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Preparation method of low iron content ternary precursor

A technology of iron content and precursor, applied in the field of preparation of ternary precursors, can solve the problems of battery capacity loss, battery flatulence, large self-discharge, etc., and achieve the effects of improving sphericity, increasing tap density, and reducing iron content

Active Publication Date: 2014-01-29
河南科隆电源材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of Fe in the material is too high, because of the mutual conversion between different ion valence states, it will produce a large self-discharge phenomenon, resulting in the loss of battery capacity
The existence of Fe elemental substance will also cause micro-short circuit of the battery, cause battery flatulence, and even cause explosion in severe cases

Method used

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  • Preparation method of low iron content ternary precursor
  • Preparation method of low iron content ternary precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Experimental conditions: temperature 30°C, nitrogen flow rate 0.5L / min, stirring speed 700r / min, pH value 12.50, reactor 10L, mechanical stirring.

[0016] Solution preparation:

[0017] 1. Prepare a mixed solution of nickel sulfate, cobalt sulfate, and manganese sulfate with a value of 0.1mol / L. The ratio of nickel, cobalt, and manganese is 5:2:3.

[0018] 2. Bottom liquid solution preparation: prepare a solution with an ammonia concentration of 0.5mol / L.

[0019] 3. Washing solution preparation: add NaOH solution to pure water to adjust the pH to about 12.0. For washing hydroxide precipitates.

[0020] Take 5L of the prepared bottom liquid and add it to the reaction kettle, start stirring, turn on the circulation heating system to heat, when the temperature rises to 30°C, inject three kinds of reaction liquids into the reaction kettle through the metering pump, the flow rate of the nickel-cobalt-manganese mixture is 5ml / min. The pH was stabilized at 7.0 by contro...

Embodiment 2

[0022] Experimental conditions: temperature 60°C, nitrogen flow rate 0.7L / min, stirring speed 1000r / min, pH value 8.0, reactor 10L, mechanical stirring.

[0023] Solution preparation:

[0024] 1. Using BiNO 3 , NH 3 Preparation of Bi(OH) from water and glycerol 3 , dried at 500–700°C to make Bi 2 o 3 .

[0025] Add Bi to the KOH solution 2 o 3 , lye and Bi 2 o 3 The ratio is 50~100:1, stir for 10~60min, and filter to get the spare lye. The lye used in the test is the treated KOH solution.

[0026] 2. Prepare a mixed solution of nickel chloride, cobalt chloride, and manganese chloride with a value of 3.0mol / L. The ratio of nickel, cobalt, and manganese is 1:1:1.

[0027] 3. Bottom liquid solution preparation: Prepare a solution with an ammonia concentration of 1.0 mol / L.

[0028] 4. Washing solution preparation: add KOH solution to pure water to adjust the pH to about 12.5. For washing hydroxide precipitates.

[0029] Take 5L of the prepared bottom liquid and add ...

Embodiment 3

[0031] Experimental conditions: temperature 80°C, nitrogen flow rate 0.7L / min, stirring speed 1500r / min, pH value 8.0, reactor 10L, mechanical stirring.

[0032] Solution preparation:

[0033] 1. Use MgSO 4 Prepare Mg(OH) with NaOH (both are of superior grade) 2 Precipitate, dry to semi-dry, add NaOH solution, stir for 10-60min, filter to obtain standby lye, the NaOH solution used in the experiment is the treated lye.

[0034] 2. Prepare a mixed solution of nickel nitrate, cobalt nitrate, and manganese nitrate with a value of 4.0mol / L, and the ratio of nickel, cobalt, and manganese is 1:1:1.

[0035] 3. Bottom liquid solution preparation: prepare a solution with an ammonia concentration of 2.0 mol / L.

[0036] 4. Washing solution preparation: Add liquid caustic soda to pure water to adjust the pH to about 12.0. For washing hydroxide precipitates.

[0037] Take 5L of the prepared bottom liquid and add it to the reaction kettle, start stirring, turn on the circulation heatin...

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Abstract

The invention relates to a preparation method of a low iron content ternary precursor. The preparation method comprises the following steps of: continuously adding a nickel salt, a cobalt salt, a manganese salt, a basic water solution and an NH3 complexing agent into a synthetic reaction kettle, and stirring continuously; synthesizing a spherical ternary positive electrode material precursor by adopting a controlled crystallization method and stabilizing the technological parameters, wherein the chemical formula of the precursor is NixCoyMnz(OH)2, x is more than or equal to 0.5 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.5, and x+y+z=1; washing and drying to obtain the ternary positive electrode material precursor. According to the preparation method, an iron remover is added in the basic solution, so that the content of impurity iron in the ternary positive electrode material precursor finished product is reduced greatly, and the safety and physical and chemical properties of the material are improved.

Description

technical field [0001] The invention relates to a lithium ion battery, in particular to a method for preparing a ternary precursor with low iron content for making the positive electrode material of the lithium ion battery. Background technique [0002] At present, lithium-ion battery cathode materials mainly include four series of lithium cobaltate, lithium nickelate, lithium manganate and lithium iron phosphate. Lithium cobaltate is still the mainstream in the market, but cobalt resources are limited, expensive, toxic and safe. Poor shortcomings limit its large-scale application in the future; the actual capacity of lithium nickelate is higher than that of lithium cobaltate, and the price of Ni is cheaper than cobalt, but lithium nickelate is difficult to prepare and has poor thermal stability; lithium manganate has abundant raw materials and low price. , environmental friendliness, and good thermal stability, but lithium manganate has low capacity and poor cycle performan...

Claims

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Application Information

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IPC IPC(8): H01M4/50H01M4/52
CPCH01M4/50H01M4/52H01M4/628Y02E60/10
Inventor 吕志杰王丛
Owner 河南科隆电源材料有限公司