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Method for preparing lithium-rich solid solution positive electrode material by gas oxidation-acid solution combined treatment

A technology of combined processing and cathode material, applied in the manufacture of hybrid/electrical double-layer capacitors, electrical components, battery electrodes, etc., can solve the problems that affect the electrochemical performance of the prepared samples, mix discharge, cannot exclude the influence of oxygen, etc., and achieve excellent discharge. The effect of performance, less time-consuming and low cost of raw materials

Active Publication Date: 2014-10-22
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have shown that in the prepared lithium-rich solid solution materials, different lithium-site, manganese-site and nickel-site ions are often mixed, which seriously affects the electrochemical performance of the prepared samples.
In order to solve this problem, in the preparation of hydroxide precipitation, some literatures use the method of nitrogen protection precipitation. However, the method of nitrogen protection precipitation can only eliminate the influence of oxygen in the air, but cannot exclude the influence of oxygen dissolved in water.

Method used

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  • Method for preparing lithium-rich solid solution positive electrode material by gas oxidation-acid solution combined treatment

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Embodiment 1

[0038] Lithium hydroxide, nickel hydroxide, manganese acetate, and cobalt hydroxide were weighed respectively according to the molar ratio of lithium ion, nickel ion, manganese ion, and cobalt ion being 1.15: 0.0425: 0.4543: 0.3825. The total weight of reactants is the total weight of lithium hydroxide, nickel hydroxide, manganese acetate and cobalt hydroxide. The weight ratio of the total weight of reactants to deionized water is 1:10. Weigh deionized water (equivalent to (2·(1-x)·y+4·(x+z-x·z)+3·( 1-x) k-x-3)=-0.10).

[0039] Mix the weighed nickel hydroxide, manganese acetate and cobalt hydroxide in deionized water, wet grind and mix with a wet grinder for 1 hour, add ammonia water to make the solution acidity pH 10, add lithium hydroxide, and prepare a reaction mixture containing the precipitate The solution was wet milled and mixed for 1 hour to prepare a reaction mixture solution containing the precipitate. Aging the reaction mixture solution containing the precipitate...

Embodiment 2

[0042] According to the mol ratio of lithium ion, nickel ion, manganese ion, cobalt ion is 1.60: 0.18: 0.65: 0.18 respectively weigh lithium nitrate, nickel oxalate, manganese sulfate, cobalt chloride (equivalent to the (2.(1 -x) y + 4 (x+z-x z) + 3 (1-x) k-x-3)=-0.10); the total weight of reactants is lithium nitrate, nickel oxalate, manganese sulfate and chloride For the total weight of cobalt, weigh the aqueous ethanol solution according to the weight ratio of the total weight of the reactants to the aqueous ethanol solution being 5:1. The volume ratio of ethanol to deionized water in the ethanol aqueous solution is 10:1.

[0043] Mix the weighed nickel oxalate, manganese sulfate and cobalt chloride into the ethanol aqueous solution, wet-mill and mix for 15 hours with a common ball mill, add ammonia water to make the solution acidity pH 14, add lithium nitrate, and wet-mill and mix with a common ball mill for 24 hours to prepare Reaction mixed solution containing precipita...

Embodiment 3

[0046] According to the molar ratio of lithium ion, nickel ion, manganese ion, cobalt ion is 1.6 : 0.02: 0.90 : 0.02 respectively take lithium iodide, nickel nitrate, manganese oxalate, cobalt oxalate; , the gross weight of manganese oxalate and cobalt oxalate, according to reactant total weight and methanol aqueous solution weight ratio is 5:75 weighing methanol aqueous solution (equivalent to (2 · (1-x) · y+4 · (x) of summary of the invention part +z-x z) + 3 (1-x) k-x-3)=0.10). The volume ratio of methanol to deionized water in methanol aqueous solution is 1:10.

[0047] Mix weighed nickel nitrate, manganese oxalate and cobalt oxalate into methanol aqueous solution, wet mill and mix for 1 hour with a super energy ball mill, add ammonia water to make the solution acidity pH 10, add weighed lithium iodide, and wet mill with a super energy ball mill Mix for 1 h to prepare a reaction mixture solution containing the precipitate. Precursor 1 was obtained by aging the reaction m...

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Abstract

The invention relates to a method for preparing a lithium-rich solid solution cathode material through gas oxidation and acid solution combined treatment. The method comprises the following steps of: weighing a lithium compound, a nickel compound, a manganese compound and a cobalt compound in a molar ratio of lithium ions to nickel ions to manganese ions to cobalt ions of (1+x):(1-x).y:(x+z-x.z):(1-x).k; mixing the weighed nickel compound, manganese compound and cobalt compound in a wet grinding medium, performing wet grinding and mixing, adding ammonia water and the lithium compound, performing wet grinding and mixing again, aging a reaction mixed solution containing a precipitate, heating, drying, putting a precursor 2 in air, oxygen-rich gas or pure oxygen atmosphere, and performing two-section sintering to prepare a precursor 3; and treating the precursor 3 by using an acid solution, drying, and sintering to obtain the lithium-rich solid solution cathode material. The electrode material prepared by the method has uniform composition, high discharge performance, and high charge and discharge current efficiency particularly under the high-current condition.

Description

technical field [0001] The invention belongs to the technical field of battery electrode material preparation, and in particular relates to a method for preparing a lithium-rich solid solution positive electrode material using oxidative gas oxidation-acid solution combined treatment, which can be used for lithium batteries, lithium ion batteries, polymer batteries and supercapacitors. technical background [0002] Spinel LiMn 2 o 4 It has the characteristics of high working voltage, low price, and environmental friendliness, but the reversible capacity of the positive electrode material is low, and the discharge point capacity is only 90-100mAh / g when charging and discharging at a rate of 1C; at high temperatures, the discharge capacity of the positive electrode material will change with the Charge-discharge cycles proceed with rapid attenuation. [0003] Lithium-rich solid solution cathode material Li 2 MnO 3 ·Li[Ni 1 / 3 co 1 / 3 mn 1 / 3 ]O 2 It shows the advantages of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/48H01G11/86
CPCY02E60/10
Inventor 童庆松
Owner FUJIAN NORMAL UNIV