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Method for preparing lithium-rich positive electrode material through adjustable low temperature combustion method

A lithium-rich cathode material, low-temperature combustion technology, applied in battery electrodes, electrical components, electrochemical generators, etc., can solve the problems of irreversible capacity loss, high price, poor rate discharge performance, etc., to save equipment investment costs, improve The rate of crystallization, the effect of high specific surface area and pore size

Inactive Publication Date: 2018-11-16
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The positive electrode materials currently used and researched are mainly lithium-containing materials with crystal structures such as layered, spinel, and olivine, mainly LiCoO 2 , LiNiO 2 , LiMnO 2 , LiMn 2 o 4 、LiFePO 4 、LiCo 1 / 3 Ni 1 / 3 mn 1 / 3 o 2 And some other series of cathode materials, but each has disadvantages such as poor safety, high price, low energy density, poor cycle performance, etc., which limit its development
With the national requirement for the energy density of lithium-ion batteries to reach 300Wh / Kg, none of the current commercial cathode materials can meet the demand
The new lithium-rich cathode material x Li 2 MnO 3 ·(1- x )LiMO 2 (M=Co, Ni, Mn) The theoretical specific capacity is as high as 350mAh / g, and commercialization is expected to obtain a specific energy of 300Wh / Kg. However, the irreversible capacity loss of the material produced by the traditional co-precipitation method reaches 40~100mAh / g for the first charge and discharge. , due to the erosion of the electrolyte, the poor cycle performance of the material, and the poor discharge performance of the rate, etc.
The current improvement methods mainly include ion doping and surface coating, which undoubtedly increases the cost of battery production

Method used

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  • Method for preparing lithium-rich positive electrode material through adjustable low temperature combustion method
  • Method for preparing lithium-rich positive electrode material through adjustable low temperature combustion method
  • Method for preparing lithium-rich positive electrode material through adjustable low temperature combustion method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In this example, carbonamide is used as a reducing agent, and an appropriate amount of polyethylene glycol is added to a mixed solvent of deionized water and ethanol to prepare a lithium-rich positive electrode material 0.4Li 2 MnO 3 0.4Li[Ni 1 / 3 co 1 / 3 mn 1 / 3 ]O 2 . Prepare 100ml of ethanol solution with a volume fraction of 50%, and prepare 0.5mol / L LiNO according to the stoichiometric ratio 3、 Ni(NO 3 ) 2 ·6H 2 O, Co(NO 3 ) 2 ·6H 2 O and Mn(NO 3 ) 2 (50% aqueous solution) metal salt mixed solution A, add 0.14mol carbonamide, 5ml polyethylene glycol, stir evenly, add ammonia water dropwise to adjust the pH to 8, and obtain solution B. Put solution B in a 100-degree oil bath and stir the reaction until the solution is concentrated to 50ml, pour it into a crucible, burn it at 600 degrees, keep it warm for 1 hour and take it out to obtain powder C, collect and grind C, and place it under a muffle furnace at high temperature Calcined at 900°C for 12 hours, c...

Embodiment 2

[0028] In this example, carbonamide and citric acid were used as reducing agents, and an appropriate amount of Tween 20 was added to deionized water to prepare a lithium-rich cathode material 0.5 / 3Li 2 MnO 30.5Li[Ni 1 / 3 co 1 / 3 mn 1 / 3 ]O 2 . Prepare 100ml of propanol solution with a volume fraction of 50%, and prepare 0.5mol / L LiNO according to the stoichiometric ratio 3 , Ni(NO 3 ) 2 ·6H 2 O, Co(NO 3 ) 2 ·6H 2 O and Mn(NO 3 ) 2 (50% aqueous solution) metal salt mixed solution A, add 0.1mol carbonamide and 0.5mol citric acid, 2ml Tween 20, stir evenly, add ammonia water dropwise to adjust the pH to 8, and obtain solution B. Put solution B in a 90-degree oil bath and stir the reaction until the solution is concentrated to 65ml, pour it into a crucible, burn it at 550 degrees, keep it warm for 0.5h, take it out to obtain powder C, collect and grind C, and place it under a muffle furnace Calcined at a high temperature of 900 degrees for 12 hours, cooled and sieved b...

Embodiment 3

[0031] In this example, carbohydrazide was used as a reducing agent, and an appropriate amount of PVDF was added to a mixed solvent of deionized water and ethylene glycol to prepare a lithium-rich cathode material 0.2 / 3Li 2 MnO 3 0.9Li[Ni 0.4 co 0.2 mn 0.2 ]O 2 . Prepare 100ml of ethylene glycol solution with a volume fraction of 20%, and prepare 0.5mol / L CH 3 COOLi·2H 2 O 、Ni(CH 3 COO) 2 4H 2 O, Co(CH 3 COO) 2 4H 2 O and Mn(CH 3 COO) 2 4H 2 O metal salt mixed solution A, add 0.08mol carbohydrazide, 2g PVDF powder, stir evenly, add ammonia water dropwise to adjust the pH to 7, and obtain solution B. Put solution B in a 100-degree oil bath and stir the reaction until the solution is concentrated to 60ml, pour it into a crucible, burn it at 500 degrees, keep it warm for 2 hours and take it out to obtain powder C, collect and grind C, and place it under a muffle furnace at high temperature Calcined at 900°C for 12 hours, cooled and sieved by a ball mill to obtain ...

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Abstract

The invention belongs to the technical field of the preparation of positive materials for lithium-ion batteries, and specifically provides a method for preparing a lithium-rich positive electrode material 2x / 3Li2MnO3*(1-x)LiMO2 through an adjustable low temperature combustion method, wherein x is greater than 0 and smaller than 1, and M is Ni, Co and Mn. The method comprises the following steps: dissolving an Ni-Co-Mn metal salt into a solvent according to a stoichiometric proportion, adding a certain amount of a reducing agent and a certain amount of an additive, stirring uniformly, dropwiseadding an appropriate amount of ammonia water to adjust PH so as to obtain a solution A; After heating and evaporating the solution A for a certain period of time, putting the solution A in a heatingfurnace so that the heating furnace is combusted at the temperature of 300 to 700 DEG C to obtain powder B, collecting and grinding the B, putting the powder B in a muffle furnace for combustion for 5to 24 h at the high temperature of 700 to 1100 DEG C, and carrying out ball-milling sieving after cooling to obtain the lithium-rich positive electrode material. The preparation method is simple andquick, various elements in the solution can be mixed in a molecular level, the ultrafine nanoscale material can be prepared, the energy consumption is low, the reaction can be adjusted through parameters, the synthesizing cost of the lithium-rich positive electrode material is greatly reduced, and the rate capability and cycle performance of the lithium-rich positive electrode material are also obviously improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of positive electrode materials for lithium ion batteries, and specifically provides a method for preparing lithium-rich positive electrode materials by an adjustable low-temperature combustion method. Background technique [0002] With the world's energy crisis and environmental protection issues becoming more and more prominent, the background of seeking new energy is the increasing importance of national energy security. In recent years, the market demand for new energy materials such as lithium carbonate has surged, and the new energy revolution will break out in an all-round way and the momentum has already emerged. At present, my country urgently needs to develop lithium-ion batteries with high energy density, high power, long cycle life and high safety. The positive electrode material is the material with the highest cost of lithium-ion batteries, accounting for about 1 / 3 of the cost o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/505H01M4/525H01M10/0525
CPCH01M4/364H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 温广武王桢
Owner SHANDONG UNIV OF TECH
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