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Method for preparing manganese phosphate lithium / carbon composite material

A technology of carbon composite materials and lithium manganese iron phosphate, which is applied in the field of materials science, can solve the problems of difficulty in improving and solving the yield rate of battery factories, difficulty in ensuring product batches, and difficulty in industrialization, and achieve good cycle stability. , reduce equipment investment and production costs, and shorten working hours

Inactive Publication Date: 2012-11-07
ZHEJIANG WELLY ENERGY CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since LiMnPO 4 The material is extremely poorly conductive and is considered an insulator, leading to the synthesis of LiMnPO capable of reversible charge and discharge 4 Very difficult, which limits its development and application
[0004] In many patent application numbers of lithium manganese iron phosphate / carbon composite materials, the electrochemical performance of the material is improved through carbon coating and metal doping, and a relatively ideal capacity is obtained, but the preparation methods are relatively cumbersome, and most of them are two Secondary mixing or secondary calcination greatly lengthens the process flow, increases the difficulty of its industrialization, increases the cost and makes it difficult to guarantee the batch nature of the product, making it more difficult to improve and solve the problem in the battery factory.

Method used

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  • Method for preparing manganese phosphate lithium / carbon composite material
  • Method for preparing manganese phosphate lithium / carbon composite material
  • Method for preparing manganese phosphate lithium / carbon composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] At room temperature, take lithium carbonate 16.3284g (battery grade 99.5%), glucose powder 19.7562g (food grade), manganese monoxide 24.0000g (high purity), ammonium dihydrogen phosphate 51.1024g (food grade), ferrous oxalate 15.1390 g (battery grade), 1.3501g of magnesium hydroxide (nano-grade), 150ml of absolute ethanol as a dispersant, added to a 500ml stainless steel ball mill tank, added 200g of zirconium balls, and ball milled at a speed of 300r / min for 4 Hours, then dry in a protective oven with 99.99% nitrogen at a drying temperature of 60-80°C. After drying, use a high-speed pulverizer to pulverize it, and then place it in a tube furnace with 99.99% nitrogen as the sintering atmosphere , the gas flow rate is 6L / min, and the furnace temperature is raised to 660°C at a heating rate of 3°C / min, and then sintered at 660°C for 6 hours. After cooling to room temperature, it passes through a 300 mesh screen to obtain lithium manganese phosphate Carbon composite materi...

Embodiment 2

[0023] At room temperature, take lithium carbonate 16.3284g (battery grade 99.5%), glucose powder 9.8780g (food grade), manganese monoxide 24.0000g (high purity), ammonium dihydrogen phosphate 51.1024g (food grade), ferrous oxalate 15.1390 g (battery grade), 1.3501g of magnesium hydroxide (nano-grade), 150ml of absolute ethanol as a dispersant, added to a 500ml stainless steel ball mill tank, added 200g of zirconium balls, and ball milled at a speed of 300r / min for 4 Hours, then dry in a protective oven with 99.99% nitrogen at a drying temperature of 60-80°C. After drying, use a high-speed pulverizer to pulverize it, and then place it in a tube furnace with 99.99% nitrogen as the sintering atmosphere , the gas flow rate is 6L / min, and the furnace temperature is raised to 550°C at a heating rate of 3°C / min, and then sintered at 660°C for 6 hours. After cooling to room temperature, it passes through a 300-mesh screen to obtain lithium iron manganese phosphate Carbon composite ma...

Embodiment 3

[0025] At room temperature, take lithium carbonate 16.3284g (battery grade 99.5%), glucose powder 9.8780g (food grade), manganese monoxide 26.0000g (high purity), ammonium dihydrogen phosphate 51.1024g (food grade), ferrous oxalate 10.0920 g (battery grade), 1.3501g of magnesium hydroxide (nano-grade), 150ml of absolute ethanol as a dispersant, added to a 500ml stainless steel ball mill tank, added 200g of zirconium balls, and ball milled at a speed of 300r / min for 4 Hours, then dry in a protective oven with 99.99% nitrogen at a drying temperature of 60-80°C. After drying, use a high-speed pulverizer to pulverize it, and then place it in a tube furnace with 99.99% nitrogen as the sintering atmosphere , the gas flow rate is 6L / min, and the furnace temperature is raised to 550°C at a heating rate of 3°C / min, and then sintered at 660°C for 6 hours. After cooling to room temperature, it passes through a 300-mesh screen to obtain lithium iron manganese phosphate Carbon composite ma...

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Abstract

The invention discloses a solid-liquid combined method for preparing a manganese phosphate lithium / carbon composite material. According to the method, raw materials comprising ammonium dihydrogen phosphate, a lithium source, a manganese source, an iron source, a carbon source and metal doped elements are mixed, dried, heated to 450-700 DEG C under atmosphere conditions, dried for 1-12 h at the constant temperature, and cooled to obtain the manganese phosphate lithium / carbon composite material. The invention adopts a principle of solid-liquid combination, effectively improves uniformity of material mixing, and facilitates improvement on stability and degree of crystallinity of the product. The composite material synthesized by the method is uniformly dispersed, and has effectively improved electronic conductivity. One-time calcination adopted by the invention can effectively reduce energy consumption; and the obtained composite material has particle size distribution of 1-20 mum, and 0.1C rate discharge capacity of 142mAh / g; and electrochemical tests show that the electrode has obvious discharge platform at about 4V, high discharge capacity and good cycle stability.

Description

technical field [0001] The invention belongs to the field of materials science, and in particular relates to a preparation method of lithium iron manganese phosphate / carbon composite material. Background of the invention [0002] The development of lithium-ion secondary batteries has a history of 20 years. So far, the transition metal oxides that can form intercalated compounds with lithium are the most researched. In the past two decades, people have found six practical positive electrode active materials through the research on lithium-ion secondary battery electrode materials: lithium cobaltate (LiCoO 2 ), lithium nickelate (LiNiO 2 ), lithium manganate (LiMn 2 o 4 ), lithium vanadate (Li 1+x V 3 o 8 ), lithium vanadium phosphate (Li 3 V 2 (PO 4 ) 3 ) and lithium iron phosphate (LiFePO 4 ) and various doping compounds derived from them. LiCoO 2 It is highly toxic and expensive, and it is difficult to guarantee the safety when making large-scale power batterie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12Y02E60/10
Inventor 吴清国王飞吴奎辰赵留涛徐中领高璐璐
Owner ZHEJIANG WELLY ENERGY CORP
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