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Doped cobaltosic oxide and preparation method thereof

A doped cobalt tetroxide technology, which is applied in the field of doped cobalt tetroxide and its preparation, can solve the problems of inapplicability to the preparation of doped single crystal cobalt tetroxide, low compaction density of positive electrode materials, uneven distribution of doping elements, etc., to achieve The effect of dense particles, fine crystal nuclei, and accelerated growth rate

Pending Publication Date: 2021-05-07
HUNAN SHANSHAN ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation technology of single crystal tricobalt tetroxide is generally prepared by spray pyrolysis method. The spray pyrolysis method mainly obtains single crystal tricobalt tetroxide by pyrolysis of cobalt chloride solution, but this method will cause a large amount of hydrogen chloride gas to be produced, and the tail gas treatment is stricter, and The spray pyrolysis method cannot be applied to the preparation of doped single crystal cobalt tetroxide
[0004] At present, lithium cobaltate cathode materials are mostly made of polycrystalline small particles of cobalt tetroxide with conventional secondary spherical particles, but there are relatively high pores inside the polycrystalline small particle raw materials, and due to the small particle size, cobalt and doping elements are in the sintering process. It is easy to form a state of phase separation, which makes the distribution of doping elements uneven, and the positive electrode material prepared by using polycrystalline aggregates has low compaction density and serious battery gas production.

Method used

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  • Doped cobaltosic oxide and preparation method thereof
  • Doped cobaltosic oxide and preparation method thereof
  • Doped cobaltosic oxide and preparation method thereof

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Embodiment 1

[0057] A kind of doping type tricobalt tetroxide precursor of the present invention, molecular formula is Co 2.97 Al 0.027 o 4 , the morphology is single crystal particles, the primary grain size is 400nm, the half-maximum width of the 311 crystal plane is 0.25, and the particle size of doped cobalt tetroxide is D 10 = 2.72 μm, D 50 = 4.52 μm, D 90 =6.73μm; particle size distribution (D 90 -D 10 ) / D 50 =0.88, tap density TD=1.77g / cm 3 , bulk density = 1.25g / cm 3 , (BET-2.5) / (TD-1.5)=0.91.

[0058] The preparation method of the doped tricobalt tetroxide precursor of this embodiment comprises the following steps:

[0059] (1) According to Co 2.97 Al 0.027 o 4 The stoichiometric ratio preparation metal ion total concentration (aluminum ion and cobalt ion) is the soluble mixed salt solution of 110g / l;

[0060] (2) Add 10L of pure water in the 50L reactor as the bottom liquid of the reactor, pump a certain amount of ammonium bicarbonate solution into the bottom liquid ...

Embodiment 2

[0069] A kind of doping type cobalt tetroxide of the present invention, molecular formula is Co 2.97 Al 0.02 Mg 0.01 o 4 , its morphology is similar to single crystal aggregates, the primary grain size is 300nm, the half-maximum width of the 311 crystal plane is 0.3, and the particle size of doped tricobalt tetroxide is D 10 = 2.22 μm, D 50 = 4.3 μm, D 90 =6.42μm; particle size distribution (D 90 -D 10 ) / D 50 =0.97, tap density TD=2.05g / cm 3 , bulk density = 1.25g / cm 3 , (BET-2.5) / (TD-1.5)=0.73.

[0070] The preparation method of the doped tricobalt tetroxide of the present embodiment comprises the following steps:

[0071] (1) According to Co 2.97 Al 0.02 Mg 0.01 o 4 The stoichiometric ratio, preparation metal ion total concentration (cobalt ion and doping metal ion) is the soluble mixed salt solution of 110g / l;

[0072] (2) Add 10L of pure water in the 50L reactor as the bottom liquid of the reactor, pump a certain amount of ammonium bicarbonate solution into ...

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Abstract

The invention discloses doped cobaltosic oxide; the morphology of the doped cobaltosic oxide is single-crystal particles or single-crystal-like aggregates, the primary grain size is 200-500 nm, and the half-peak width of the 311 crystal face is 0.2-0.6. The preparation method comprises the steps: adjusting the pH value of a reaction kettle base solution to 7.1+ / -0.05; adding a mixed salt solution containing cobalt and doped elements and an ammonium bicarbonate solution into a reaction kettle for reaction, and controlling the pH value of a reaction system to be 7.1+ / -0.05; standing and clarifying the slurry overflowing from the full liquid level of the reaction kettle, removing the supernatant, controlling the solid content of the slurry, returning the slurry to the reaction kettle for reaction, and stopping feeding until the reaction reaches the target particle size; and washing, drying, sieving and calcining the obtained material to obtain the doped cobaltosic oxide. The doped cobaltosic oxide has a monocrystal or monocrystal-like aggregate morphology, the compaction density is obviously higher, and a guarantee is provided for synthesis of a lithium cobalt oxide positive electrode material with high energy density.

Description

technical field [0001] The invention belongs to the field of lithium ion battery materials, and in particular relates to a doped tricobalt tetroxide and a preparation method thereof. Background technique [0002] With the iterative upgrade of products in the digital field and the rapid development of various high-end aircraft models, drones and other emerging electronic products, the requirements for the lightweight and battery capacity of lithium batteries are getting higher and higher. Lithium cobaltate cathode material has an important application direction in the digital field. As electronic products have increasingly stringent requirements on the performance of lithium batteries, the update and iteration of lithium cobaltate cathode material is particularly important. The performance of the lithium cobalt oxide cathode material largely depends on the performance of the precursor. Currently, in order to prepare a high energy density cathode material, on the one hand, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/22C30B7/10C30B1/10C01G51/04H01M4/52H01M4/62H01M10/0525
CPCC30B29/22C30B7/10C30B1/10C01G51/04H01M4/523H01M4/62H01M10/0525H01M2004/028H01M2004/021Y02E60/10
Inventor 胡进陈九华杨志
Owner HUNAN SHANSHAN ENERGY TECH CO LTD
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