Prepn process of submicron level positive pole material for lithium ion cell

A technology for lithium ion batteries and cathode materials, which is applied in the field of liquid phase synthesis, can solve the problems of large ion arrangement disorder, wide particle size distribution range, poor chemical uniformity, etc., and achieves excellent electrochemical performance, shortened synthesis cycle, and processing time. short effect

Inactive Publication Date: 2004-06-23
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

However, there are obvious shortcomings in the synthesis of this material by high-temperature solid-state reaction method: (1) the degree of mixing is limited, cobalt clusters are easy to form, and the ion arrangement is disordered; (2) higher heat treatment temperature and longer heat treatment time are required , and a large amount of lithium salt volatilizes, which consumes a lot of energy; (3) the product material has a large grain size, a wide range of particle size distribution, and poor chemical uniformity
But because the solubility in the inorganic salt organic solvent is less, need consume more organic solvent, cause the time of evaporation and drying of solvent longer, also cause the increase of cost to a certain extent, also have the nitrate that adopts serious environmental pollution, Not suitable for industrial production

Method used

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  • Prepn process of submicron level positive pole material for lithium ion cell
  • Prepn process of submicron level positive pole material for lithium ion cell
  • Prepn process of submicron level positive pole material for lithium ion cell

Examples

Experimental program
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Effect test

Embodiment 1

[0030] First weigh 0.115mol of LiOH·H 2 O was dissolved in 30ml of distilled water to form a solution, and another 0.08mol of nickel acetate and 0.02mol of cobalt acetate were dissolved in 150ml of distilled water to form a transparent deep purple solution; the two aqueous solutions were mixed and stirred to form a deep purple suspension. Then gradually add 0.1mol citric acid solution dissolved in 90ml ethanol to it, stir continuously until a clear and uniform solution is formed, heat to 80°C and stir to evaporate the solvent, concentrate for about 3 hours to form a gel, and then dry it in an oven to obtain the precursor body dry gel. Put the dry gel in a muffle furnace at 400°C for 8 hours to decompose the organic matter, take it out and grind it into a powder (brown); the powder is then sintered in a tube furnace at a rate of 3°C / min to 800°C 2 Hours later, lower the temperature to 700°C and roast for 12 hours. During the sintering process, the oxygen flow is 15ml / min. Fina...

Embodiment 2

[0032] Accurately weigh 0.115mol of LiOH·H 2 O, 0.07mol of nickel acetate and 0.03mol of cobalt acetate were dissolved in distilled water to form an aqueous solution, mixed and stirred to form a deep purple suspension, and then gradually added 0.1mol of citric acid solution dissolved in 90ml of ethanol, heated at 100 ° C , evaporate, concentrate to form a gel, and dry; decompose the organic matter in the air at 450°C, and then sinter at 800°C for 4 hours, then cool down to 720°C and continue sintering for 12 hours to obtain the positive electrode material LiNi 0.7 co 0.3 o 2 Powder is not.

[0033] The electrochemical performance test was carried out according to the method of Example 1. The test results at room temperature are as follows Figure 5 As shown, the initial reversible capacity is up to 174mAh / g, the first charge-discharge coulombic efficiency is 89%, and after 30 cycles, the reversible capacity is still 156mAh / g, indicating that the material has excellent elec...

Embodiment 3

[0035] Accurately weigh 0.108mol of Li(CH 3 COO), 0.08mol of nickel acetate and 0.02mol of cobalt acetate were dissolved in distilled water to form an aqueous solution, mixed and stirred to form a dark purple suspension, and then gradually added 0.1mol of citric acid solution dissolved in 90ml of ethanol, at 100 ° C Heating, evaporating, concentrating to form a gel, and drying; decompose the organic matter in the air at 450°C, and then sinter at 800°C for 12 hours to obtain the positive electrode material LiNi 0.8 co 0.2 o 2 Powder is not. Its electrochemical performance test at room temperature has an initial reversible capacity of up to 170.2mAh / g, and a coulombic efficiency of 87.1% for the first charge and discharge. After 30 cycles, the reversible capacity is still 146mAh / g, indicating that the material has excellent electrochemical properties.

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Abstract

The present invention relates to the liquid phase synthesis process of Ni-rich positive pole material LiNi1-yCoyO2, where y is 0.2-0.3, for lithium ion cell, and is especially one sol-gel process. With cheap citric acid as chelating agent, solution of ethanol solvent and the water solution of Li salt, Ni salt and Co salt are mixed and concentrated through heating and stirring to form gel; the gel is dried, thermally decomposed, sintered at high temperature, cooled and ground to obtain the submicron level lithium nickelate-cobalate powder. Compared with available technology, the present invention has the advantages of less organic solvent consumption, short synthesis period, simple apparatus, environment friendship, and homogeneous product with excellent electric performance.

Description

technical field [0001] The invention relates to a nickel-rich cathode material LiNi for a lithium ion battery 1-y co y o 2 (0.2≤y≤0.3) liquid-phase synthesis method, specifically the sol-gel method. Background technique [0002] Lithium nickel cobalt oxide has a similar 2 and LiNiO 2 The layered structure, whose space group is R-3m, has the advantages of both: good thermodynamic stability, good cycle performance, high capacity, cheap price, less pollution, relatively easy preparation, etc., is the most Promising alternative to commercialized LiCoO 2 One of the cathode materials. Its research is also becoming more and more mature, and it is gradually realizing commercialization. But relatively nickel-rich LiNi 1-y co y o 2 (0.2≤y≤0.3) and LiNiO 2 It is difficult to synthesize and prepare similarly. At present, a lot of research is focused on its preparation process, especially for LiNi, which has better performance and price. 0.8 co 0.2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00C01G51/00H01M4/525
CPCY02E60/12Y02E60/10
Inventor 于作龙袁荣忠瞿美臻
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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