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Preparation method of nano LiFel-xMxPO4/C lithium phosphate composite positive pole material

A life1-xmxpo4, composite positive electrode material technology, applied in the field of lithium ion battery positive electrode material preparation, can solve the problems of large fluctuations in phosphorus component content, unfavorable batch production, complex process steps, etc., achieve stable composition, promote smooth progress, and high The effect of reactivity

Active Publication Date: 2010-07-28
四川浩普瑞新能源材料股份有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, this method uses phosphoric acid as a raw material, and the content of phosphorus components fluctuates greatly. In order to produce lithium iron phosphate with stable quality and accurate stoichiometry in the actual production process, the precursor formula needs to be adjusted at any time, which is not conducive to industrial mass production; The co-precipitation synthesis method involved uses phosphoric acid to react with iron powder to generate insoluble phosphate, which will form crystal nuclei on the surface of the reactant and grow up and gradually cover the reactant, preventing the reaction from proceeding further. It takes a long time to react, and the required temperature High, need to add lithium source later, the process steps are complicated

Method used

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  • Preparation method of nano LiFel-xMxPO4/C lithium phosphate composite positive pole material
  • Preparation method of nano LiFel-xMxPO4/C lithium phosphate composite positive pole material
  • Preparation method of nano LiFel-xMxPO4/C lithium phosphate composite positive pole material

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh lithium dihydrogen phosphate, iron powder, and copper acetate in a molar ratio of 1:0.98:0.02, and add 5wt% glucose of the mixture, dispersed in deionized water, high-energy ball milling for 4h, and vacuum drying at 70°C to obtain the precursor. figure 1 a is its XRD pattern, no iron powder and LiH are found 2 PO 4 Diffraction peak, but the product Li after the complete reaction 3 PO 4 And Fe 3 (PO4) 2 . Placed in an atmosphere furnace, calcined at 600°C for 10 hours under the protection of argon and cooled to room temperature to obtain copper-doped nano-scale LiFePO 4 / C composite cathode material. It is determined that the composite cathode material contains 0.89wt% carbon. XRD tests that the material has a single olivine structure, and the first discharge capacity at 0.2C is 154mAh·g -1 ,Discharge capacity at 1C 140.5mAh·g -1 .

Embodiment 2

[0031] Weigh lithium dihydrogen phosphate, iron powder, lithium carbonate, and vanadium pentoxide in a molar ratio of 1:0.95:0.02:0.005, and add 6wt% sucrose in the mixture, and disperse in deionized water after high-energy ball milling for 5h, 90℃ The precursor is obtained by vacuum drying. Placed in an atmosphere furnace, calcined at 650°C under the protection of argon for 6 hours and cooled to room temperature to obtain lithium-vanadium doped nano-scale LiFePO 4 / C composite cathode material. It was detected that the composite cathode material contained 1.5wt% carbon, and the particle size was uniform about 100nm under high magnification SEM, and the discharge capacity was 130.2mAh·g at 3C. -1 , There is basically no attenuation after 70 cycles.

Embodiment 3

[0033] Weigh lithium dihydrogen phosphate, iron powder, lithium hydroxide monohydrate, and nano-silica in a molar ratio of 1:0.96:0.03:0.01, and add 10wt% polyvinyl alcohol to the mixture and disperse in deionized water-ethanol The mixed medium was subjected to high-energy ball milling for 6 hours and vacuum dried at 110°C to obtain a precursor. Placed in an atmosphere furnace, calcined at 700°C under the protection of argon and cooled to room temperature for 6 hours to obtain lithium-silicon doped nano-scale LiFePO 4 / C composite cathode material. The carbon content of the composite positive electrode material is 2.1wt%, and it can be seen from TEM that the particle size is 50-100nm, there is a good conductive carbon film connection between the particles, and the discharge capacity is 141mAh·g at 2C. -1 , There is basically no attenuation after 70 cycles.

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Abstract

The invention relates to a preparation method of nano LiFel-xMxPO4 / C lithium phosphate composite positive pole material. Lithium dihydrogen phosphate, iron powder, an M element source and an organic carbon source are uniformly mixed in a solvent medium, are treated for 2 to 7h through a high-energy ball mill, have chemical reaction under mechanical activation, and a uniformly dispersed precursor is prepared. The precursor is thermally treated for 2 to 10h at 600 to 800 DEG C under atmosphere protection and cooled to be room temperature, and the nano LiFel-xMxPO4 / C lithium phosphate composite positive pole material is prepared. The preparation method has simple and high-efficiency process and the whole process does not produce ammonia, wastewater and other polluting substances, and is applicable to industrial production. The primary particles of the prepared material are nano particles which are uniformly distributed, and the material is characterized by high specific capacity and good rate cycle performance.

Description

Technical field [0001] The invention belongs to the technical field of preparation of lithium ion battery cathode materials, and relates to a nano-level lithium phosphate series LiFe 1-x M x PO 4 / C composite cathode material preparation method. Background technique [0002] With the global energy crisis and environmental protection issues receiving more and more attention from the world, power-type lithium-ion batteries are increasingly being favored by the global battery industry and related industries. The positive electrode material is a key part of power lithium-ion batteries, and its performance improvement and cost reduction directly affect the entire power battery industry. Therefore, seeking cheap, stable, safe, and environmentally friendly battery cathode materials is essential for the development of the power battery industry. Lithium phosphate material LiMePO with olivine structure 4 (Me=Fe 2+ , Co 2+ , Ni 2+ , Mn 2+ ) Has attracted much attention because of its very...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 胡国荣曹雁冰彭忠东杜柯
Owner 四川浩普瑞新能源材料股份有限公司
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