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Method for in-situ synthesis of carbon-coated lithium iron phosphate by microwave solvothermal

A carbon-coated lithium iron phosphate and microwave solvothermal technology, which is applied to electrical components, battery electrodes, circuits, etc., can solve the problems of easy agglomeration of lithium iron phosphate powder, difficulty in obtaining uniform size, long reaction cycle, etc., and achieve improved Effect of electrochemical performance, ensuring uniformity, and short reaction cycle

Inactive Publication Date: 2017-06-13
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

High-temperature solid-phase synthesis method is the most common method used in industrial production, but this method needs to be carried out at high temperature, the equipment investment is large, the energy consumption is high, and it is not environmentally friendly. Moreover, the prepared lithium iron phosphate powder is easy to agglomerate and difficult to obtain. Lithium iron phosphate powder with uniform size and regular shape
However, although the size and shape of the powder are easy to control and the phase is uniform in the hydrothermal synthesis of lithium iron phosphate, the reaction cycle is long and usually takes more than ten hours to complete.

Method used

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  • Method for in-situ synthesis of carbon-coated lithium iron phosphate by microwave solvothermal
  • Method for in-situ synthesis of carbon-coated lithium iron phosphate by microwave solvothermal
  • Method for in-situ synthesis of carbon-coated lithium iron phosphate by microwave solvothermal

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Experimental program
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Effect test

Embodiment 1

[0039] 0.01mol LiAc 2H 2 O and 0.01mol Fe(NO 3 ) 3 ·9H 2 O was dispersed in 70 mL of diethylene glycol, and after stirring evenly, 0.01 mol H was slowly added 3 PO 4 , and kept stirring, then 3 mL of ethylenediamine was added dropwise, and the precursor solution was obtained by stirring evenly. Take 40 mL of the precursor solution and put it into a 100 mL microwave reactor, react at 220 °C for 1 h, cool down to room temperature, wash the reaction solution with deionized water and ethanol for many times, and then dry it in a 100 °C oven to obtain the precursor. The precursor was placed in a reducing atmosphere (5vol.%H 2 and 95vol.% Ar) was heated to 700°C and calcined for 10h. Naturally cooled to room temperature with the furnace to obtain a carbon-coated three-dimensional bicontinuous structure LiFePO 4 / C.

[0040] The carbon-coated lithium iron phosphate prepared by the above method is subjected to powder X-ray diffraction, and its collection of illustrative plates ...

Embodiment 2

[0042] 0.005mol LiAc 2H 2 O and 0.005mol Fe(NO 3 )3 ·9H 2 O was dispersed in 70 mL of diethylene glycol, and after stirring evenly, 0.005 mol H was slowly added 3 PO 4 , and kept stirring, then 3 mL of ethylenediamine was added dropwise, and the precursor solution was obtained by stirring evenly. Take 35 mL of the precursor solution and put it into a 100 mL microwave reactor, react at 220 °C for 1 h, cool to room temperature, wash the reaction solution with deionized water and ethanol for many times, and then dry it in a 100 °C oven to obtain the precursor. The precursor was placed in a reducing atmosphere (5vol.%H 2 and 95vol.% Ar) was heated to 700°C and calcined for 10h. Naturally cooled to room temperature with the furnace to obtain a carbon-coated three-dimensional bicontinuous structure LiFePO 4 / C.

[0043] The scanning electron microscope (SEM) images of the as-prepared precursor (a) and the calcined product lithium iron phosphate (b) are as follows Figure 4 s...

Embodiment 3

[0045] 0.005mol LiAc 2H 2 O and 0.005mol Fe(NO 3 ) 3 ·9H 2 O was dispersed in 70 mL of diethylene glycol, and after stirring evenly, 0.005 mol H was slowly added 3 PO 4 , and kept stirring, then 3 mL of ethylenediamine was added dropwise, and the precursor solution was obtained by stirring evenly. Take 50 mL of the precursor solution and put it into a 100 mL microwave reactor, react at 220 °C for 20 min, cool down to room temperature, wash the reaction solution with deionized water and ethanol for many times, and then dry it in a 100 °C oven to obtain the precursor. The precursor was placed in a reducing atmosphere (5vol.%H 2 and 95vol.% Ar) was heated to 700°C and calcined for 10h. Naturally cooled to room temperature with the furnace to obtain a carbon-coated three-dimensional bicontinuous structure LiFePO 4 / C.

[0046] The scanning electron microscope (SEM) image of the as-prepared precursor is shown as Figure 5 shown. It can be seen from the figure that the pre...

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Abstract

The invention relates to a method for performing microwave solvothermal in-situ synthesis on carbon-coated lithium iron phosphate. The method comprises the following steps: dispersing a lithium source and an iron source in an alcohol reducing agent; adding a phosphorus source, stirring, adding a chelating agent, and stirring, thereby obtaining a precursor solution; adding part of the precursor solution into a microwave reactor, heating and reacting to obtain a product; washing the obtained product and drying, thereby obtaining a precursor; and calcining the precursor in a reducing atmosphere, thereby obtaining the product. The method disclosed by the invention has the beneficial effects that the time can be saved by virtue of in-situ carbon coating, and the uniformity of coated carbon can be ensured. Meanwhile, the conductivity of the lithium iron phosphate can be enhanced by virtue of the coated carbon, and the electrochemical performance is improved; the lithium iron phosphate is of a three-dimensional bi-continuous structure, nano-particles in the structure are connected with one another, a three-dimensional network is formed, the lithium-ion transmission distance is greatly shortened, and the electrochemical performance of the material is improved; the reaction period is short, and the process is simple; and the prepared lithium iron phosphate is high in specific capacity, good in cycle performance, high in repeatability and excellent in processability.

Description

technical field [0001] The invention belongs to the technical field of energy material manufacturing, and particularly relates to a method for in-situ synthesis of carbon-coated lithium iron phosphate by microwave solvothermal. Background technique [0002] As a high-performance rechargeable green power source, lithium-ion battery has been widely used in various portable electronic products and communication tools in recent years, and has been gradually developed as a power source for electric vehicles. In the research of lithium ion batteries, the research and development of new electrode materials, especially cathode materials, is extremely critical. [0003] Among the widely studied cathode materials for lithium-ion batteries, LiFePO 4 It has the advantages of low price, good safety performance and thermal stability, no pollution and high mass specific energy, and is a potential cathode material for lithium ion batteries. However, the low electronic conductivity (ca.10 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M4/136
CPCH01M4/136H01M4/5825H01M4/625Y02E60/10
Inventor 李昱张倩许骏蒙黄绍专王洪恩陈丽华苏宝连
Owner WUHAN UNIV OF TECH