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A kind of preparation method of quasi-spherical lithium nickel manganese oxide positive electrode material

A technology of lithium nickel manganese oxide and positive electrode materials, applied in battery electrodes, electrical components, circuits, etc., can solve the problems of uneven particle size of products and uneven local concentration of solutions, so as to simplify the production process and improve electrochemical performance , the effect of large specific surface area

Active Publication Date: 2016-10-05
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method of adding a direct precipitant is likely to cause the problem of uneven local concentration of the solution, resulting in uneven particle size of the product

Method used

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  • A kind of preparation method of quasi-spherical lithium nickel manganese oxide positive electrode material
  • A kind of preparation method of quasi-spherical lithium nickel manganese oxide positive electrode material
  • A kind of preparation method of quasi-spherical lithium nickel manganese oxide positive electrode material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 6.22g (0.025mol) nickel acetate (Ni(CH 3 COO) 2 4H 2 O) and 12.98g (0.075mol) manganese acetate (Mn(CH 3 COO) 2 ) was dissolved in 50ml of ethanol, the total concentration of metal ions was 2.0M, and 15.02g (0.25mol) of urea was added according to the molar ratio of urea to metal ions of 2.5:1, and 0.08g of CTAB and 0.16g of PVP were added after magnetic stirring for 30min. The mixed solution was magnetically stirred for 2 hours, then transferred to a polyvinyl fluoride-lined autoclave, sealed and reacted at 160°C for 12 hours, cooled to room temperature naturally, centrifuged, washed, and dried to obtain Ni 0.25 mn 0.75 CO 3 Precursor. It looks like figure 2 As shown, it is flocculent-like spherical secondary particles composed of primary flake-like particles.

[0031] The resulting Ni 0.25 mn 0.75 CO 3 The precursor was pre-fired at 500 °C for 3 hours, and then combined with Li 2 CO 3 According to Li:(Ni+Mn)=1.03:2 (molar ratio), after mixing evenly, cal...

Embodiment 2

[0033] 6.54g (0.0225mol) nickel nitrate (Ni(NO 3 ) 2 ·6H 2 O) and 16.88g (0.0675mol) manganese nitrate (Mn(NO 3 ) 2 4H 2 O) Dissolve in 60ml of ethylene glycol, the total concentration of metal ions is 1.5M, add 8.11g (0.135mol) urea according to the molar ratio of urea to metal ions of 1.5:1, stir magnetically for 30 minutes, then add 0.05g CTAB and 0.15g PVP, the mixed solution was magnetically stirred for 2 hours, then transferred to a polyvinyl fluoride-lined autoclave, sealed and reacted at 165°C for 15 hours, naturally cooled to room temperature, centrifuged, washed, and dried , making Ni 0.25 mn 0.75 CO 3 Precursor.

[0034] The resulting Ni 0.25 mn 0.75 CO 3 The precursor was pre-fired at 500 °C for 3 hours, and then mixed with LiNO 3 According to Li:(Ni+Mn)=1.07:2 (molar ratio), after mixing evenly, calcining at 780°C in the air for 12 hours, after natural cooling and grinding, the LiNi 0.5 mn 1.5 o 4 Cathode material. Mix this material with acetylene ...

Embodiment 3

[0036] 4.98g (0.02mol) nickel acetate (Ni(CH 3 COO) 2 4H 2 O) and 10.38g (0.06mol) manganese acetate (Mn(CH 3 COO) 2 ) was dissolved in 80ml of ethylenediamine, the total concentration of metal ions was 1.0M, and 9.61g (0.16mol) of urea was added according to the molar ratio of urea to metal ions of 2:1, and 0.04g of CTAB and 0.12 g PVP, the mixed solution was magnetically stirred for 2 hours, then transferred to a polyvinyl fluoride-lined autoclave, sealed and reacted at 170°C for 10 hours, cooled to room temperature naturally, and the obtained precipitate was centrifuged, washed, and dried. Made Ni 0.25 mn 0.75 CO 3 Precursor.

[0037] The resulting Ni 0.25 mn 0.75 CO 3 After the precursor was pre-fired at 500 °C for 3 hours, it was mixed with LiOH·H 2 O is mixed uniformly according to Li:(Ni+Mn)=1.05:2 (molar ratio), calcined at 800°C in air for 12 hours, and the LiNi is obtained after natural cooling and grinding. 0.5 mn 1.5 o 4 Cathode material. Its X-ray d...

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Abstract

The invention discloses a preparation method for a sphere-like lithium nickel manganese oxide positive electrode material. The preparation method comprises the following steps: (1) weighing and dissolving soluble manganese salt and nickel salt into an organic solvent according to a stoichiometric ratio of LinNi0.5Mn1.5O4, wherein the total concentration of metal ions is 0.2-2 M; (2) by taking urea as a uniform precipitator and taking CTAB (cetyltrimethyl ammonium bromide) and PVP (polyvinyl pyrrolidone) as dual templates, preparing a flocculent sphere-like Ni0.25Mn0.75CO3 precursor through solvent thermal reaction, and then performing high-temperature lithiation to prepare the sphere-like lithium nickel manganese oxide positive electrode material. According to the preparation method disclosed by the invention, an anionic surfactant CTAB and a non-ionic high polymer compound PVP are taken dual templates to control so as to obtain flocculent sphere-like precursor particle with a relatively large specific surface area; a plurality of holes are formed between sheets, so that the contact and the penetration of a lithium source in a follow-up lithiation process are facilitated and the lithiation temperature is greatly lowered.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a method for preparing a spherical-like lithium nickel manganese oxide positive electrode material. Background technique [0002] With the shortage of global oil resources and the intensification of air pollution, the awareness of energy conservation and environmental protection has been deeply rooted in the hearts of the people, and the state has also increased its support for the field of new energy. Lithium-ion batteries take this as an opportunity to occupy the consumer market with their advantages such as low self-discharge rate, high specific energy, and no memory effect, and are widely used in portable electronic devices and other high-energy devices. In recent years, spinel lithium nickel manganese oxide (LiNi 0.5 mn 1.5 o 4 ) due to having 4.7V (vs.Li / Li + ) operating voltage, 147mAh / g theoretical specific capacity and higher energy density are consider...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/505H01M4/525
CPCH01M4/505H01M4/525H01M4/62Y02E60/10
Inventor 王丽刘贵娟郅晓科陈丹梁广川
Owner HEBEI UNIV OF TECH
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