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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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 wi

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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

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[0027] Example 1

[0028] Prepare an aqueous solution of ferrous sulfate with a concentration of 2.0 moles / liter, add 0.5 mole of sulfuric acid and 100 grams of urea per liter of solution, add the precipitant oxalic acid to the total metal ion molar ratio of 1.1:1, stir to dissolve the solids to make the system into a solution, pass The heating jacket heats the solution to control the reaction time. With the decomposition of urea, the hydrogen ions in the solution are consumed, the pH value of the solution gradually increases, 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 dried to obtain FeC 2 O 4 ·2H 2 O one yuan precursor. The precursor is added with a stoichiometric ratio of ammonium dihydrogen phosphate and lithium hydroxide, and ball milled and dried in an a...

Example Embodiment

[0029] Example 2

[0030] Prepare a mixed aqueous solution of manganese sulfate, ferrous sulfate, and cobalt sulfate, in which the total concentration of manganese sulfate, ferrous sulfate, and cobalt sulfate is 1.5 moles / liter, the molar ratio of the three is 5:4:1, and 2 moles are added per liter of solution Nitric acid and 80 grams of urea, add the precipitant ammonium oxalate to the total metal ion molar ratio of 3:1, stir the dissolved solids to make the system into a solution, heat the solution through a heating mantle, control the reaction time, as the urea decomposes Hydrogen ions are consumed, the pH value of the solution gradually increases, and the solubility of the precipitate gradually decreases and precipitates. Control the temperature in the reactor to 90°C. The reaction is stirred for 12 hours, filtered and washed until the sulfate radical in the washing water can not be detected with barium chloride, and dried to obtain Mn 0.5 Fe 0.4 Co 0.1 C 2 O 4 ·2H 2 O terna...

Example Embodiment

[0031] Example 3

[0032] Prepare a mixed aqueous solution of manganese sulfate, ferrous sulfate, nickel sulfate, and cobalt sulfate, wherein the total concentration of manganese sulfate, ferrous sulfate, nickel sulfate, and cobalt sulfate is 2 moles / liter, and the molar 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 of 2:1, stir the dissolved solids to make the system into a solution, heat the solution through a heating mantle, control the reaction time, With the decomposition of urea, hydrogen ions in the solution are consumed, the pH value of the solution gradually increases, and the solubility of the precipitate gradually decreases and precipitates. Control the temperature in the reactor to 150°C. The reaction is stirred for 10 hours, filtered and washed until the sulfate radical in the washing water can not be detected with barium chloride, and dr...

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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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