Preparation method for metal-doped lithium/carbon manganese phosphate composite from manganese phosphate

A carbon composite material, lithium manganese phosphate technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of difficult to improve and solve the yield, difficult to ensure the stability of product batches, poor material conductivity, etc., to reduce Effects of natural cooling time, improved electrochemical performance, and improved batch performance

Inactive Publication Date: 2013-12-25
ZHEJIANG WELLY ENERGY CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
In the public documents of many patent applications for lithium manganese iron phosphate / carbon composite materials, the electrochemical performance of the material is improved by carbon coating and metal doping, and a relatively ideal capacity is obtained, but the preparation methods are relatively cumbersome, making it The difficulty of industrialization is high, and it increases the cost and it is difficult to guarantee the batch stability of the product, making it more difficult to improve the yield in the battery factory and solve the problem

Method used

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  • Preparation method for metal-doped lithium/carbon manganese phosphate composite from manganese phosphate
  • Preparation method for metal-doped lithium/carbon manganese phosphate composite from manganese phosphate
  • Preparation method for metal-doped lithium/carbon manganese phosphate composite from manganese phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Embodiment 1, under room temperature, get manganese sulfate 82.82g, the solution that concentration is 1mol / L (99.5% of industrial high purity) and phosphoric acid 57.62g (AR) are made into the solution of 500ml, after stirring evenly, add oxidant hydrogen peroxide 50ml (excessive ), oxidize divalent manganese to trivalent manganese, the color of the solution becomes darker, continue to stir for 2 hours under rapid stirring at 500-100r / min, then heat to 50°C, and adjust the pH value with 1mol / L ammonium bicarbonate solution , The feeding rate is 500ml / h. Use a pH instrument to control the pH value to 5.5, then continue to stir and keep warm for 2 hours, then filter, beat and wash for 3 times, wait until the filtrate is added with BaCl2 without white precipitation, and finally adjust to 60°C in a vacuum oven and dry for 24 hours. The manganese phosphate precursor material is obtained by pulverization and classification, and its electron microscope SEM sees figure 1 .

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example 2

[0043] Example 2, at room temperature, get manganese sulfate 82.82g, concentration is 1mol / L solution (industrial high purity 99.5%) and phosphoric acid 57.62g (AR) are respectively made into 500ml solution, mixes 200ml deionized water bottom liquid, adds oxidizing agent Hydrogen peroxide 50ml (excess). Manganese sulfate solution, phosphoric acid solution and 1mol / L ammonia solution were added dropwise in parallel to adjust the pH value, and the feeding rate was 50ml / h. Use a pH instrument to control the pH value from 4.5 to 5.5, then continue to stir and keep warm for 2 hours, then filter, beat and wash for 3 times, wait until the filtrate is added with BaCl2 without white precipitation, and finally adjust to 60°C in a vacuum oven and dry for 24 hours. Finally, the manganese phosphate precursor material is obtained by crushing and grading, and its electron microscope SEM sees Figure 5 .

[0044] Manganese phosphate 100g (self-made), lithium carbonate 24.76g (battery grade ...

example 3

[0045] Example 3, at room temperature, get manganese acetate 123.78g, concentration is 1mol / L solution (99.5% of industrial high purity) and phosphoric acid 57.62g (AR) and is made into 500ml solution, after stirring evenly, add oxidant hydrogen peroxide 50ml (excessive) , oxidize divalent manganese to trivalent manganese, the color of the solution becomes darker, continue to stir for 2 hours, then heat to 50°C, continue to stir and react for 2 hours, then add polyethylene glycol (PEG) 1000, heat to 80 ℃ to continue to react for 2 hours, and finally evaporate to jelly, put it in a vacuum oven at 60 ℃ and dry for 24 hours, and finally pulverize and classify to obtain the manganese phosphate precursor material. Its electron microscope SEM sees Figure 7

[0046]Manganese phosphate 100g (self-made) prepared above, lithium carbonate 24.76g (battery grade 99.5%), magnesium hydroxide 0.757g (nano-grade), glucose 11.67g (food grade 99.5%), use 150ml absolute ethanol as dispersant ,...

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Abstract

The invention discloses a preparation method for a metal-doped lithium / carbon manganese phosphate (LiMXMn1-XPO4 / C) composite from manganese phosphate. The method comprises the following steps: preparing active manganese phosphate materials (MnPO4) with different shapes by using a precipitation or sol-gel method; then subjecting prepared manganese phosphate, a lithium source and a metal-doped elemental compound to ball milling for 20 to 50 h and mixing with alcohol used as a dispersant; carrying out vacuum drying and crushing to obtain a crushed substance; placing the crushed substance in a stainless steel container, heating the crushed substance to a temperature of 450 to 800 DEG C in a furnace protected by an inert atmosphere and maintaining the temperature for 2 to 12 h; and rapidly placing the substance to a liquid coolant under the conditions of a high temperature and air isolation and carrying out rapid cooling so as to obtain the LiMXMn1-XPO4 / C composite. The method provided by the invention has shortened process flow, can maintain particle activity in a high temperature, effectively gives rise to structural dislocation, improves the ionic migration rate and electronic conductivity of the composite and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of energy materials, and discloses a method for preparing metal-doped lithium manganese phosphate / carbon LiM with manganese phosphate X mn 1-X PO 4 / C composite material method, especially one adopts precipitation method and sol-gel method to control crystallization to prepare manganese phosphate precursor primary ion and ion activity, ball mill mixing, controlled calcination, and rapid cooling method to prepare metal-doped manganese phosphate Lithium / carbon LiM X mn 1-X PO 4 / C composite method. Background technique [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 ...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 吴清国王飞高璐璐
Owner ZHEJIANG WELLY ENERGY CORP
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