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Method for preparing lithium-rich solid solution cathode material through reduction co-precipitation

A technology of co-precipitation and positive electrode materials, applied in battery electrodes, hybrid capacitor electrodes, electrical components, etc., can solve the problems of affecting the electrochemical performance of the prepared samples, mixed discharge, inability to exclude the influence of oxygen, etc., to achieve excellent discharge performance, consumption The effect of less time and low cost of raw materials

Active Publication Date: 2013-01-16
DYNABAT NEW ENERGY SCI & TECH CO CLD FUJIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 cathode material through reduction co-precipitation

Examples

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Embodiment 1

[0039] Lithium hydroxide, nickel hydroxide, manganese acetate, cobalt hydroxide, and hydrazine were weighed according to the molar ratio of lithium ion, nickel ion, manganese ion, cobalt ion, and hydrazine being 1.35: 0.195: 0.526: 0.319: 0.27. The total reactant volume is the sum of the volumes of lithium hydroxide, nickel hydroxide, manganese acetate and cobalt hydroxide. Measure two parts of deionized water (equivalent to (2·(1-x)·y+4·(x+z-x·z)+ 3 (1-x) k-x-3) = 0.0998).

[0040] At 40°C, mix a measured portion of deionized water with weighed nickel hydroxide, manganese acetate and cobalt hydroxide to obtain a mixed solution; add weighed hydrazine to the mixed solution, stir and mix, then add hydrogen The acidity of the reaction mixture solution containing the precipitate is pH 10 with a 1:1 weight ratio of lithium oxide to water, and it is wet-milled with a wet grinder for 0.5 hours, and the reaction mixture solution containing the precipitate is aged at 40°C for 2 Hours...

Embodiment 2

[0043]According to the molar ratio of lithium ion, nickel ion, manganese ion, cobalt ion, vitamin C is 1.15: 0.0425: 0.358: 0.51: 0.01, respectively weigh the total amount of lithium nitrate, nickel oxalate, manganese sulfate, cobalt chloride and vitamin C reactants. The volume is the sum of the volumes of lithium nitrate, nickel oxalate, manganese sulfate and cobalt chloride, and two parts of ethanol aqueous solution are measured according to the volume ratio of the total volume of reactants to ethanol aqueous solution at 1:0.5. The volume ratio of ethanol to deionized water in the ethanol aqueous solution is 10:1. (equivalent to (2 · (1-x) · y + 4 · (x+z-x · z) + 3 · (1-x) · k-x-3) = -0.10).

[0044] At 95°C, mix a measured portion of ethanol aqueous solution with weighed nickel oxalate, manganese sulfate, and cobalt chloride to obtain a mixed solution. Add weighed vitamin C to the mixed solution, and at the same time add a lye with a weight ratio of lithium hydroxide to di...

Embodiment 3

[0047] According to lithium ion, nickel ion, manganese ion, cobalt ion, reducing agent molar ratio is 1.6: 0.18: 0.77: 0.02: 0.77 respectively weighs lithium iodide, nickel nitrate, manganese oxalate, cobalt oxalate, titanium trichloride; Reactant The total volume is the sum of the volumes of lithium iodide, nickel nitrate, manganese oxalate and cobalt oxalate, and two parts of aqueous methanol (equivalent to (2·(1-x) y + 4 (x+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.

[0048] At 50°C, mix a measured portion of methanol aqueous solution with weighed nickel nitrate, manganese oxalate, and cobalt oxalate to obtain a mixed solution. Add weighed titanium trichloride to the mixed solution, and at the same time add a lye with a weight ratio of sodium hydroxide to deionized water of 1:5, and wet grind for 5 hours with a wet mill to prepare a reaction mixed solution containing precipitates. Wherein, alkali s...

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Abstract

The invention relates to a method for preparing a lithium-rich solid solution cathode material through reduction co-precipitation. The method comprises the following steps of: weighing lithium, nickel, manganese, cobalt and a reducing agent in a molar ratio of (1+x):(1-x).y:(x+z-x.z):(1-x).k:q; and mixing a measured wet grinding medium, the nickel, the manganese and the cobalt, adding the reducing agent, stirring, mixing, adding alkali liquor, performing wet grinding, aging, filtering, washing, adding the wet grinding medium and a lithium compound, performing wet grinding, drying to prepare a precursor, putting the precursor in air, oxygen-rich gas or pure oxygen atmosphere, and sintering to prepare the lithium-rich solid solution cathode material. The electrode material prepared by the method has uniform composition, high discharge performance, and high discharge cycle performance particularly under the high-current condition.

Description

technical field [0001] The invention belongs to the technical field of battery electrode material preparation, and specifically relates to a method for preparing a lithium-rich solid solution positive electrode material by a reduction co-precipitation method, which can be used for lithium batteries, lithium ion batteries, polymer batteries and supercapacitors. Background technique [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 high specific capacity, g...

Claims

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Application Information

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IPC IPC(8): H01M4/48H01G11/30
CPCY02E60/12Y02E60/10
Inventor 童庆松周惠王浪蔡斌李秀华黄能贵
Owner DYNABAT NEW ENERGY SCI & TECH CO CLD FUJIAN
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