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Ion exchange assisted preparation method of LiFePO4/C nano composite material

A nano-composite material and ion-exchange technology, which is applied in the field of ion-exchange-assisted preparation of LiFePO4/C nano-composite materials, can solve the problems of expensive reduction of lithiation agents, difficulty in popularization and promotion, etc., and achieve excellent electrochemical lithium storage performance, crystal grain Small and uniform, to 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

However, these soft chemical lithiation processes all involve the use of expensive reductive lithiation agents, which are difficult to further scale up and popularize.

Method used

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  • Ion exchange assisted preparation method of LiFePO4/C nano composite material
  • Ion exchange assisted preparation method of LiFePO4/C nano composite material
  • Ion exchange assisted preparation method of LiFePO4/C nano composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Weigh 18.5g FeCl 3 ·6H 2 O was dissolved in 300mL deionized water, stirred well, marked as solution A; weighed 7.86g NH 4 h 2 PO 4 Dissolve in 600mL deionized water, add 3mL aniline monomer, stir well, mark as solution B;

[0032] (2) With solution B under vigorous stirring (450rpm), slowly add solution A dropwise (2.5mL min -1 ), and aged for 5 h with stirring at room temperature. After the reaction, the precipitated product was suction filtered, washed with deionized water, and dried (60°C, 24h) to obtain amorphous FePO 4 ·xH 2 O / PANI powder precursor;

[0033] (3) Weigh 2.325g of the powder precursor obtained in step (2) and uniformly disperse it into 60mL of lithium acetate ethanol solution with a concentration of 0.6M, and lithiate at 60°C for 2h with constant temperature stirring (150rpm). After the system was cooled, the product was subjected to suction filtration, washed with ethanol, and dried at 60°C for 2 hours to obtain Li-Fe(III)PO 4 / PANI lith...

Embodiment 2

[0036] (1) Weigh 2.703g FeCl 3 ·6H 2 O was dissolved in 50mL deionized water, stirred well, marked as solution A; weighed 1.15g NH 4 h 2 PO 4 Dissolve in 100mL deionized water, stir well, and mark it as solution B;

[0037] (2) With solution B under strong stirring (600rpm), slowly add solution A dropwise (1.5mL min -1 ), and aging with stirring at room temperature for 0.5h. After the reaction, the precipitated product was suction filtered, washed with deionized water, and dried (50°C, 12h) to obtain amorphous FePO 4 ·xH 2 O powder precursor;

[0038] (3) Weigh 0.3 g of the powder precursor obtained in step (2) and uniformly disperse it into 10 mL of lithium acetate ethanol solution with a concentration of 0.3 M, and lithiate at 65° C. with constant temperature stirring (180 rpm) for 2 h. After the system was cooled, the precipitated product was suction filtered, washed with ethanol, and dried at 60°C for 1.5h to obtain Li-Fe(III)PO 4 Lithiated intermediates;

[0039...

Embodiment 3

[0041] (1) Weigh 4.04g Fe(NO 3 ) 3 9H 2 O was dissolved in 50mL deionized water, stirred well, marked as solution A; weighed 1.15g NH 4 h 2 PO 4 Dissolve in 100mL deionized water, add 0.5mL aniline monomer, stir well, and mark it as solution B;

[0042] (2) With solution B under strong stirring (600rpm), slowly add solution A dropwise (2.0mL min -1 ), and aged with stirring at room temperature for 8h. After the reaction, the precipitated product was suction filtered, washed with deionized water, and dried (60°C, 10h) to obtain amorphous FePO 4 ·xH 2 O / PANI powder precursor;

[0043] (3) Weigh 0.2g of the powder precursor obtained in step (2) and uniformly disperse it into 10mL of lithium acetate ethanol solution with a concentration of 0.2M, and lithiate at 60°C for 2.5h with constant temperature stirring (150rpm). After the system was cooled, the product was subjected to suction filtration, washed with ethanol, and dried at 60°C for 2 hours to obtain Li-Fe(III)PO 4 ...

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Abstract

The invention provides an ion exchange assisted preparation method of a LiFePO4 / C nano composite material and belongs to the technical field of electrochemical energy storage materials. The ion exchange assisted preparation method comprises the following steps: firstly, slowly dropwise adding an inorganic iron source and a phosphorus source water solution containing a proper amount of aniline (unnecessary) at room temperature and mixing to obtain an amorphous FePO4.xH2O or FePO4.xH2O / PANI (polyaniline) nano composite material; secondly, dispersing the material into a non-aqueous lithium salt system and carrying out low-temperature H<+> / Li<+> ion exchange transformation to obtain a lithium-containing intermediate; finally, uniformly mixing the lithium-containing intermediate and a carbon source, and further carrying out high-temperature carbon heat reduction treatment to transform a mixture into the LiFePO4 / C nano composite material. The nano composite material provided by the invention has ideal physical structure properties, namely high active LiFePO4 crystallization property and small crystal grain size; one layer of semi-graphitized conductive thin carbon uniformly covers the surface (N doping and nitrogen doping can be realized by adding an aniline monomer), so that the LiFePO4 / C nano composite material has excellent electrochemical lithium storage performance and has a potential application prospect in the aspects including portable electronic products, large-size energy storage power stations, power batteries for vehicles and the like.

Description

technical field [0001] The invention belongs to the technical field of electrochemical energy storage materials, in particular to a LiFePO 4 Ion-exchange-assisted preparation of / C nanocomposites. Background technique [0002] Olivine LiFePO 4 It has abundant resource reserves, low cost, green environmental protection, and high specific capacity (170mAh g -1 ), suitable working voltage (3.45V vs. Li / Li + ), ideal platform characteristics, strong overcharge resistance, and good thermodynamic and electrochemical stability, etc., are regarded as one of the most promising cathode materials for lithium-ion batteries (LIBs) in the 21st century. But LiFePO 4 In electrons (<10 -9 S cm -1 ) and ions (10 -12 ~10 -14 cm 2 the s -1 ) conductivity is far less than LiCoO 2 and LiMn 2 o 4 Such as traditional metal oxide cathode materials, which largely limits the practical application of this material in the field of high-power LIBs. Scholars at home and abroad have carrie...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 张宗弢王洪宾王润伟刘丽佳
Owner JILIN UNIV
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