Cathode material Li3V2(PO4)3 of lithium ion battery and its making method
A lithium-ion battery and cathode material technology, applied in the field of lithium vanadium phosphate material preparation, can solve problems such as difficult control of heating temperature and time, unguaranteed product purity, short synthesis time by microwave method, etc., and achieve excellent cycle stability , low cost, the effect of preventing particle agglomeration
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[0030] The preparation method of lithium vanadium phosphate lithium ion battery cathode material of the present invention adopts the following steps:
[0031] 1. Preparation of nanoparticles: respectively process non-water-soluble lithium source compounds, vanadium source compounds, phosphorus source compounds and complexing agents through wet ultra-fine ball milling to submicron or nanometer particles; ball milling or crushing equipment, ball milling or The pulverizing equipment is a stirring ball mill, a sand mill, a colloid mill, a jet pulverizer, an impact micropowder ball mill, a jet vortex micropowder machine, an impact pulverizer or a rod mechanical pulverizer.
[0032] 2. Liquid phase mixing reaction: weigh the lithium source compound and the vanadium source compound according to the ratio of the amount of substances Li:V:P:L (complexing agent)=(3.0~3.3):2:3:(1.5~2.2) , phosphorus source compound and complexing agent are dissolved in deionized water at 40-90°C, and sti...
Embodiment 1
[0042] The raw materials lithium carbonate, ammonium metavanadate, and glucose are respectively pulverized by a circulating stirring ball mill to a particle size of submicron or nanometer order, and lithium carbonate (Li 2 CO 3 )54.4 grams, ammonium metavanadate (NH 4 VO 3 ) 114.8 g, phosphoric acid (H 3 PO 4 ) 169.7 grams and 176.6 grams of glucose were respectively dissolved in 150 milliliters of deionized water at 60° C., and stirred at a constant temperature for 3 hours; the glucose solution was first added to the phosphoric acid solution, then lithium carbonate and ammonium metavanadate solution were added successively, and stirred at a constant temperature of 60° C. for 2 Hours until the reaction of the mixed solution is complete and no bubbles are produced.
[0043] The above samples were added with 1wt.% ZrO 2 Afterwards, ball mill (QM-1SP4 planetary ball mill) at a speed of 300r / min for 1 hour, spray dry and granulate in a centrifugal spray granulation dryer at 1...
Embodiment 2
[0046] The raw materials lithium hydroxide, vanadium pentoxide, ammonium dihydrogen phosphate and citric acid were ball milled to submicron or nanoscale, and lithium hydroxide (LiOH·H 2 O) 48.76 grams, vanadium pentoxide (V 2 o 5 )69.05 grams, ammonium dihydrogen phosphate (NH 4 h 2 PO 4 ) 128.26 grams and citric acid 154.66 grams. Dissolve citric acid in 800 ml of deionized water at 80°C and stir at constant temperature for 3 hours; mix lithium hydroxide, vanadium pentoxide and ammonium dihydrogen phosphate and ball mill at 300r / min for 0.5 hours, then add the mixture to lemon acid solution, stirred at 80°C for 3 hours until the reaction was complete.
[0047] The above sample was mixed with 3wt.% Al 2 o 3 After mixing, ball mill at a speed of 400r / min for 1 hour, spray dry and granulate at 300°C, then place the product under the protection of argon and treat it in a tube furnace at 350°C for 4 hours, and obtain phosphoric acid after natural cooling Precursor of vanad...
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