A method for preparing a lithium-rich manganese-based cathode material coated with lithium titanium phosphate

A lithium-rich manganese-based, cathode material technology, applied in the direction of positive electrode, battery electrode, active material electrode, etc., can solve the problems of electrochemical performance to be improved, uncontrollable hydrothermal method, unsuitable for large-scale production, etc. The effect of alleviating layered-spinel phase transition, excellent cycle stability, and improving poor electrical conductivity

Active Publication Date: 2019-01-01
CENT SOUTH UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] CN107591529A discloses a synthetic method of coating titanium lithium phosphate on nickel-cobalt-manganese ternary positive electrode material by using a hydrothermal method, but the first discharge capacity of the obtained material is only 173.7mAh / g at 0.1C, and the electrochemical performance needs to be improved ; and, the hydrothermal method has certain uncontrollability, the yield is low, and it is not suitable for large-scale production

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  • A method for preparing a lithium-rich manganese-based cathode material coated with lithium titanium phosphate
  • A method for preparing a lithium-rich manganese-based cathode material coated with lithium titanium phosphate
  • A method for preparing a lithium-rich manganese-based cathode material coated with lithium titanium phosphate

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Embodiment 1

[0044] This embodiment includes the following steps:

[0045] (1) Preparation of lithium-rich manganese-based cathode materials

[0046] Weigh 0.0840mol lithium-rich manganese-based precursor Mn 4 / 6 Ni 1 / 6 co 1 / 6 CO 3 With 0.1302molLiOH. h 2O was hand-milled and mixed (the amount of excess lithium was 5%), and the grinding time was 2h; the raw materials were put into a crucible, placed in a muffle furnace, and pre-sintered at 500°C for 6h in an air atmosphere, and then sintered at 900°C for 10h, and the temperature was raised. The rate is 5°C / min. After the furnace temperature is cooled to room temperature, the lithium-rich manganese-based cathode material 0.5Li 2 MnO 3 0.5Li(Ni 1 / 3 co 1 / 3 mn 1 / 3 )O 2 ;

[0047] (2) Dissolve 3.0000 g of lithium-rich manganese-based cathode material (337.8 mmol) obtained in step (1) in 90 mL CH 3 CH 2 OH, stir evenly, add 20.0000mmol C 16 h 36 o 4 Ti (density 0.9660g / cm 3 ), and stir evenly to obtain a black suspension a;

[...

Embodiment 2

[0054] This embodiment includes the following steps:

[0055] (1) Preparation of lithium-rich manganese-based cathode materials

[0056] Weigh 0.1680mol lithium-rich manganese-based precursor Mn 4 / 6 Ni 1 / 6 co 1 / 6 CO 3 with 0.1310molLi 2 CO 3 Carry out hand grinding and mixing (the amount of lithium is 6%), and the grinding time is 3 hours; put the raw materials into a crucible, place them in a muffle furnace, and pre-sinter at 500°C for 6 hours in an air atmosphere, then sinter at 950°C for 15 hours, and then heat up The rate is 5°C / min. After the furnace temperature is cooled to room temperature, the lithium-rich manganese-based cathode material 0.5Li 2 MnO 3 0.5Li(Ni 1 / 3 co 1 / 3 mn 1 / 3 )O 2 ;

[0057] (2) Dissolve 1.5000 g (168.9 mmol) of the lithium-rich manganese-based cathode material obtained in step (1) in 90 mL CH 3 CH 2 OH, stir evenly, add 20.0000mmol C 16 h 36 o 4 Ti (density 0.9660g / cm 3 ), and stir evenly to obtain a black suspension a;

[0058] ...

Embodiment 3

[0064] This embodiment includes the following steps:

[0065] (1) Preparation of lithium-rich manganese-based cathode materials

[0066] Weigh 0.1680mol lithium-rich manganese-based precursor Mn 4 / 6 Ni 1 / 6 co 1 / 6 CO 3 with 0.1302molLi 2 CO 3 Carry out hand-grinding and mixing (the amount of excess lithium is 5%), and the grinding time is 2 hours; put the raw materials into a crucible, place them in a muffle furnace, pre-sinter at 500°C for 5 hours, and then sinter at 900°C for 12 hours, with a heating rate of 3°C / min, after the furnace temperature is cooled to room temperature, the lithium-rich manganese-based cathode material 0.5Li 2 MnO 3 0.5Li(Ni 1 / 3 co 1 / 3 mn 1 / 3 )O 2 ;

[0067] (2) Dissolve 3.0000 g of lithium-rich manganese-based cathode material (337.8 mmol) obtained in step (1) in 40 mL CH 3 CH 2 OH, stir evenly, add 20.0000mmol C 16 h 36 o 4 Ti (density 0.9660g / cm 3 ), and stir evenly to obtain a black suspension a;

[0068] (3) Add 30.0000mmolH 3...

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Abstract

A method for preparing a lithium-rich manganese-based cathode material coated with lithium titanium phosphate comprises the following steps: (1) mixing and grinding a lithium-rich manganese-based precursor with a lithium source, calcining in an air atmosphere, and cooling; 2, dispersing the lithium-rich manganese-based cathode material in an anhydrous organic solvent I and uniformly stirring; thenadding a titanium source, uniformly stirring to obtain a black suspension a; 3, weighing a lithium source and phosphorus source, adding the lithium source and phosphorus source into an anhydrous organic solvent II, uniformly stirring to obtain a mixed suspension b; 4) adding the mixed suspension b into the black suspension a for reaction, evaporating in an oil bath to obtain dry gel powder; 5, calcining the dry gel powder under a reducing atmosphere to obtain the material. As the surface coating layer, the lithium titanium phosphate of the invention can not only alleviate the cracking and lamellar-snipel phase change of the secondary particles, but also can improve the positive pole-electrolyte interface kinetics, and thus the lithium-rich manganese-based cathode material composite coatedwith lithium titanium phosphate have excellent cycle stability.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material, in particular to a preparation method of a lithium-rich manganese-based positive electrode material coated with lithium titanium phosphate. Background technique [0002] Lithium-ion batteries have the advantages of high specific energy density, long charge and discharge life, no memory effect, less environmental pollution, and low self-discharge rate. Since their inception, lithium-ion batteries have been occupying the high-end market of portable batteries. [0003] Lithium-rich manganese-based cathode material is currently the most concerned material in the research of lithium-ion batteries. The general formula x Li 2 MnO 3 ·(1- x )LiMO 2 (M=Ni, Co, Mn, 0< x <1) means that it has many advantages such as high capacity, high thermal stability, and high energy density, but it also has problems such as serious voltage attenuation and low conductivity. This is due t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/505H01M4/525H01M4/62H01M10/0525
CPCH01M4/366H01M4/505H01M4/525H01M4/624H01M4/628H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 郑俊超杨书棋王鹏博田业成韦韩信
Owner CENT SOUTH UNIV
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