Preparation method for iron lithium phosphite anode material simultaneously doped with fluorine ion and metallic ion
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Embodiment 1
[0027] According to lithium ion: ferrous ion: phosphorus ion: fluorine ion: the mol ratio of cobalt ion is 0.95: 0.90: 0.95: 0.10: 0.10 weighing reaction composition lithium carbonate, ferrous oxalate, phosphorus pentoxide, lithium fluoride, co 2 o 3 . Add 1% polypropylene based on the mass of lithium ferrous phosphate calculated based on the mass of the reactant, methanol of 1 / 10 volume of the above reaction mixture, ball mill and mix for 3 hours at a speed of 100 rpm, at 70 ° C under a pressure of 10 Pa Drying is carried out under vacuum. The dried powder sample was placed under a nitrogen atmosphere, heated from room temperature to 650 °C at a heating rate of 1 °C / min, kept at the temperature for sintering for 5 hours, and cooled to room temperature to prepare a reaction precursor.
Embodiment 2
[0029] According to lithium ion: ferrous ion: phosphorus ion: fluorine ion: the mol ratio of cobalt ion is 1.07: 1.02: 1.00: 0.10: 0.050 weighing reaction composition lithium oxalate, ferrous acetate, phosphorus pentoxide, lithium fluoride, co 3 o 4 . Add 20% glucose based on the mass of lithium ferrous phosphate calculated based on the mass of the reactant, and 10 times the volume of ethanol of the above reaction mixture, ball mill and mix for 15 hours at a speed of 1000 rpm, and vacuum at 120°C at a pressure of 10132Pa down to dry. The dried powder sample was placed in an atmosphere of 90% nitrogen and 10% hydrogen gas mixture, heated from room temperature to 650 °C at a heating rate of 30 °C / min, kept at the temperature for sintering for 15 hours, and cooled to room temperature to obtain a reaction precursor. Add 10 times the volume of ethanol to the reaction mixture, ball mill and mix for 15 hours at a speed of 800 rpm, and dry at 120° C. under a vacuum of 1013 Pa. The...
Embodiment 3
[0031] According to lithium ion: ferrous ion: phosphorus ion: fluorine ion: the mol ratio of nickel ion is 0.95: 1.02: 0.95: 0.05: 0.08 weighing reaction composition lithium hydroxide, ferrous carbonate, the phosphorus pentoxide of 60% mole And 40% mole mixture of phosphorus trioxide, sodium fluoride, NiO. Add 15% sweet potato powder based on the mass of lithium ferrous phosphate calculated according to the mass of the reactant, and formic acid of 2 times the volume of the above reaction mixture, ball milling and mixing for 8 hours at a speed of 500 rpm, at 100 ° C under a pressure of 5000 Pa Drying is carried out under vacuum. The dried powder sample was placed in an atmosphere of 80% nitrogen and 20% argon gas mixture, heated from room temperature to 580 °C at a heating rate of 10 °C / min, kept at the temperature for sintering for 10 hours, and cooled to room temperature to obtain a reaction precursor. Add 3 times the volume of acetone of the reaction mixture to the reaction...
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