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Synthesizing method of nano-grade lithium ion battery composite positive electrode material LiMnPO4/C

A composite positive electrode material and lithium-ion battery technology, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of inability to ensure the tight packaging of conductive carbon, reduce the material volume energy density, material processing and coating performance, etc.

Inactive Publication Date: 2013-02-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, excessive carbon addition will greatly reduce the volumetric energy density of the material and the processing and coating properties of the material
And since most of the carbon coating process is not in situ recombination but LiMnPO 4 After the material is crystallized and mixed with conductive carbon, it cannot ensure that the conductive carbon is tightly wrapped on the surface of lithium manganese phosphate and evenly dispersed among the particles.

Method used

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  • Synthesizing method of nano-grade lithium ion battery composite positive electrode material LiMnPO4/C
  • Synthesizing method of nano-grade lithium ion battery composite positive electrode material LiMnPO4/C
  • Synthesizing method of nano-grade lithium ion battery composite positive electrode material LiMnPO4/C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Lithium dihydrogen phosphate and manganese powder were weighed according to a molar ratio of 1:1, and 50 wt% glucose was added to the mixed material, dispersed in deionized water-triethylene glycol medium, and subjected to high-energy ball milling for 4 hours to obtain a precursor slurry. Transfer the slurry into a round-bottomed flask with a reflux device, and add an appropriate amount of triethylene glycol as a dispersant and reflux medium. After ultrasonic treatment for 30 min, the reaction was strengthened for 4 h at a stirring speed of 300 r / min in a boiling state. Gained product obtained gray product through high-speed centrifugation after alcohol washing 3 times (XRD sees embodiment figure 1 a). Then the gray product was placed in an atmosphere furnace, calcined at 600 °C for 9 h under the protection of argon and cooled to room temperature to obtain nano-sized LiMnPO 4 / C composite cathode material (TEM sees embodiment figure 2 a and b), XRD detection of the ...

Embodiment 2

[0032] Lithium carbonate, manganese phosphate (MnPO 4 ·H 2 O) Weigh it according to the molar ratio of 0.5:1, add 20wt% sucrose of the mixed material, disperse in the deionized water-tetraethylene glycol medium, and undergo high-energy ball milling for 5 hours to obtain the precursor slurry. Transfer the slurry into a round-bottomed flask with a reflux device, and add an appropriate amount of tetraethylene glycol as a dispersant and reflux medium. After ultrasonic treatment for 20min, the reaction was strengthened for 8h at the stirring speed of 400r / min in the boiling state. The obtained product was washed with alcohol for 3 times, and then separated by high-speed centrifugation to obtain a gray product. Then the gray product was placed in an atmosphere furnace, calcined at 700 °C for 2 h under the protection of argon and cooled to room temperature to obtain nano-sized LiMnPO 4 / C composite cathode material. Detect 3.5wt% carbon in the composite positive electrode materia...

Embodiment 3

[0034] Lithium dihydrogen phosphate and manganese monoxide were weighed according to a molar ratio of 1:1, and 30 wt% citric acid was added to the mixed material, dispersed in an anhydrous ethanol-glycerol medium, and subjected to high-energy ball milling for 6 hours to obtain a precursor slurry . Transfer the slurry into a round-bottomed flask with a reflux device, and add an appropriate amount of glycerol as a dispersant and reflux medium. After ultrasonic treatment for 40 min, the reaction was strengthened for 6 h at a stirring speed of 450 r / min in a boiling state. The obtained product was washed with alcohol for 3 times, and then separated by high-speed centrifugation to obtain a gray product. Then the gray product was placed in an atmosphere furnace, calcined at 500 °C for 10 h under the protection of argon and cooled to room temperature to obtain nano-sized LiMnPO 4 / C composite positive electrode material, XRD detects that this material has a single olivine structure...

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Abstract

The invention relates to a synthesizing method of a nano-grade lithium ion battery composite positive electrode material LiMnPO4 / C. According to the invention, a lithium source, a phosphorous source, a manganese source and an organic carbon source are well mixed in a solvent medium; the mixture is processed for 2-7h in a high-energy ball mill, and a uniformly dispersed precursor slurry is obtained with the activation effect of mechanical forces; the precursor slurry is subjected to ultrasonic dispersion in a high-boiling-point polyol solvent, and is subjected to a reflux reaction; an obtained product is filtered and washed; and the product is subjected to a heat treatment for 1-10h under inert atmosphere protection and under a temperature of 600-800 DEG C, such that the nano-grade lithium manganese phosphate / carbon (LiMnPO4 / C) positive electrode material is obtained. According to the material provided by the invention, primary particles are well distributed nano-particles, and a conductive carbon layer is formed in-situ on the surfaces of the LiMnPO4 / C particles. The method provided by the invention is simple and highly efficient. With the method, no pollutant such as ammonia gas or wastewater is produced during the entire process. Therefore, a development requirement of green chemistry is satisfied.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery cathode material preparation, and in particular relates to a nanoscale lithium-ion battery composite cathode material LiMnPO 4 / C synthesis method. Background technique [0002] Power lithium-ion batteries are increasingly favored by the global battery industry and related industries, and the development of high-performance lithium-ion battery energy storage electrode materials has become one of the important cores of lithium-ion battery industry research. Recently, the advent of polyanion-type cathode materials has become a research hotspot for lithium-ion power battery cathode materials due to its advantages of good safety and cycle stability. LiFePO 4 It has aroused people's great interest for its rich resources, low price, environmental friendliness, long life and high safety. by LiFePO 4 Inspired by success, olivine-type LiMnPO belonging to the orthorhombic crystal system 4 al...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62
CPCY02E60/12Y02E60/10
Inventor 曹雁冰段建国胡国荣彭忠东杜柯
Owner CENT SOUTH UNIV
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