Anode material vanadium lithium phosphate and preparation method thereof
A technology of lithium vanadium phosphate and cathode material, applied in the field of lithium vanadium phosphate material and its preparation, can solve the problems of difficult control of heating temperature and time, unguaranteed product purity, short synthesis time by microwave method, etc., and achieve excellent cycle stability performance, low production cost, and the effect of preventing particle agglomeration
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[0032] The preparation method of cathode material lithium vanadium phosphate of the present invention adopts the following steps:
[0033] 1. Preparation of nanoparticles: Water-insoluble vanadium source compounds and carbon materials are treated by wet ultrafine ball milling to submicron or nanometer particles, while water-soluble vanadium source compounds and carbon materials do not need to undergo this step. Wet ultra-fine ball milling adopts ball milling or pulverizing equipment, ball milling or pulverizing equipment is stirring ball mill, sand mill, colloid mill, airflow mill, impact micropowder ball mill, airflow spiral micropowder machine, impact mill or bar type mechanical pulverizer.
[0034] 2. Mixing reaction in liquid phase: dissolve lithium phosphate salt compound, vanadium source compound and carbon material with submicron or nanometer particles in 20-90°C deionization according to the ratio of substances of 2.9-3.3:2:1.0-3.5 water, stirred for 0.5 to 3 hours to...
Embodiment 1
[0044] The raw materials, conductive acetylene carbon black and vanadium pentoxide, were pulverized by a circulating stirring ball mill to a particle size of the order of nanometers, and lithium dihydrogen phosphate (LiH2PO4) was accurately weighed. 2 PO 4 ) 115.2 grams, vanadium pentoxide (V 2 o 5 ) 67.7 grams and 6.7 grams of conductive acetylene carbon black were successively added to 250 milliliters of deionized water at 20° C., and stirred at constant temperature for 3 hours.
[0045] After adding 0.1wt.% CuO to the above sample, ball mill (QM-1SP4 planetary ball mill) at a speed of 500r / min for 0.5 hour, spray-dry and granulate at 100°C in a centrifugal spray granulation dryer, and granulate at 200r / min / min speed of fusion treatment for 2 hours, and then the product was pretreated in a tube furnace at 300 ° C for 4 hours under the protection of argon, and the pretreated powder was obtained after natural cooling, which is the precursor of lithium vanadium phosphate. T...
Embodiment 2
[0052] The raw material lithium dihydrogen phosphate was ball milled to a submicron scale, and 231.6 grams of lithium dihydrogen phosphate, 172.1 grams of ammonium metavanadate and 61.3 grams of glucose were accurately weighed. Glucose was dissolved in 600 ml of deionized water at 90°C, and stirred at constant temperature for 0.5 hours; lithium dihydrogen phosphate and ammonium metavanadate were added to the above solution in sequence, and ball milled at a speed of 300 r / min for 1 hour.
[0053] The above sample was mixed with 2wt.% Al 2 o 3 After mixing, ball mill at a speed of 400r / min for 1 hour, spray dry and granulate at 360°C, perform fusion treatment at a speed of 600r / min for 1 hour, and then place the product in a tube furnace under the protection of argon. Pretreatment at 350°C for 4 hours, and natural cooling to obtain pretreated powder.
[0054] The obtained pretreated powder was fused with a fusion machine at a rotational speed of 300r / min for 2.5 hours, then pl...
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