A preparation method of nano-micro graded manganese phosphate lithium/carbon composite positive electrode material

Active Publication Date: 2021-04-13
CENT SOUTH UNIV
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Problems solved by technology

[0006] For the existing micro-nano structure LiMnPO 4 In the material preparation process, the preparation process is complicated, the synthesized particle size is large, and the electrochemical performance is not good. The first purpose of the present invention is to provide a method for preparing a lithium manganese phosphate material with a nano-micro hierarchical structure. Micro-nanostructured LiMnPO with secondary porous particles assembled from primary nanocrystals through controlled particle growth 4 Material

Method used

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  • A preparation method of nano-micro graded manganese phosphate lithium/carbon composite positive electrode material
  • A preparation method of nano-micro graded manganese phosphate lithium/carbon composite positive electrode material
  • A preparation method of nano-micro graded manganese phosphate lithium/carbon composite positive electrode material

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Embodiment 1

[0064] Fixed stoichiometric ratio Li:Mn:P:HMT=2.7:0.95:1:1.2, weighing 0.054mol lithium nitrate, 0.019mol manganese sulfate, 0.02mol phosphoric acid (85%) and 0.024mol hexamethylenetetramine, the nitric acid Lithium, manganese sulfate and hexamethylenetetramine were respectively dissolved in 20ml of ethylene glycol to obtain lithium nitrate solution, manganese sulfate solution, phosphoric acid solution and hexamethylenetetramine solution, heated and stirred at 35°C for 20min; into the manganese sulfate solution being stirred, then drop the lithium nitrate solution into it, and finally drop into the hexamethylenetetramine solution solution, stir sufficiently to finally obtain a mixed emulsion; the emulsion slurry is transferred to a 180ml high-pressure reactor, Place the autoclave in an oven for 1 hour at 80°C and 180°C for 10 hours. After cooling, take out the autoclave, centrifuge the slurry, wash the reactant twice with deionized water and absolute ethanol, and place the wash...

Embodiment 2

[0067]With the metering ratio Li:Mn:P:HMT=3:1:1:1.7, weigh 0.06mol lithium chloride, 0.02mol manganese chloride, 0.02mol phosphoric acid (85%) and 0.034mol hexamethylenetetramine, Dissolve lithium chloride, manganese chloride tetrahydrate and hexamethylenetetramine in 20ml of ethylene glycol respectively to obtain lithium nitrate solution, manganese chloride solution, phosphoric acid solution and hexamethylenetetramine solution; heat at 40°C Stir for 30 minutes; drop the phosphoric acid solution into the manganese chloride solution being stirred, then drop the lithium chloride solution into it, and finally drop into the hexamethylenetetramine solution, stir for 50 minutes to obtain a mixed emulsion; transfer the emulsion to 180ml of high-pressure Reactor, put the high-pressure reactor in an oven for 2 hours at 75°C, and keep it at 160°C for 12 hours. After cooling, take out the high-pressure reactor, centrifuge the slurry, and wash the reactants twice with deionized water and a...

Embodiment 3

[0070] Weigh 0.06 mol of lithium nitrate, 0.019 mol of manganese nitrate (50%), 0.02 mol of lithium dihydrogen phosphate and 0.02 mol of hexamethylenetetramine at the metering ratio Li:Mn:P:HMT=3:0.95:1:1, Lithium nitrate, manganese nitrate and hexamethylenetetramine were dissolved in 20ml of ethylene glycol, and lithium dihydrogen phosphate was dissolved in 30ml of deionized water to obtain lithium nitrate solution, manganese nitrate solution, lithium dihydrogen phosphate solution and hexaethylene tetramine respectively. Methyltetramine solution. Add the lithium dihydrogen phosphate solution dropwise into the stirring manganese nitrate solution, then drop the lithium chloride solution into it, and finally drop into the hexamethylenetetramine solution, and stir for 30 minutes to obtain a mixed emulsion; the emulsion is transferred to a high-pressure 180ml Reactor, put the autoclave in an oven at 70°C for 1 hour, and at 200°C for 10 hours. After cooling, take out the autoclave,...

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Abstract

The invention belongs to the technical field of batteries, and specifically discloses a preparation method of a lithium manganese phosphate / carbon composite material with a nano-micro hierarchical structure, which will contain a manganese source, a lithium source, a phosphorus source, hexamethylenetetramine, ethylene glycol The raw material solution is heat-treated at 70°C to 80°C in advance, and then solvothermally obtained at 160°C to 200°C. The prepared lithium manganese phosphate material with nano-micro hierarchical structure is mixed with a polymer carbon source, dried and calcined at 500°C to 650°C in a protective atmosphere. The primary particles of the material prepared by the invention are nano-scale, have preferential growth and uniform distribution, and are beneficial to the diffusion of lithium ions in the material. The size of the secondary particles is at the micron level, which is conducive to the stability of the structure. The prepared material has a high charge and discharge capacity, excellent cycle stability, and good rate performance.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery cathode material preparation, and relates to a composite cathode material LiMnPO for lithium-ion batteries with hierarchical structure 4 / C synthesis method. Background technique [0002] The development of new power lithium-ion batteries with high safety, high energy density and long life has become a research hotspot. LiMnPO 4 With an olivine structure, the theoretical capacity is 170mAh / g equivalent to that of lithium iron phosphate, but its voltage platform is 4.1V (for Li / Li+), which is 0.7V higher than lithium iron phosphate (3.4V), thereby increasing the energy density. Therefore LiMnPO 4 Cathode materials have aroused the interest of many researchers. [0003] However, the pure phase LiMnPO 4 Conductivity than LiFePO 4 Worse, at the same time, lithium ion diffusion is also a limited one-dimensional channel, making the migration rate of lithium ions smaller at room tempera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/583H01M4/62H01M4/58H01M10/0525C01B25/26C01B25/45C01B25/37
CPCC01B25/26C01B25/375C01B25/45H01M4/362H01M4/5825H01M4/583H01M4/625H01M10/0525Y02E60/10
Inventor 曹雁冰胡国荣彭忠东杜柯许炼谢永强亓先跃
Owner CENT SOUTH UNIV
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