Oxalate coprecipitation preparation method for high-capacity lithium-rich cathode material

A lithium-rich positive electrode material and oxalate technology, which is applied in battery electrodes, nickel oxide/nickel hydroxide, electrical components, etc., can solve the problems such as difficult to accurately control the impurity content and proportion of sediments, and improve structural stability and charge-discharge specific capacity, shape and size are easy, and the effect of low temperature

Inactive Publication Date: 2012-10-17
CHINA FIRST AUTOMOBILE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the basic salt co-precipitation method is used to prepare the precursor, there is a disadvantage that the content and ratio of impurities in the precipitate are difficult to accurately control.

Method used

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  • Oxalate coprecipitation preparation method for high-capacity lithium-rich cathode material
  • Oxalate coprecipitation preparation method for high-capacity lithium-rich cathode material
  • Oxalate coprecipitation preparation method for high-capacity lithium-rich cathode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Preparation of Li[Li 0.13 co 0.61 mn 0.26 ]O 2 material, namely x Li 2 MnO 3 ? ( 1-x )LiMO 2 M=Co in the material, x = 0.3.

[0022] (1) Preparation of metal salt solution: Co(NO 3 ) 2 and Mn(NO 3 ) 2 According to the molar ratio n (Co(NO3)2) :n (Mn(NO3)2) =0.61:0.26 ratio dissolved in deionized water, prepared to a concentration of 1mol L -1 solution of metal salts.

[0023] (2) Preparation of oxalate solution: Na 2 C 2 o 4 Dissolved in deionized water, prepared to a concentration of 2.5mol L -1 sodium oxalate solution.

[0024] (3) The solution is mixed and added: adopt the method of "reverse addition", add 1mol L -1 Slowly drop the metal salt solution with a concentration of 2.5mol L -1 In the sodium oxalate solution, the pH value of the mediation solution is 6.5, forming a co-precipitation solution.

[0025] (4) Solid-liquid separation: filter the above co-precipitation solution through filter paper, wash with dei...

Embodiment 2

[0028] Preparation of Li[Li 0.184 Ni 0.224 mn 0.725 ]O 2 material, namely x Li 2 MnO 3 ? ( 1-x )LiMO 2 M= Ni in the material 1 / 2 mn 1 / 2 ， x = 0.45 .

[0029] (1) Preparation of metal salt solution: NiSO 4 and MnSO 4 According to the molar ratio n (NiSO4) :n (MnSO4) =0.224:0.725 ratio dissolved in deionized water, prepared to a concentration of 2.5mol L -1 solution of metal salts.

[0030] (2) Preparation of oxalate solution: K 2 C 2 o 4 Dissolved in deionized water, prepared to a concentration of 3.5mol L -1 of potassium oxalate solution.

[0031] (3) The solution is mixed and added: adopt the method of "adding together", add 2.5mol·L -1 The metal salt solution and the concentration is 3.5mol L -1 The potassium oxalate solution was dropped into a beaker equipped with deionized water at the same time, and the pH value of the mediation solution was 8 to form a co-precipitation solution.

[0032] (4) Solid-liquid separati...

Embodiment 3

[0036] Preparation of Li[Li 0.133 Ni 0.3 mn 0.567 ]O 2 material, namely x Li 2 MnO 3 ? ( 1-x )LiMO 2 M= Ni in the material 1 / 2 mn 1 / 2 ， x = 0.3 .

[0037] (1) Preparation of metal salt solution: NiSO 4 and Mn(NO 3 ) 2 According to the molar ratio n (NiSO4) :n (Mn(NO3)2) The ratio of =0.300:0.567 is dissolved in deionized water, and the concentration is 3mol L -1 solution of metal salts.

[0038] (2) Preparation of oxalate solution: add NH 4 HC 2 o 4 Dissolved in deionized water, prepared to a concentration of 3mol L -1 ammonium hydrogen oxalate solution.

[0039] (3) The solution is mixed and added: adopt the method of "reverse addition", add 3mol L -1 Slowly drop the metal salt solution with a concentration of 3mol L -1 In the ammonium hydrogen oxalate solution, the pH value of the mediation solution is 7, forming a co-precipitation solution.

[0040] (4) Solid-liquid separation: filter the above co-precipitation sol...

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Abstract

The invention relates to an oxalate coprecipitation preparation method for a high-capacity lithium-rich cathode material. The preparation method is characterized by comprising the following concrete steps: dissolving soluble Ni salt, or Co salt and Mn salt, or Ni salt, Co salt and Mn salt in a proper amount of deionized water according to a stoichiometric ratio to prepare a metal salt solution with certain concentration, dissolving oxalate or oxalic acid in deionized water to prepare an oxalate solution with certain concentration, mixing the metal salt solution with an oxalate or oxalic acid solution in a way of straight adding, reverse adding or combined adding, adjusting the pH value of a mixed solution to be in a range of from 6.5 to 8.5, allowing a coprecipitation solution to be formed, and carrying out filtration with filter paper, rinsing with deionized water and drying on the coprecipitation solution so as to obtain precipitation precursor; and subjecting excess Li salt and the precipitation precursor in a certain stoichiometric ratio to ball milling and mixing and carrying out high temperature sintering so as to obtain an xLi2MnO3.(1 - x)LiMO2 (wherein M is Co, Ni1/2Mn1/2 or Ni1/3Co1/3Mn1/3) material at last. The method costs little and does not need a high temperature in preparation of a lithium-rich material and allows the shape and the size of the prepared material to be easily controllable.

Description

technical field [0001] The invention relates to an oxalate co-precipitation preparation method of a high-capacity lithium-rich positive electrode material, and belongs to the technical field of lithium-ion battery materials. Background technique [0002] Since SONY manufactured the first lithium-ion battery in 1990, lithium-ion batteries have developed rapidly and replaced nickel-metal hydride batteries, and have been widely used in the fields of electronic equipment, energy storage and new energy vehicles. Nowadays, the improvement of the capacity and cycle performance of lithium-ion batteries is a problem that researchers from all over the world are eager to solve, mainly to find new positive and negative electrode materials with higher capacity. If the capacity of the positive electrode material can be increased and doubled, the total capacity and energy of the battery can be greatly improved. Therefore, in order to improve the performance of lithium-ion batteries and in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02C01G53/04C01G51/04H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 姜涛陈慧明张克金张斌赵中令王丹
Owner CHINA FIRST AUTOMOBILE
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