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Solvothermal assisted preparation method of LiFePO4/C multistage composite microspheres

A composite microsphere, solvothermal technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low electronic and ionic conductivity, achieve excellent electrochemical lithium storage performance, and achieve the effect of large-scale commercial production

Inactive Publication Date: 2017-05-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

around LiFePO 4 The existing problem of low electronic and ionic conductivity, several modification measures such as surface coating, bulk phase doping and morphology control have been developed and reported, and some of them have achieved industrial improvement, but LiFePO 4 The large-scale production still needs to be further improved, and there is still a lot of room for improvement in performance, especially in terms of power and energy density, which is particularly important for the storage of renewable clean energy and the development of power vehicles

Method used

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  • Solvothermal assisted preparation method of LiFePO4/C multistage composite microspheres
  • Solvothermal assisted preparation method of LiFePO4/C multistage composite microspheres
  • Solvothermal assisted preparation method of LiFePO4/C multistage composite microspheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) 1.153g H 3 PO 4 Aqueous solution (H 3 PO 4 The mass fraction is 85%), 0.84g LiOH·H 2 O, 4.04g Fe(NO 3 ) 3 9H 2 O and 0.55g resorcinol were sequentially added to 10g H 2 O, stir well;

[0031](2) Add 10 g of methanol solution containing 0.81 g of formaldehyde solution (the mass fraction of formaldehyde is 37%) to the solution obtained in step (1), and stir well;

[0032] (3) The mixed solution in step (2) was transferred to a reaction kettle, sealed, and crystallized under autogenous pressure at 180° C. with constant temperature stirring (600 rpm) for 6 hours. After the reaction was completed, the product was suction filtered, washed with deionized water, and air-dried in an oven at 70°C for 12 hours to obtain LiFePO 4 OH / RF powder precursor;

[0033] (4) LiFePO obtained in step (3) 4 OH / RF powder precursor placed in Ar / H 2 (H 2 The volume fraction is 6%) in a tube furnace with an atmosphere at 2°C min -1 The heating rate was increased to 700°C and kept...

Embodiment 2

[0035] (1) 1.153g H 3 PO 4 Aqueous solution (H 3 PO 4 The mass fraction is 85%), 0.84g LiOH·H 2 O, 4.04g Fe(NO 3 ) 3 9H 2 O and 0.66g resorcinol were sequentially added to 10g H 2 O, stir well;

[0036] (2) Add 10 mL of methanol solution containing 1.215 g of formaldehyde aqueous solution (the mass fraction of formaldehyde is 37%) to the solution in step (1), and stir well;

[0037] (3) The mixed solution in step (2) was transferred to a reaction kettle, sealed, and crystallized under autogenous pressure at 170° C. with constant temperature stirring (450 rpm) for 8 hours. After the reaction was completed, the product was suction filtered, washed with deionized water, and dried in an oven at 80°C for 10 hours to obtain LiFePO 4 OH / RF powder precursor;

[0038] (4) LiFePO obtained in step (3) 4 OH / RF powder precursor placed in Ar / H 2 (H 2 The volume fraction is 6%) in a tube furnace with an atmosphere at 2°C min -1 The heating rate was increased to 700°C and kept a...

Embodiment 3

[0040] (1) 1.153g H 3 PO 4 Aqueous solution (H 3 PO 4 The mass fraction of is 85%), 1.53g CH 3 COOLi·2H 2 O, 4.04g Fe(NO 3 ) 3 9H 2 O and 0.55g resorcinol were sequentially added to 10g H 2 O, stir well;

[0041] (2) Add 10 g of methanol solution containing 1.215 g of formaldehyde solution (the mass fraction of formaldehyde is 37%) to the solution of step (1), and stir well;

[0042] (3) The mixed solution in step (2) was transferred to a reaction kettle, sealed, and crystallized under autogenous pressure at 200° C. with constant temperature stirring (600 rpm) for 5 hours. After the reaction was completed, the product was suction filtered, washed with deionized water, and dried in an oven at 80°C for 12 hours to obtain LiFePO 4 OH / RF powder precursor;

[0043] (4) LiFePO obtained in step (3) 4 The OH / RF powder precursor was placed in a tube furnace with an Ar atmosphere at 3 °C min -1 The temperature was raised to 650°C at a constant rate and kept at a constant te...

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Abstract

The invention discloses a solvothermal assisted preparation method of LiFePO4 / C multistage composite microspheres and belongs to the technical field of electrochemical energy storage materials. The method is characterized by taking tervalent Fe3<+> as an iron source, carrying out in-situ synthesis of resorcinol-formaldehyde resin (RF) surface modified LiFePO4OH multistage composite microspheres LiFePO4OH / RF through a one-step mixed solvothermal method; and further converting the composite microspheres into LiFePO4 / C multistage composite microspheres through high-temperature carbon thermal reduction treatment under the protective atmosphere. The compaction density of LiFePO4 / C reaches up to 1.3g / cm<3>; meanwhile, nanoscale primary particles ensure sufficient electrode / electrolyte active contact area, so that the material shows excellent electrochemical lithium storage performance and has a potential application prospect in the field of high-energy / power lithium ion batteries; the preparation process is free of additional introduction of carbon source or treatment of grinding and mixing; the method is an economical, efficient and environment-friendly synthesis method; the large-scale commercial production is expected to be achieved.

Description

technical field [0001] The invention belongs to the technical field of electrochemical energy storage materials, in particular to a LiFePO 4 A solvothermal-assisted preparation method of / C multi-level composite microspheres. Background technique [0002] With the acceleration of the industrialization process, people's living style and living standards have undergone earth-shaking changes, but at the same time, the excessive exploitation and wanton consumption of fossil energy such as coal, oil, and natural gas have also intensified. Today, energy shortages, environmental degradation and other problems It has become the most urgent problem in the world to be solved. In view of the sustainable development strategy, vigorously developing new clean energy industries has become an inevitable choice to solve the current energy and environmental crisis. Lithium-ion batteries (LIBs) are clean chemical power sources developed at the end of the 20th century. Since their commerciali...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62
CPCH01M4/5825H01M4/625Y02E60/10
Inventor 张宗弢王洪宾王润伟刘丽佳
Owner JILIN UNIV
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