge capacity and good cycling stability.

Description

technical field [0001] The invention relates to the field of high-energy battery materials, in particular to the preparation of positive electrode materials for lithium ion batteries. Background technique [0002] Lithium-ion batteries have the advantages of small size, light weight, large specific capacity, long cycle life, small self-discharge, and no memory effect. At present, it has been widely used in portable mobile tools, digital products, artificial satellites, aerospace and other fields, and has very broad prospects in the fields of electric bicycles and automobiles. At present, the mainstream cathode material on the market is layered lithium cobalt oxide. However, due to the high toxicity of Co, severe scarcity of resources, high price, low actual specific capacity, and unsatisfactory thermal stability, researchers have been prompted to develop other high-capacity cathodes. material to replace lithium cobalt oxide. Both layered lithium nickel oxide and lithium ma...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/1391C01G53/04C01G45/02C01D15/02
CPCY02E60/122Y02E60/10
Inventor 黄可龙王海燕刘素琴
Owner CENT SOUTH UNIV
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