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

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
In the public documents of many patent applications for lithium manganese iron phosphate/carbon composite materials, the electrochemical performance of the

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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Example Embodiment

[0041] Example 1, at room temperature, take 82.82g of manganese sulfate, a solution of 1mol / L (industrial high purity 99.5%) and 57.62g of phosphoric acid (AR) to make a 500ml solution. After stirring, add 50ml of oxidant hydrogen peroxide (excess ), the divalent manganese is oxidized to trivalent manganese, the color of the solution becomes darker, and the stirring is continued for 2 hours under rapid stirring at 500-100r / min, and then heated to 50°C, and the pH value is adjusted with 1mol / L ammonium bicarbonate solution , The feeding speed is 500ml / h. Use a pH instrument to control the pH value to 5.5, then continue to stir and keep for 2 hours, then filter, beat and wash 3 times, wait until the filtrate is added with BaCl2 without white precipitation, and finally adjust to 60 ℃ in a vacuum oven to dry for 24 hours, and finally The manganese phosphate precursor material is obtained by crushing and classification. figure 1 .

[0042] 100g of manganese phosphate (homemade), 24.7...

Example Embodiment

[0043] Example 2: At room temperature, take 82.82g of manganese sulfate and a concentration of 1mol / L solution (industrial high purity 99.5%) and 57.62g of phosphoric acid (AR) to make 500ml solution, 200ml of deionized water bottom solution, add oxidant 50ml of hydrogen peroxide (excess). Simultaneously, manganese sulfate solution, phosphoric acid solution and 1mol / L ammonia solution were added dropwise 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 for 2 hours, then filter, beating and washing 3 times, wait until the filtrate is added with BaCl2 without white precipitation, and finally adjust to 60 ℃ in a vacuum oven and dry for 24 hours. Finally, the manganese phosphate precursor material is obtained by crushing and grading. The electron microscope SEM sees Figure 5 .

[0044] 100g of manganese phosphate (homemade), 24.76g of lithium carbonate (99.5% of battery grade), 0.757...

Example Embodiment

[0045] Example 3, at room temperature, take 123.78g of manganese acetate with a concentration of 1mol / L (industrial high purity 99.5%) and 57.62g of phosphoric acid (AR) to make a 500ml solution. After stirring, add 50ml of oxidant hydrogen peroxide (excess) , The divalent manganese is oxidized to trivalent manganese, the color of the solution becomes darker, continue to stir for 2 hours, then heat to 50 ℃, continue to stir and react for 2 hours, then add polyethylene glycol (PEG) 1000, and heat to 80 Continue the reaction at ℃ for 2 hours, and finally evaporate to a jelly, put it in a vacuum oven at 60 ℃ and dry for 24 hours, and finally crush and classify to obtain the manganese phosphate precursor material. See the electron microscope SEM Figure 7

[0046] 100g of manganese phosphate prepared above (homemade), 24.76g of lithium carbonate (99.5% of battery grade), 0.757g of magnesium hydroxide (nano grade), 11.67g of glucose (99.5% of food grade), 150ml of absolute ethanol as ...

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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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