Synthesis method of lithium ion battery composite cathode material LiMn1-xFexPO4/C

A composite cathode material, lithium ion battery technology, applied in battery electrodes, positive electrodes, secondary batteries, etc., can solve problems such as poor performance, achieve short lithium ion diffusion paths, high packing density, and improve energy density and rate. performance effect

Inactive Publication Date: 2016-02-24
CENT SOUTH UNIV
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Problems solved by technology

0.01C discharge specific capacity is 135mAhg -1 , but the discharge specific capacity is only 83mAhg at a higher rate of 1C -1 , the article only mentions the performance of looping 5 times, the performance is not good

Method used

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  • Synthesis method of lithium ion battery composite cathode material LiMn1-xFexPO4/C
  • Synthesis method of lithium ion battery composite cathode material LiMn1-xFexPO4/C
  • Synthesis method of lithium ion battery composite cathode material LiMn1-xFexPO4/C

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Experimental program
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Embodiment 1

[0028] Weigh trimanganese tetroxide, ferric iron tetroxide and ammonium dihydrogen phosphate according to the Mn:Fe:P molar ratio of 0.8:0.2:1, and add 5wt% polyvinyl alcohol of the product material, mix through octagonal ball milling for 4h, and rotate at 100r / min. The mixture was reacted at 600°C for 5 h under the protection of argon atmosphere to obtain a gray product. Then the mechanically pulverized gray pyrophosphate, lithium carbonate and superconducting carbon were mixed in proportion, wherein Li:P molar ratio was 1:1 to weigh lithium carbonate, and the superconducting carbon was added in an amount of 1.5wt% of the product. Place in a high-speed fusion machine and mix for 3 hours at a speed of 700r / min. Then it was calcined at 650 °C for 8 h under the protection of argon and cooled to room temperature to obtain LiMn 0.8 Fe 0.2 PO 4 / C composite cathode material (XRD figure sees embodiment figure 1 a, topography see embodiment figure 2 a, 2b). It can be seen fr...

Embodiment 2

[0030] Manganese ferrite (MnFe 2 o 4 ), diammonium hydrogen phosphate is weighed according to (Mn+Fe):P molar ratio 1:1, and the polypropylene of product 3wt% is added, mixes and disperses in the ball mill jar of planetary ball mill, passes through planetary ball mill ball mill 2h, rotating speed 400r / min, to obtain the precursor mixture. The mixture was reacted at 650 ° for 8h under the protection of argon atmosphere to obtain (Mn 1 / 3 Fe 2 / 3 ) 2 P 2 o 7 / C pyrophosphate precursor. Then the pyrophosphate precursor, lithium hydroxide and sucrose were mixed in proportion, Li:P molar ratio was 1:1 to weigh lithium hydroxide, and the added amount of sucrose was 7wt% of the product. Place in a high-speed mixer and mix for 5 hours at a speed of 1000r / min. Then it was calcined at 750 °C for 6 h under the protection of argon and cooled to room temperature to obtain LiMn 1 / 3 Fe 2 / 3 PO 4 / C composite cathode material. It is detected that the composite positive electrode mat...

Embodiment 3

[0032] Ammonium phosphate, manganese dioxide, and ferric oxide were weighed according to the Mn:Fe:P molar ratio of 0.9:0.1:1, and 9 wt% phenolic resin was added to the product material, mixed and passed through a V-type mixing ball mill for 3 hours at a speed of 200r / min. The mixture was reacted at 550 ° for 6h under the protection of argon atmosphere to obtain a gray (Mn 0.9 Fe 0.1 ) 2 P 2 o 7 / C, to detect the XRD structure see the embodiment figure 1 b. Then gray pyrophosphate, lithium carbonate and polypropylene are mixed in proportion, wherein Li:P molar ratio is 1:1 to weigh lithium carbonate, and the addition amount of polypropylene is 15wt% of the product. Place in a high-speed mixer and mix for 6 hours at a speed of 700r / min. Then calcined at 600 °C for 4 h under the protection of argon and cooled to room temperature to obtain LiMn 0.9 Fe 0.1 PO 4 / C composite positive electrode material (topographical figure sees embodiment figure 2 c). SEM shows that ...

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Abstract

The invention relates to a synthesis method of lithium ion battery composite cathode material LiMn1-xFexPO4 / C. A manganese source, an iron source, a phosphorus source and an organic carbon source are evenly mixed and processed by a high-energy ball mill. Mixtures are subjected to heat treatment at 500-700 DEG C under the protection of inert atmosphere so that (Mn1-xFex)2P2O7 / C can be prepared; then, pyrophosphate / carbon, a lithium source and a carbon source are mixed, heat treatment is performed at 600-750 DEG C under protection of inert atmosphere, and ferromanganese lithium phosphate / carbon anode materials with a composite conductive network are obtained. The synthesis method is suitable for large-scale industrialized production, the prepared materials are composed of secondary particles of primary nano-crystals covered with amorphous carbon, distribution is uniform, and the uniform conductive network is formed on the surfaces of phosphate particles in an in-situ mode. The obtained composite cathode material has high rate capacity and high compaction intensity and has good application prospects in the aspect of high-energy-density lithium ion batteries.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery cathode material preparation, and relates to a high energy density lithium ion battery composite cathode material LiMn 1-x Fe x PO 4 / C synthesis method. Background technique [0002] The research and development of positive electrode materials with high safety, low cost, green and high energy density has important research value and significance for the research and development of energy storage (power) lithium-ion batteries. Polyanionic LiMnPO 4 The cathode material has become a very potential cathode material for lithium-ion batteries due to its high-voltage discharge platform, good safety, and abundant resources. LiMnPO 4 With a higher voltage platform (4.1VvsLi + / Li), LiMnPO 4 than LiFePO 4 with a higher theoretical energy density. while LiMnPO 4 The energy density of is considered to be the maximum energy density achievable in the electrochemical stability window of ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M4/136H01M4/1397H01M10/0525
CPCH01M4/136H01M4/1397H01M4/362H01M4/5825H01M4/625H01M10/0525H01M2004/028Y02E60/10
Inventor 胡国荣曹雁冰彭忠东杜柯程守强陈鹏伟
Owner CENT SOUTH UNIV
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