Preparation method of cathode material for lithium ion battery based on transition metal carbonate precursor

A lithium-ion battery and transition metal technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of complex process, commercial production of unfavorable materials, long reaction time, etc., and achieve narrow particle size distribution, high rate charge and discharge The effect of excellent performance and short reaction time

Active Publication Date: 2011-12-28
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

Although the electrochemical properties of materials prepared by co-precipitation method are relatively excellent, due to the complex process, the need to precisely con

Method used

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  • Preparation method of cathode material for lithium ion battery based on transition metal carbonate precursor
  • Preparation method of cathode material for lithium ion battery based on transition metal carbonate precursor
  • Preparation method of cathode material for lithium ion battery based on transition metal carbonate precursor

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Embodiment 1

[0026] Mix nickel nitrate, manganese nitrate, and urea according to the molar ratio of 1:3:10 to form a 250ml mixed solution. The concentration of nickel ions in the mixed solution is 1M. After thermal reaction for 12 hours, the precipitate was collected, washed and dried in vacuum to obtain the Ni0.25Mn0.75CO3 precursor. The resulting Ni 0.25 mn 0.75 CO 3 The precursor and lithium hydroxide were mixed at a molar ratio of 2:1, and then dry ball milled at 500 rpm with a ball-to-material ratio of 10:1 for 5 hours to obtain a powder.

[0027] The obtained powder is placed in a microwave air atmosphere furnace and sintered at a constant temperature of 550°C for 0.1h, then sintered at a constant temperature of 850°C for 0.5h, annealed at 600°C for 0.5h, and naturally cooled to room temperature to obtain a spinel transition Metal oxide material LiNi 0.5 mn 1.5 o 4 .

[0028] LiNi 0.5 mn 1.5 o 4 The X-ray diffraction pattern of figure 1 As shown, the scanning electron micr...

Embodiment 2

[0031] Nickel sulfate, manganese sulfate, and hexamethylenetetramine were mixed according to a molar ratio of 1:3:8 to form a 150ml solution. The concentration of nickel ions in the mixed solution was 1M, and the resulting solution was placed in a 50ml reactor at 180 Under the condition of ℃ hydrothermal reaction for 12h, the collected precipitate was washed and dried by rotary evaporation to obtain Ni 0.25 mn 0.75 CO 3 Precursor.

[0032] The resulting Ni 0.25 mn 0.75 CO 3The precursor and lithium carbonate were subjected to wet ball milling at a molar ratio of 1:1, the wet ball milling speed was 500 rpm, the ball milling time was 10 h, and the ball-to-material ratio was 10:1. Then the obtained powder was placed in a conventional resistance heating furnace for sintering at a constant temperature of 550°C for 2h, then sintered at a constant temperature of 850°C for 18h, annealed at 500°C for 8h, and naturally cooled to room temperature to obtain a spinel-type transition m...

Embodiment 3

[0034] Mix nickel sulfate, manganese sulfate, hexamethylene tetramonium, and sodium dodecylbenzenesulfonate in a molar ratio of 1:3:8:2 to form a 50ml solution. The concentration of nickel ions in the mixed solution is 2M , put the obtained solution in a 50ml reaction kettle for hydrothermal reaction at 180°C for 24 hours, collect the precipitate, wash and dry it in vacuum to prepare Ni 0.25 mn 0.75 CO 3 Precursor.

[0035] The resulting Ni 0.25 mn 0.75 CO 3 The precursor and lithium carbonate were mixed according to the stoichiometric ratio to form a 1M solution, and the resulting solution was dried with a high-speed centrifugal drying sprayer to obtain a mixed powder, and the feeding solution speed was 10ml / min; the gas flow rate of the nozzle was controlled by the pressure of compressed air. The pressure is controlled at 0.4MPa; the air inlet temperature is 200°C, and the outlet temperature is 80°C. The obtained powder was placed in a microwave air atmosphere furnace ...

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Abstract

The invention relates to a preparation method for lithium ion battery positive electrode materials based on transition metal carbonate precursors, which is characterized by comprising the following steps that: (1) transition metal element compounds, precipitation agents and additives are sufficiently mixed and prepared into mixed solution with the transition metal ion concentration being 0.01 M to 10M, the mixed solution is placed into a reaction kettle to carry out hydrothermal reaction at 80 to 200 DEG C for 2h to 48h, then, precipitates are washed and dried, and the transition metal carbonate precursors are obtained; and (2) the prepared transition metal carbonate precursors and lithium compounds conforming to the chemical measurement proportion are sufficiently mixed and are then placed into an air atmosphere furnace for carrying out heat treatment, and the required lithium ion battery positive electrode materials based on the transition metal carbonate precursors are obtained. Compared with the prior art, the preparation method has the advantages that the metal ions of the obtained materials are sufficiently mixed, the forms and the appearances are uniform, the grain diameter distribution is narrow, the tap density is high, the charging and discharging voltage platform is higher, the rate charging and discharging performance is excellent, and the circulation performance is stable. Simultaneously, the method is simple, the implementation is easy, the control parameters are fewer, the reaction time is short, and the cost is low.

Description

technical field [0001] The invention relates to the field of preparation of lithium-ion secondary battery materials, in particular to a preparation method of a lithium-ion battery anode material based on a transition metal carbonate precursor. Background technique [0002] Since they were first commercially produced in the 1990s, lithium-ion secondary batteries have been widely used in personal electronic devices such as mobile phones, laptop computers, and music players. Due to the high energy density and excellent charge-discharge performance of lithium-ion secondary batteries, people are trying to use lithium-ion secondary batteries (instead of conventional energy sources) as power sources for large mechanical equipment such as electric vehicles, thereby solving the problem of twenty-one Issues such as energy depletion that may be faced in the development of human society in the next century. In the field of lithium-ion secondary battery technology, the research and deve...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 刘兆平张明浩夏永高袁国霞
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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