Liquid-phase synthesis of anode material for lithium ion secondary battery

A cathode material and a technology for secondary batteries, which are applied in the field of preparing cathode materials for lithium ion batteries, can solve the problems of uneven composition of synthetic materials, time-consuming, high calcination temperature, and achieve good industrial application prospects, shorten sintering time, and high charge-discharge capacity. Effect

Inactive Publication Date: 2005-12-28
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

[0004] In the prior art, the synthesis of positive electrode materials mostly adopts the solid-state reaction method, that is, the oxide or carbonate of lithium and cobalt or manganese is used for long-term calcination at a high temperature of 800-900 ° C. The advantage of this method is that the process is simple , but there are also obvious disadvantages: the composition of the synthetic material is uneven, the particles are large and the distribution range is wide, the calcination temperature is high and the time is long. Generally speaking, the positive electrode material must have a good crystal structure, uniform composition, submicron size particles diameter, narrow particle size distribution, large specific surface, etc. to obtain high electrochemical performance, it is obvious that the solid-phase method is difficult to meet these conditions; Chinese patent application 99113860.0 uses polyvinyl alcohol or polyethylene glycol aqueous solution as a solvent, after heating , Concentrate to form a gel, and obtain the required powder after calcination. This method has the advantages of high product purity and uniform chemical composition, but it needs a long time of heating and stirring the concentrated solution, which is time-consuming and consumes a lot of energy; Chinese patent application 02123112.5 A citrate gel method is proposed to prepare lithium battery cathode materials. This method has the advantages of low synthesis temperature and uniform particle size, but it is necessary to strictly control the pH value of the solution during the preparation process. If the control is not good, it will Form precipitation, and can not obtain gel; It is similar with it, proposes to utilize nano-reactor to prepare the new technology of nanometer lithium cobalt oxide in the Chinese patent application 0112937.6, but also there is need to adjust the problem of pH value and reaction slower, so in practice The process of application is subject to certain restrictions; Chinese patent application 97112128.1 also proposes a preparation scheme utilizing hydrothermal method. The preparation process of this scheme is simple, but the reaction needs 5 days. Obviously, the reaction time is too long, and there are also production problems. Disadvantages of low rate

Method used

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  • Liquid-phase synthesis of anode material for lithium ion secondary battery
  • Liquid-phase synthesis of anode material for lithium ion secondary battery
  • Liquid-phase synthesis of anode material for lithium ion secondary battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 2.8969g of LiNO respectively 3 and 11.6412g of Co(NO 3 ) 2 ·6H 2 O (that is, the molar ratio of Li:Co is 1.05:1), was stirred and dissolved in 10mL of water, and then 10mL of acrylic acid was added. According to the dose rate of 55Gy / min, the irradiation time is 90min), the purple polymer gel is finally obtained, the gel is dried at 100℃~150℃, then slowly heated to 450℃, thermally decomposed for 2 hours, and removed Organic matter in the gel, forming LiCoO 2 Powder precursor. Then the LiCoO was sintered under air atmosphere 2 powder precursor, the sintering temperature is 800°C, and the sintering time is 10 hours, and finally LiCoO 2 powder.

[0021] LiCoO prepared with Example 1 2 The powder is used as a half-battery on a lithium sheet, and the electrolyte used is 1mol / L LiPF 6 / (EC+DEC) (where EC is ethylene carbonate, DEC is diethyl carbonate, the volume ratio of the two is 1:1), the test voltage range is 2.7V ~ 4.2V, and the current density is 0.67mA / cm...

Embodiment 2

[0023] Take 1.8099g of LiNO respectively 3 and 7.2758g of Co(NO 3 ) 2 ·6H 2 O (that is, the molar ratio of Li:Co is 1.05:1), stirred and dissolved in 50mL of water, then added 50mL of acrylic acid, after mixing evenly, used Co-60 as a radiation source to carry out radiation polymerization, and the radiation dose was 8000Gy ( According to the dose rate of 80Gy / min and the irradiation time of 100min), the polymer gel was obtained, and the gel was dried at 100°C to 150°C, and then slowly heated to 450°C to decompose the organic matter in the gel to form LiCoO 2 Powder precursor. Then the LiCoO was sintered under air atmosphere 2 Powder precursor, the sintering temperature is 800°C, and the sintering time is 10 hours.

Embodiment 3

[0025] Take 1.8099g of LiNO respectively 3 and 7.2758g of Co(NO 3 ) 2 ·6H 2 O (that is, the molar ratio of Li:Co is 1.05:1), stirred and dissolved in 12.5mL of water, then added 12.5mL of acrylic acid, after mixing evenly, used Co-60 as the radiation source to carry out radiation polymerization, and the radiation dose was 2000Gy (The irradiation dose rate is 50Gy / min, and the irradiation time is 40min). Finally, the polymer gel is dried at 100°C to 150°C, and then slowly heated to 450°C to decompose the organic matter in the gel. , forming LiCoO 2 Powder precursor. Then the LiCoO was sintered under air atmosphere 2 Powder precursor, sintered at 800°C for 10 hours to obtain LiCoO 2 powder.

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Abstract

The method includes following steps: 1) prepares mixing aqueous solution containing cobalt or manganic compounds, lithium compounds and polymer monomer; the mole number ratio of lithium to cobalt is (0.9-1.1):1; the mole number ratio of lithium to manganese is (1~1.1): 2; the volumetric ratio of water to polymer monomer in mixing aqueous solution is (0.2-5): 1; the structure formula of polymer monomer is alkene compound; 2) the mixing aqueous solution is put into the condition under the Y-ray irradiation; Y-ray is used to lead polymerization of polymer monomer in solution and to get macromolecule gel; 3) the gel is processed through drying, thermal decomposition and sintering to form the anode material.

Description

technical field [0001] The invention relates to a lithium ion battery preparation technology, in particular to a method for preparing a lithium ion battery cathode material. Background technique [0002] Lithium-ion batteries were developed and commercialized by Japan's SONY company in 1990. Its appearance can be regarded as a leap in the history of secondary batteries. With the rapid development of the information industry, the consumer market for portable communication devices and laptop computers is getting bigger and bigger. Lithium-ion batteries are a new generation of power sources. Compared with other batteries, lithium-ion batteries have the advantage of high open circuit voltage (commercially available batteries) Most of them are 3.6V, while the open circuit voltage of nickel-hydrogen and nickel-cadmium secondary batteries is 1.2V), large specific capacity (2.5 times that of nickel-cadmium secondary batteries, 1.5 times that of nickel-hydrogen secondary batteries), ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04
CPCY02E60/10
Inventor 丁宁陈春华
Owner UNIV OF SCI & TECH OF CHINA
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