Preparation method of rare earth doped iron lithium phosphate powder
A lithium iron phosphate and rare earth doping technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem that the modification effect of lithium iron phosphate LiFePO4 has not been reported, and can improve the capacity and capacity cycle performance. , the composition is uniform, the effect of wide application prospects
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[0015] The invention provides a method for preparing a rare earth-doped lithium iron phosphate powder, which is a positive electrode material for a lithium-ion battery, by doping a rare-earth lanthanoid compound and significantly improving the basic electrical properties of the matrix. Said lithium ion battery anode material lithium iron phosphate uses molecular formula Li 1-x RE x FePO 4 Indicates that RE is the dopant source element, 0<x≤0.05;
[0016] The specific method of the preparation method of the rare earth-doped lithium iron phosphate powder is as follows:
[0017] Lithium salt, ferrous salt, phosphate and rare earth dopant are fed at one time according to the molar ratio of element Li:Fe:P:RE=(1-x):1:1:x, and then deionized water and industrial alcohol are added and at least one of anhydrous ethanol as a mixing medium, mixed ball milling for 6-12 hours, and dried at 40-70°C; after drying, the powder was heated at 400-550°C in an inert atmosphere or a reducing at...
Embodiment 1
[0028] 0.0975 moles of lithium hydroxide LiOH·H 2 O, 0.1 mole ferrous oxalate Fe(C 2 o 4 )·2H 2 O and 0.1 mole ammonium dihydrogen phosphate NH 4 h 2 PO 4 and 0.00125 moles of lanthanum oxalate nonahydrate La 2 (C 2 o 4 ) 3 9H 2 O mixed and added to a polyester tank, added 70ml of absolute alcohol, sealed and ball milled on a planetary ball mill for 10 hours. To 400°C, keep warm for 8 hours, cool down to room temperature with the furnace, get pre-burned material, use denatured alcohol as the medium for ball milling for 6 hours, and after drying the material, in a nitrogen atmosphere of 0.3 liters / min, the temperature rises at a rate of 4°C / min The rate was raised to 700°C, kept at a temperature of 8 hours, and then cooled to room temperature with the furnace, and the obtained positive electrode material Li 0.975 La 0.025 FePO 4 .
[0029] Weigh 0.9g of the above-mentioned positive electrode material powder, add 0.19g of carbon black, 0.096g of polyvinylidene fluo...
Embodiment 2
[0031] 0.04975 moles of lithium carbonate Li 2 CO 3 , 0.1 mol of ferrous acetate Fe(CH 3 COO) 2 2H 2 O and 0.1 mole ammonium phosphate (NH 4 ) 3 PO 4 and 0.00025 moles of lanthanum oxide La 2 o 3 Mix, add to a polyester tank, add 100ml of industrial alcohol, seal and mix on a planetary ball mill for 6 hours, discharge and dry, and raise the temperature to 430 at a rate of 5°C / min under a nitrogen atmosphere of 0.3 liters / min ℃, keep warm for 7.5 hours, cool down to room temperature with the furnace, obtain the pre-fired material, take water as the medium ball mill for 10 hours, discharge and dry in a nitrogen-hydrogen mixed atmosphere of 0.3 liters / minute (nitrogen: hydrogen = 9: 1, volume ratio), the temperature was raised to 720 °C at a rate of 4 °C / min, kept for 7 hours, and cooled to room temperature with the furnace to obtain the positive electrode material Li 0.995 La 0.005 FePO 4 .
[0032] Weigh 1.125g of positive electrode material powder, add 0.169g of ca...
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