A kind of sodium zirconium manganese fluoride phosphate/carbon composite material, positive electrode material, positive electrode and sodium ion battery and preparation method thereof
A technology of fluorinated sodium zirconium manganese phosphate and sodium zirconium manganese phosphate, which is applied in the field of sodium ion battery materials, can solve the problem of poor specific capacity, kinetic performance and cycle performance of electrode materials, lagging technology maturity, and difficulties in intercalation and diffusion and other issues, to achieve the effects of rapid migration, improved electrical properties, and excellent electrochemical properties
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Embodiment 1
[0071] Take 0.01mol zirconium oxynitrate, 0.01mol manganese acetate, 0.02mol ammonium dihydrogen phosphate dissolved in deionized water, stir and evaporate at 80 degrees to form a gel, put the gel in a vacuum oven at 80 degrees to dry 4h, and then put it into a tube furnace with argon gas, and sinter at 750 degrees for 10h. To obtain the intermediate zirconium manganese phosphate, mix the zirconium manganese phosphate intermediate with sodium fluoride at a molar ratio of 1:3, and add 0.03 mol of citric acid. Ball milling at 500r / min for 8h, sintering at 700°C for 12h under argon gas. Get Na 3 ZrMn(PO 4 ) 2 f 3 / C,xrd as figure 1 , sem, figure 2 .
[0072] Utilize the prepared Na 3 ZrMn(PO 4 ) 2 f 3 / C composite material, assembled into a sodium ion button battery, the measured electrochemical data has an average voltage of 4.0V, and after 100 cycles at 0.5C, the discharge specific capacity reaches 90.5mAh / g, and the capacity retention rate reaches more than 95%. ....
Embodiment 2
[0074] Take 0.01mol zirconium oxynitrate, 0.01mol manganese acetate, 0.02mol ammonium dihydrogen phosphate dissolved in deionized water, stir and evaporate at 80 degrees to form a gel, put the gel in a vacuum oven at 80 degrees to dry 4h, and then put it into a tube furnace with argon gas, and sinter at 650 degrees for 8h. To obtain the intermediate zirconium manganese phosphate, mix the intermediate zirconium manganese phosphate and sodium fluoride at a molar ratio of 1:3, and add 0.03 mol of citric acid. Ball milling at 500r / min for 8h, sintering at 700°C for 12h under argon gas. Get Na 3 ZrMn(PO 4 ) 2 f 3 / C.
[0075] Utilize the prepared Na 3 ZrMn(PO 4 ) 2 f 3 / C composite material, assembled into a sodium ion button battery, the measured electrochemical data has an average voltage of 4.0V, and after 100 cycles at 0.5C, the discharge specific capacity reaches 87.5mAh / g, and the capacity retention rate reaches more than 90%. .
Embodiment 3
[0077] Take 0.01mol zirconium oxynitrate, 0.01mol manganese acetate, 0.02mol ammonium dihydrogen phosphate dissolved in deionized water, stir and evaporate at 80 degrees to form a gel, put the gel in a vacuum oven at 80 degrees to dry 4h, and then put it into a tube furnace with argon, and sinter at 850 degrees for 16h. To obtain the intermediate zirconium manganese phosphate, mix the intermediate zirconium manganese phosphate and sodium fluoride at a molar ratio of 1:3, and add 0.03 mol of citric acid. Ball milling at 500r / min for 8h, sintering at 700°C for 12h under argon gas. Get Na 3 ZrMn(PO 4 ) 2 f 3 / C.
[0078] Utilize the prepared Na 3 ZrMn(PO 4 ) 2 f 3 / C composite material, assembled into a sodium ion button battery, the measured electrochemical data has an average voltage of 4.0V, and after 100 cycles at 0.5C, the discharge specific capacity reaches 84.5mAh / g, and the capacity retention rate reaches more than 90%. .
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