Method for preparing ternary complex anode material (LiNixCoyMn1-x-yO2)

A positive electrode material and ternary composite technology, applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of uniform mixing of difficult elements, limited mechanical mixing uniformity, agglomeration and excessive particle growth, etc., to achieve the suppression of particle agglomeration and Effects of overgrowth, excellent electrochemical performance, and increased particle surface area

Inactive Publication Date: 2012-03-21
CENT SOUTH UNIV
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  • Claims
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Problems solved by technology

Due to the limited uniformity of mechanical mixing, the high-temperature solid-phase method is not easy to mix the elements uniformly, and it is difficult to form a solid solution with uniform properties during the sintering process, and the material particle size is large and the distribution is uneven.
Yang-Kook Sun et al. used the hydroxide coprecipitation method to LiNi 1-x-y co x mn y o 2 A lot of research has been done on the preparation and modification of multi-metal oxides. Although the composition of the synthesized materials is uniform, it is difficult to prepare LiNi with fine particles. 1-x-y co x mn y o 2 multi-metal oxides
In the sintering process, the problems of material agglomeration and excessive particle growth have not been effectively solved so far.

Method used

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  • Method for preparing ternary complex anode material (LiNixCoyMn1-x-yO2)
  • Method for preparing ternary complex anode material (LiNixCoyMn1-x-yO2)
  • Method for preparing ternary complex anode material (LiNixCoyMn1-x-yO2)

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Experimental program
Comparison scheme
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Embodiment 1

[0020] NiCl 2 ·6H 2 O, CoCl 2 ·6H 2 O, MnCl 2 4H 2 O is the raw material, and the molar ratio of Ni, Co, and Mn is 9:0.5:0.5. Add deionized water to make a solution with a total metal ion concentration of 2mol / L. Add ammonia water and NaOH solution to adjust the pH value to 12.5. Stir at constant temperature 1min, get the hydroxide precipitate, filter, wash, utilize 10% polyvinylpyrrolidone and tetraethyl orthosilicate (15% by Si amount), stir, filter, the gained precipitate is dried in 110 ℃ of forced air ovens, and then The obtained powder was added with LiOH·H according to the stoichiometric ratio 2 O (excess 5%), calcined at 950°C for 2h in an air atmosphere, and the obtained product was removed with a sodium hydroxide solution in an ultrasonic oscillator to obtain a nanoscale, high specific surface area composite cathode material LiNi 0.9 co 0.05 mn 0.05 o 2 , its first discharge specific capacity is as high as 210.3mAh / g.

Embodiment 2

[0022] Use nickel acetate, cobalt acetate, and manganese acetate as raw materials, mix according to the molar ratio of Ni, Co, and Mn as 1:1:8, add deionized water to make a solution with a total metal ion concentration of 0.5mol / L, and keep the temperature at 50°C Add ammonia water and NaOH mixed solution (NH 3 ·H 2 O, NaOH molar ratio 1: 1), adjust the pH to be 9, stir at constant temperature for 24h, obtain hydroxide precipitate, filter, wash, utilize 0.2% polyvinylpyrrolidone and dimethyl dichlorosilane (0.5% by Si amount) ), stirred, filtered, and the obtained precipitate was dried in a blast drying oven at 110°C, then the obtained powder was added with lithium acetate according to the stoichiometric ratio, and calcined at 450°C for 24 hours in an oxygen atmosphere, and the obtained product was treated with sodium hydroxide solution in ultrasonic Removing the surface Si in the oscillator, that is, nano-scale, high specific surface area composite cathode material LiNi 0....

Embodiment 3

[0024] Using nickel nitrate, cobalt nitrate, and manganese nitrate as raw materials, the molar ratio of Ni, Co, and Mn is 6:2:2, and deionized water is added to make a solution with a total metal ion concentration of 1mol / L. Ammonia, add NaOH solution, adjust the pH value to 10, stir at constant temperature for 1h, obtain hydroxide precipitate, filter, wash, utilize 5% pvp and methyl trichlorosilane (5% by Si amount), stir, filter, The obtained precipitate was dried in a blast drying oven at 110°C, and then the obtained powder was added with lithium carbonate (2% excess) according to the stoichiometric ratio, calcined at 750°C for 12 hours in an oxygen atmosphere, and the obtained product was vibrated with sodium hydroxide solution in ultrasonic Remove the surface Si in the device, and then get the quasi-nanoscale composite cathode material LiNi 0.6 co 0.2 mn 0.2 o 2 . Its primary particle size can reach 160-180nm, and its initial discharge specific capacity can reach 194....

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Abstract

The invention discloses a method for preparing a ternary complex anode material (LiNixCoyMn1-x-yO2), which is characterized in that the lithium ion battery anode material (LiNixCoyMn1-x-yO2) is prepared by adopting a coprecipitation-silicon cladding-high temperature sintering-desilicication integrated method, and specifically comprises the following steps: mixing a nickel source and a cobalt source with a manganese source according to molar ratio of nickel-cobalt-manganese: x:y:(1-x-y), adding with water, stirring to form a solution, adding with a certain amount of ammonia water and a sodium hydroxide solution to generate a uniform NixCoyMn1-x-y(OH)2 ocyhydrate precursor, washing and filtering the precursor, adding with a certain amount of polyvinylpyrrolidone, stirring for a certain period, adding with a certain quantity of organosilicon reagents, stirring continuously to obtain an ocyhydrate precursor wrapped by organosilicon reagent-polyvinylpyrrolidone, washing, filtering, drying and then mixing the ocyhydrate precursor with a lithium source, calcining the mixture under air or an oxygen atmosphere under the temperature of 450-950 DEG C for 2-48 hours, and removing a silicon wrapping layer on a product by the utilizing a sodium hydroxide solution, thus obtaining the nanoscale or standard nanoscale lithium ion battery ternary complex anode material (LiNixCoyMn1-x-yO2). The particle size of the anode material prepared by the invention ranges from 80nm-180nm, the initial charging/discharging performance achieves 194.4-210.3mAh/g, and the electrochemical performance is excellent.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials and preparation methods thereof, and more specifically relates to a ternary composite cathode material LiNi x co y mn 1-x-y o 2 Methods. technical background [0002] In recent years, with the popularity of portable electronic devices and the development of electric vehicles, lithium-ion batteries as a new generation of high-energy power sources have received great attention. As a cathode material for lithium-ion batteries, layered LiCoO 2 It has been used commercially on a large scale, but its further development is limited due to the toxicity and high cost of cobalt; LiMn 2 o 4 Due to the Jahn-Teller effect in the charge and discharge process, the material undergoes crystal transformation and has a low capacity; LiNiO 2 with LiCoO 2 Similar layered structure, low toxicity, low cost, and large capacity, but nickel and lithium are prone to mixing, resulting in poor stability of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/525H01M4/505
CPCY02E60/122Y02E60/10
Inventor 王志兴王接喜李新海郭华军彭文杰胡启阳张云河
Owner CENT SOUTH UNIV
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