Method for preparing lithium iron phosphate material by raw material solid phase dry grinding

A technology of lithium iron phosphate and raw materials, which is applied in the field of lithium battery material preparation, can solve the problems of uneven physical and chemical composition of products, irregular shape of precursors, wide particle size distribution, etc., and achieve excellent quality stability and consistency , the effect of uniform particle size

Inactive Publication Date: 2013-01-02
JIANGSU FREY NEW ENERGY
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Problems solved by technology

To solve the problems of irregular precursor shape, wide particle size distribution, uneven physical and chemica

Method used

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  • Method for preparing lithium iron phosphate material by raw material solid phase dry grinding
  • Method for preparing lithium iron phosphate material by raw material solid phase dry grinding
  • Method for preparing lithium iron phosphate material by raw material solid phase dry grinding

Examples

Experimental program
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Example Embodiment

[0019] Embodiment 1,

[0020] Using lithium dihydrogen phosphate and ferrous oxalate with a molar ratio of 1:1 as raw materials, the lithium dihydrogen phosphate is pulverized through disc milling and jet pulverization technology, and the pulverization pressure is adjusted to 10KG, so that the particle size and the ferrous oxalate are 10kg. The medium particle size is the same, both are less than 5um, put the two raw materials into a ball mill, the ratio of raw materials and zirconium balls is 1:5, ball mill for 2 hours, put in a tube furnace, at room temperature, pass nitrogen as a protective gas , the heating rate is 5 °C / min, the temperature is raised to 350 °C, and the temperature is kept for 10 hours. After taking it out, it is mixed with sucrose. The weight of the sucrose is 5% of the total amount of raw materials added. At room temperature, nitrogen was introduced as a protective gas, the heating rate was 5 °C / min, the temperature was raised to 850 °C, and the temperatu...

Example Embodiment

[0021] Embodiment 2,

[0022] Using lithium dihydrogen phosphate and ferrous oxalate with a molar ratio of 1:1 as raw materials, the median particle size of lithium dihydrogen phosphate is 408.5um, and the median particle size of ferrous oxalate is 5um. Put it in a ball mill, the ratio of raw materials and zirconium balls is 1:5, ball milled for 2 hours, placed in a tube furnace, at room temperature, nitrogen is introduced as a protective gas, the heating rate is 5 °C / min, and the temperature is raised to 350 °C , kept for 10h, mixed with sucrose after taking out, the weight of sucrose was 5% of the total amount of raw materials added, put it in a ball mill for 2 hours, and then placed it in a tube furnace, and at room temperature, nitrogen was introduced as protective gas, The heating rate was 5 °C / min, the temperature was raised to 850 °C, and the temperature was kept for 22 hours. After taking out, the particle size was 1um, and the prepared lithium iron phosphate cathode m...

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Abstract

The invention relates to a raw material solid phase dry grinding technology, in particular to a method for preparing a lithium iron phosphate material by raw material solid phase dry grinding, and belongs to the field of preparation of a lithium battery material. According to the method, a novel high temperature solid phase dry closed-loop grinding system combining an ultrafine grinding technology with an air classification technology is adopted; raw materials of a lithium iron phosphate cathode material are subjected to nano-scale grinding and mixingl and the raw materials are sintered to obtain the nano-scale lithium iron phosphate cathode material. The invention aims to solve the problems of irregular morphology of a precursor, wide particle size distribution and nonuniform physical and chemical composition of a product, which are caused by large particle size, wide distribution and nonuniform mixing of the raw materials. The invention overcomes the defects of pollution of ammonia and an organic solvent to the environment and energy consumption, which is caused by the wet grinding material drying, in the conventional high temperature solid phase production. Moreover, in the production process, only harmless gases such as CO2, water and the like are discharged; and a lithium iron phosphate green environmental-friendly production process is really implemented.

Description

technical field [0001] The invention relates to a raw material solid phase dry pulverization technology, in particular to a method for preparing a lithium iron phosphate material by pulverizing a raw material solid phase dry method, and belongs to the field of lithium battery material preparation. Background technique [0002] At present, the production methods of lithium iron phosphate at home and abroad mainly include solid phase method and liquid phase method. The solid phase method includes high temperature solid phase method, carbothermal reduction method, microwave synthesis method and pulse laser precipitation method; Gel synthesis, hydrothermal synthesis, precipitation and solvent synthesis. ①High temperature solid phase method: Usually iron salts, lithium compounds and ammonium phosphate are used as raw materials. After fully mixing according to the stoichiometric ratio, they are first treated at low temperature for 5-10 hours under the protection of inert gas to fu...

Claims

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Application Information

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IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/12Y02E60/10
Inventor 石红霞王延延
Owner JIANGSU FREY NEW ENERGY
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