Preparation method of compound phosphate-series positive electrode material for lithium-ion battery

A lithium-ion battery and composite phosphate technology, which is applied to battery electrodes, secondary batteries, circuits, etc., can solve the problem of uneven mixing of precipitant and salt solution, different thickness of precipitated particles, single-element or multi-element composite phosphate lithium ion Poor battery cathode material performance and other issues, to achieve good cycle performance, good batch, and good consistency

Inactive Publication Date: 2016-07-27
WUXI JIABANG ELECTRIC POWER PIPE FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the method described in this application, uneven mixing of the precipitating agent and the salt solution and uneven thickness of the precipitated particles are likely to occur, which is not conducive to obtaining a precursor with a stable composition ratio, uniform particle size distribution, and good consistency, and ultimately leads to the synthesis of mono- or Poor performance of cathode materials for multi-component composite phosphate lithium-ion batteries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Prepare a mixed solution of ferrous sulfate, cobalt sulfate and manganese sulfate, the total concentration is 2.0 mol / liter, the molar ratio of the three is 5:4:1, add 2 moles of sulfuric acid and 80 grams of urea per liter of solution, add a precipitant The molar ratio of oxalic acid to total metal ions is 1.1:1. Stir to dissolve the solids to make the system into a solution. Heat the solution through the heating mantle to control the reaction time. With the decomposition of urea, the hydrogen ions in the solution are consumed, and the pH value of the solution gradually increases. , the solubility of the precipitate gradually decreased and precipitated. The temperature in the reactor is 120°C, the reaction is stirred for 14 hours, filtered and washed until the sulfate radical in the washing water cannot be detected with barium chloride, and dried to obtain Mn 0.1 co 0.4 Fe 0.5 C 2 o 4 2H 2O Ternary precursor. The precursor was added stoichiometric ratio of ammoni...

Embodiment 2

[0028] Prepare manganese sulfate, ferrous sulfate, nickel sulfate, cobalt sulfate mixed aqueous solution, wherein the total concentration of manganese sulfate, ferrous sulfate, nickel sulfate, cobalt sulfate is 0.1 mol / liter, and the mol ratio of the four is 1:1:1: 1. Add 0.1 mole of hydrochloric acid and 40 grams of urea per liter of solution, add the precipitant oxalic acid to the total metal ion molar ratio of 0.8:1, stir and dissolve the solid to make the system into a solution, heat the solution through the heating mantle, control the reaction time, and With the decomposition of urea, the hydrogen ions in the solution are consumed, the pH value of the solution increases gradually, and the solubility of the precipitate gradually decreases and precipitates. The temperature inside the reactor was controlled to be 150°C. The reaction was stirred for 10 hours, filtered and washed until the sulfate radical in the washing water could not be detected with barium chloride, and dri...

Embodiment 3

[0030] Prepare manganese sulfate, ferrous sulfate, nickel sulfate, cobalt sulfate mixed aqueous solution, wherein the total concentration of manganese sulfate, ferrous sulfate, nickel sulfate, cobalt sulfate is 3 mol / liter, and the mol ratio of four is 1:1:1: 1. Add 5 moles of hydrochloric acid and 300 grams of urea per liter of solution, add the precipitant oxalic acid to the total metal ion molar ratio of 1.5:1, stir and dissolve the solid to make the system into a solution, heat the solution through the heating mantle, control the reaction time, and With the decomposition of urea, the hydrogen ions in the solution are consumed, the pH value of the solution increases gradually, and the solubility of the precipitate gradually decreases and precipitates. The temperature in the reactor was controlled to be 100°C. The reaction was stirred for 30 hours, filtered and washed until the sulfate group in the washing water could not be detected with barium chloride, and dried to obtain...

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Abstract

The invention relates to a preparation method of a compound phosphate-series positive electrode material for a lithium-ion battery. The method comprises the following steps: preparing a solution from a soluble bivalent iron salt and a soluble transition metal nickel salt, cobalt salt or manganese salt, and then adding an acid and urea to prepare a mixed solution; adding a precipitant to the mixed solution for reaction and preparing a mixed oxalate precursor; and carrying out ball-mill mixing on the precursor, a lithium source and a phosphorus source evenly and preparing the compound phosphate-series positive electrode material for the lithium-ion battery in an inert or weak reductive atmosphere. The used aqueous urea solution is slowly hydrolyzed under the acid, alkali and urease catalysis or heating conditions. The urea hydrolysis rate is low and the hydrolysis product is simple and easy to volatilize, so that the aqueous urea solution can be applied to homogeneous precipitation of elements and ions. The first charge and discharge specific capacity of the obtained product at a room temperature and 0.1C rate can reach about 160mAh/g; and the compound phosphate-series positive electrode material is good in cycle performance and charge and discharge performance.

Description

technical field [0001] The invention relates to a preparation method of a composite phosphate series lithium ion battery cathode material which is doped with metal ions by a co-precipitation method, and belongs to the technical field of material preparation. Background technique [0002] In recent years, the research and development of lithium-ion batteries have made gratifying achievements, especially the improvement of the performance of the negative electrode and the development of the electrolyte system have achieved great results, but the research on the cathode materials of lithium-ion batteries appears to be relatively lagging behind, which has become a constraint for lithium-ion batteries. The bottleneck of battery market and application expansion. Lithium cobalt oxide, lithium nickel oxide, lithium nickel cobalt composite oxide, lithium manganese oxide, lithium vanadate and other positive electrode materials have always been a hot spot in the field of positive elect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/139H01M10/0525
CPCH01M4/139H01M4/5825H01M10/0525Y02E60/10
Inventor 徐德生
Owner WUXI JIABANG ELECTRIC POWER PIPE FACTORY
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