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Preparation method of nickel-manganese spinel high-voltage positive material of lithium secondary battery

A lithium secondary battery and positive electrode material technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of unbalanced element loss, difficult control of product stoichiometric ratio, uncertainty, etc.

Inactive Publication Date: 2015-03-25
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of the loss of dissolution during the washing process, the uneven loss of elements caused by pH changes during the washing process will still bring difficulties to the control of the composition of the material
In addition, even if an inert gas is introduced into the system during the precipitation process, it is difficult to avoid a small amount of ions being oxidized to a high valence state, which also brings uncertainty to the calculation of the amount of Li source added based on the precursor weight method, resulting in product chemistry. Measuring ratio is difficult to control

Method used

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  • Preparation method of nickel-manganese spinel high-voltage positive material of lithium secondary battery
  • Preparation method of nickel-manganese spinel high-voltage positive material of lithium secondary battery
  • Preparation method of nickel-manganese spinel high-voltage positive material of lithium secondary battery

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Effect test

Embodiment 1

[0035] Add 0.02mol of lithium acetate, 0.01mol of nickel acetate, and 0.03mol of manganese acetate into deionized water, dissolve, stir and mix uniformly to obtain mixed solution A; weigh 0.08mol of organic precipitant 8-hydroxyquinoline, and dissolve at 60°C In ethanol, solution B was obtained. Under continuous magnetic stirring, solution A was slowly added dropwise to solution B, and stirring was continued for 2 hours after the addition was completed, during which precipitation was continuously formed. The precipitated dispersion was evaporated in a water bath at 80°C to remove the solvent, and then dried in a blast oven at 110°C for 10 hours to obtain a precipitate. The obtained precipitate was pre-calcined at 300° C. for 2 h to obtain a precursor. After the precursor was ground, it was pressed into pellets under a pressure of 10 MPa. In an air atmosphere, the temperature was raised to 800 °C at a rate of 10 °C / min and kept for 10 h, and then cooled to room temperature at ...

Embodiment 2

[0037] Add 0.03mol lithium oxalate, 0.015mol nickel oxalate, and 0.045mol manganese oxalate into deionized water respectively, dissolve, stir and mix uniformly to obtain a mixed solution A; weigh 0.10mol organic precipitant dinitroaniline, and dissolve it in In cyclohexane, solution B was obtained. Under continuous magnetic stirring, solution B was slowly added dropwise to solution A, and stirring was continued for 3 hours after the addition was completed, during which precipitation was continuously formed. The precipitated dispersion was evaporated in a water bath at 80°C to remove the solvent, and then dried under vacuum at 120°C overnight to obtain a precipitate. The obtained precipitate was pre-calcined at 400° C. for 5 h to obtain a precursor. After the precursor was ground, it was pressed into pellets under a pressure of 8 MPa. Under an oxygen atmosphere, the temperature was raised to 750 °C at a rate of 5 °C / min and kept for 20 h, and then cooled to room temperature at...

Embodiment 3

[0039] Add 0.02mol of lithium hydroxide, 0.01mol of nickel chloride, and 0.03mol of manganese chloride into deionized water respectively, dissolve, stir and mix uniformly to obtain a mixed solution A; weigh 0.06mol of organic precipitant dimethylglyoxime, and place Dissolve in isopropanol to obtain solution B. Under continuous magnetic stirring, slowly add solution A and solution B into the beaker drop by drop at the same time. During this process, precipitates are continuously formed, and stirring is continued for 5 hours after the dropwise addition is completed. The precipitate dispersion system was evaporated in a water bath at 70°C to remove the solvent, and then dried in a blast drying oven at 120°C for 12 hours to obtain a precipitate. The obtained precipitate was pre-calcined at 470° C. for 3 h to obtain a precursor. After the precursor is ground, it is pressed into pellets under a pressure of 12MPa, and the temperature is raised to 850°C at a rate of 15°C / min under a ...

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Abstract

The invention discloses an organic coprecipitation preparation method of a nickel-manganese spinel high-voltage positive material LiNi0.5Mn1.5O4 of a lithium secondary battery. The organic coprecipitation preparation method is characterized by comprising the following steps: weighing a lithium source, a nickel source and a manganese source according to a stoichiometric ratio, dissolving the sources into deionized water to obtain a solution A, dissolving an organic precipitating agent to obtain a solution B, and mixing the solution A and the solution B to generate a precipitation; and then directly evaporating to remove a solvent without carrying out filtering and precipitation washing to obtain a precursor, and then carrying out heat treatment to obtain the target product LiNi0.5Mn1.5O4. According to the organic coprecipitation preparation method, Ni<2+> and Mn<2+> ions are compounded with the organic precipitating agent through coordination bonds in the forming process of the precipitation, so that the very high ionic selectivity is achieved; in addition, the precipitating agent can be removed by being decomposed in a sintering process, so that the precipitation is unnecessary to wash, not only is a preparation process simplified, but also the stoichiometric ratio of a product can be well controlled, and the process control and the product purity and property have the very good repeatability.

Description

technical field [0001] The invention relates to nickel-manganese spinel LiNi, a high-voltage cathode material for a lithium secondary battery 0.5 mn 1.5 o 4 The preparation method relates to a method for preparing a high-purity nickel-manganese spinel lithium secondary battery cathode material by an organic co-precipitation method, and belongs to the technical field of lithium secondary battery materials. Background technique [0002] Due to its high voltage, high energy density, long cycle life, no memory effect, small self-discharge and environmental friendliness, lithium secondary batteries have become one of the battery systems with the best comprehensive performance. They are widely used in optoelectronics, information, Transportation, national defense and aerospace, and many other fields, and is becoming the protagonist of energy storage batteries and automotive power batteries. If lithium secondary batteries want to develop faster and better in this new energy deve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/505H01M4/525
CPCH01M4/505H01M4/525Y02E60/10
Inventor 冯季军王雪华郭琳昱李水华刘永
Owner UNIV OF JINAN
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