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Method for preparing phosphate series lithium ion battery anode material

A technology for lithium-ion batteries and positive electrode materials, which is applied in battery electrodes, circuits, electrical components, etc., and can solve the problem of poor performance of positive electrode materials of one-element or multi-element composite phosphate lithium-ion batteries, and uniform particle size distribution of precursors and precipitants. Mix unevenly with salt solution and other problems to achieve the effect of avoiding uneven mixing, good batch performance and good consistency

Active Publication Date: 2011-06-08
襄阳泽东新能源发展有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] However, in the above-mentioned several technologies, uneven mixing of the precipitant and the salt solution, and uneven thickness of the precipitated particles are prone to occur, which is not conducive to obtaining a precursor with a stable composition ratio, uniform particle size distribution, and good consistency, and eventually 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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  • Method for preparing phosphate series lithium ion battery anode material
  • Method for preparing phosphate series lithium ion battery anode material
  • Method for preparing phosphate series lithium ion battery anode material

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Prepare ferrous sulfate aqueous solution, concentration is 2.0 mol / liter, every liter of solution adds 0.5 mole of sulfuric acid and 100 grams of urea, adds precipitating agent oxalic acid and total metal ion molar ratio is 1.1: 1, stirs and dissolves solid to make system into solution, passes The heating mantle heats the solution and controls the reaction time. 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 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 then dried to obtain FeC 2 o 4 2H 2 O unary precursor. The precursor was added stoichiometric ratio of ammonium dihydrogen phosphate and lithium hydroxide, and the sample was obtained by ball milling and drying in aceton...

Embodiment 2

[0030]Prepare manganese sulfate, ferrous sulfate, cobalt sulfate mixed aqueous solution, wherein the total concentration of manganese sulfate, ferrous sulfate, cobalt sulfate is 1.5 mol / liter, the molar ratio of the three is 5:4:1, every liter of solution is added 2 moles nitric acid and 80 grams of urea, adding precipitant ammonium oxalate and the total metal ion molar ratio is 3: 1, stirring and dissolving the solid to make the system into a solution, heating the solution through a heating mantle, controlling the reaction time, along with the decomposition of urea, the solution will The hydrogen ions are consumed, the pH value of the solution increases gradually, and the solubility of the precipitate decreases gradually. The temperature inside the reactor was controlled to be 90°C. The reaction was stirred for 12 hours, filtered and washed until the sulfate radical in the washing water could not be detected with barium chloride, and dried to obtain Mn 0.5 Fe 0.4 co 0.1 C ...

Embodiment 3

[0032] 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 2 mol / liter, and the mol ratio of the four is 1: 1: 1: 1. Add 3 moles of hydrochloric acid and 60 grams of urea per liter of solution, add the precipitant oxalic acid and the total metal ion molar ratio is 2:1, 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 dried...

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Abstract

The invention relates to a method for preparing a phosphate series lithium ion battery anode material, comprising the following steps: preparing one or more of divalent manganese source compound, ferrum source compound, nickel source compound or cobalt source compound into a mixed solution; adding oxalic acid or oxalate, acid and urea, and slowly hydrolyzing the urea by controlling the reaction temperature and time; causing the pH value of the system to rise to reach the condition of homogeneous precipitation; after the reaction, filtering, washing and drying to obtain a precursor; evenly mixing and carrying out ball milling on the precursor, a lithium source and a phosphorous source; and calcining the mixture under the non-oxidability atmosphere to prepare the unitary or multielement phosphate series lithium ion battery anode material. The precursor prepared with the method has the advantages of stable ingredient proportion, even granularity distribution, good consistency and simple synthetic technology, does not need to consider the influence of flow rate and agitation and is suitable for industrial production. The synthesized battery anode material is the phosphate compound with an olivine structure, the average grain size of the primary particle is 100-500nm, and the battery anode material has good electrochemistry property.

Description

technical field [0001] The invention belongs to the technical field of new energy materials, and relates to a method for synthesizing a one-component or multiple-component composite precursor by using a uniform co-precipitation method to prepare a positive electrode material for a phosphate lithium ion battery. Background technique [0002] Lithium-ion batteries are the most dynamic in the current secondary battery market due to their high operating voltage, high energy density, long cycle life, low self-discharge rate, and environmental protection. Lithium iron phosphate cathode material has the advantages of low cost, good stability and good safety performance, but its discharge voltage platform is low, around 3.4V, and its energy density is low. while Mn 3+ / Mn 2+ The electrode potential is 4.1V (vs.Li + / Li), Co 3+ / Co 2+ The electrode potential is 4.8V (vs.Li + / Li), Ni 3+ / Ni 2+ The electrode potential is 5.07V (vs.Li + / Li), the discharge platform of its synt...

Claims

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Application Information

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IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 杜柯张罗虎胡国荣彭忠东曹雁冰郭宏伟
Owner 襄阳泽东新能源发展有限公司
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