Preparation method of lithium iron phosphate-carbon material composite
A technology of lithium iron phosphate and carbon materials, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of complex preparation process and difficulty in particle size control by liquid phase method, and achieve the effect of high volume specific capacity and high cycle stability
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[0043] Specifically, the present invention provides a preparation method of lithium iron phosphate-carbon material composite, which comprises the following steps:
[0044] a) dispersing the carbon material in water and / or alcohol to obtain a dispersion;
[0045] b) dissolving the phosphorus source, iron source, and lithium source compounds (and additives) in water, alcohol, or a mixture of water and alcohol, respectively, to obtain corresponding solutions;
[0046] c) mixing the dispersion obtained in step a) with the various solutions obtained in step b) to obtain a slurry product; and
[0047] d) subjecting said slurry product to solvothermal treatment at elevated temperature in a closed vessel;
[0048] optionally:
[0049] e) The product obtained in step d) is suction-filtered, dried, pulverized, mixed with the carbon source compound in solid phase or soaked in the solution of the carbon source compound, and then filtered and dried to obtain a powder, wherein the carbon ...
Embodiment 1
[0075] Weigh 1.2g graphene (see Ning, G. for the preparation method of this kind of graphene; Fan, Z.; Wang, G.; Gao, J.; Qian, W.; Wei, F.Chemical Communications 2011,47, 5976), add 100mL of ethanol and water mixed solution (ethanol: water = 1: 3, volume ratio), and ultrasonically disperse for 5 minutes (ultrasonic instrument model KH-2200, power 600W, Kunshan Kechuang Supermarket Instrument Co., Ltd.), forming Uniform dispersion. Weigh 9.8g of phosphoric acid, 27.8g of ferrous sulfate hydrate, 4.2g of lithium hydroxide and 5g of citric acid, respectively, and add them into 500mL of deionized water to obtain respective solutions. Under stirring, first phosphoric acid aqueous solution is added dropwise in the dispersion liquid of graphene and continues to stir for 10 minutes, then drips ferrous sulfate aqueous solution and continues to stir for 10 minutes, then drips lithium hydroxide aqueous solution and continues to stir for 10 minutes, finally Aqueous citric acid solution ...
Embodiment 2
[0078] Using the same proportion and solvent heat treatment process as in Example 1, add the powder obtained after solvent heat treatment into the vertical fluidized bed, first pass 1L / min argon gas, raise the temperature to 600°C, and then pass 1L / min ethylene, turn off ethylene after 30 minutes, feed 0.03L / min hydrogen, and calcine for 6 hours. After cooling to room temperature, the obtained powder sample is taken out to be the final product.
[0079] The tap density of the obtained lithium iron phosphate-carbon material composite is 2.2g / cm 3 , The discharge specific capacity can reach 163mAh / g under the condition of 0.2C charge and discharge current, and the discharge specific capacity can reach 145mAh / g under the condition of 5C charge and discharge current. Under the condition of 1C charge and discharge current, the charge and discharge cycle is 100 times, and the capacity retention rate can reach 89%.
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