A preparation method of lithium titanium phosphate coated lithium-rich manganese-based positive electrode material

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

Active Publication Date: 2021-08-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • 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

Method used

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  • A preparation method of lithium titanium phosphate coated lithium-rich manganese-based positive electrode material
  • A preparation method of lithium titanium phosphate coated lithium-rich manganese-based positive electrode material
  • A preparation method of lithium titanium phosphate coated lithium-rich manganese-based positive electrode material

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Embodiment 1

[0044] This embodiment includes the following steps:

[0045] (1) Preparation of lithium-rich manganese positive electrode materials

[0046] Weighing 0.0840mol lithium manganese-rich precursor MN 4 / 6 Ni 1 / 6 CO 1 / 6 CO 3 About 0.1302mollioh. Hide 2O Make hand grinding (5% lithium), grinding time 2H; put the raw material into the crucible, placed in a muffle, pre-sinter 6 h in the air atmosphere, then sintered at 900 ° C for 10 h, temperature rise The rate is 5 ° C / min, and after the furnace temperature is cooled to room temperature, that is, lithium manganese-rich positive electrode material 0.5Li 2 Mno 3 0.5li (Ni) 1 / 3 CO 1 / 3 Mn 1 / 3 ) O 2 ;

[0047] (2) Lithium manganese positive electrode material (337.8 mmol) obtained by 3.0000 g of step (1) is dissolved in 90 mlCH 3 CH 2 In OH, stir evenly, add 20.0000mmol C 16 Hide 36 O 4 Ti (density is 0.9660g / cm 3 ), Mix well, get black suspension A;

[0048] (3) 30.0000mmolh will 3 PO 4 10.0000mmol ch 3 Cooli · 2H 2 O Soluble in 10mlch ...

Embodiment 2

[0054] This embodiment includes the following steps:

[0055] (1) Preparation of lithium-rich manganese positive electrode materials

[0056] Weighing 0.1680mol lithium manganese-rich precursor MN 4 / 6 Ni 1 / 6 CO 1 / 6 CO 3 0.1310molli 2 CO 3 Carrying mix (6% lithium), grinding time 3 h; put the raw material into the crucible, placed in a muffle furnace, under the air atmosphere, first sintered at 950 ° C for 15 h, warmed up The rate is 5 ° C / min, and after the furnace temperature is cooled to room temperature, that is, lithium manganese-rich positive electrode material 0.5Li 2 Mno 3 0.5li (Ni) 1 / 3 CO 1 / 3 Mn 1 / 3 ) O 2 ;

[0057] (2) Lithium manganese-based positive electrode material from 1.5000 g (168.9 mmol) is dissolved in 90 mlch 3 CH 2 In OH, stir evenly, add 20.0000mmol C 16 Hide 36 O 4 Ti (density is 0.9660g / cm 3 ), Stir evenly, black suspension A;

[0058] (3) 30.0000mmolh will 3 PO 4 10.0000mmol ch 3 Cooli · 2H 2 O Soluble in 10mlch 3 CH 2 Oh, in OH, stir evenly, mix susp...

Embodiment 3

[0064] This embodiment includes the following steps:

[0065] (1) Preparation of lithium-rich manganese positive electrode materials

[0066] Weighing 0.1680mol lithium manganese-rich precursor MN 4 / 6 Ni 1 / 6 CO 1 / 6 CO 3 About 0.1302molli 2 CO 3 Carrying mix (5% lithium), grinding time 2H; put the raw material into the crucible, placed in the muffle, first sintered at 500 ° C, then sintered at 900 ° C for 12 h, the temperature rate of 3 ° C / MIN, after the furnace temperature is cooled to room temperature, that is, lithium-rich manganese positive electrode material 0.5Li 2 Mno 3 0.5li (Ni) 1 / 3 CO 1 / 3 Mn 1 / 3 ) O 2 ;

[0067] (2) Sollar manganese positive electrode material (337.8 mmol) obtained by 3.0000 g of step (1) is dissolved in 40 mlCH 3 CH 2 In OH, stir evenly, add 20.0000mmol C 16 Hide 36 O 4 Ti (density is 0.9660g / cm 3 ), Mix well, get black suspension A;

[0068] (3) 30.0000mmolh will 3 PO 4 10.0000mmol ch 3 Cooli · 2H 2 O Soluble in 5mlch 3 CH 2 Oh, in OH, stir evenly,...

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Abstract

A method for preparing a lithium-rich manganese-based positive electrode material coated with lithium titanium phosphate, comprising the following steps: (1) mixing and grinding a lithium-rich manganese-based precursor with a lithium source, calcining and cooling in an air atmosphere; (2) mixing Lithium-rich manganese-based positive electrode material was dispersed in anhydrous organic solvent I, and stirred evenly; then titanium source was added, and stirred evenly, to obtain a black suspension a; (3) Lithium source and phosphorus source were weighed, and mixed in anhydrous organic solvent II Add lithium source and phosphorus source to the mixture, stir evenly to obtain mixed suspension b; (4) Add mixed suspension b to black suspension a for reaction, and evaporate to dryness in an oil bath to obtain xerogel powder; (5) Calcining the xerogel powder in a reducing atmosphere. The titanium lithium phosphate of the present invention is used as the surface coating layer, which can not only alleviate the rupture of the secondary particles and the layer-spinel phase transition, but also improve the dynamics of the positive electrode-electrolyte interface, so that the lithium titanium phosphate can coat the lithium-rich manganese-based positive electrode The material composite has excellent cycle stability.

Description

Technical field [0001] The present invention relates to a method of preparation of a positive electrode material, and is specifically related to a preparation method of titanium phosphate lithium packets to lithium manganese positive electrode material. Background technique [0002] Lithium-ion batteries have the advantages of high energy density, long battery life, no memory effect, small environmental pollution, low self-discharge ratio, etc., has always occupied the high-end market in portable batteries since the advent. [0003] Lithium-rich manganese positive electrode material is a material that is most concerned in lithium-ion battery research, available x Li 2 Mno 3 ·(1- x Limo 2 (M = Ni, Co, Mn, 0 < x <1) is represented; it has high capacity, high thermal stability, high energy density, etc., but there is also a severe voltage attenuation and low electrical conductivity. This is due to the migration of Mn ions from the octahedral gap in the charge and discharge pro...

Claims

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Application Information

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Patent Type & AuthorityPatents(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
OwnerCENT SOUTH UNIV