Preparation method of monodisperse nanometer olivine type manganese-based phosphate positive-pole material and lithium-ion secondary battery thereof
An olivine-type manganese-based phosphate, cathode material technology, applied in secondary batteries, battery electrodes, circuits, etc., can solve problems such as preparing monodispersion, and achieve controllable morphology, good dispersibility, and good application prospects. Effect
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[0037] A method for preparing a monodisperse nanometer olivine-type manganese-based phosphate positive electrode material, the steps are: dispersing a lithium source compound, a manganese source compound, a phosphorus source compound and a compound doped with elements in the case of doping in water and an organic solvent In the mixed solvent, the volume ratio of the organic solvent and water in the mixed solvent is controlled at 0-5:1, and the mixed solvothermal reaction is carried out in the reactor, the reaction temperature is 120-230°C, the reaction pressure is 0.2-30Mpa, and the reaction time is From 1 minute to 24 hours, the positive electrode material of monodisperse nano-olivine manganese-based phosphate particles is finally obtained, and its chemical formula is Li x mn y m 1-y PO 4 , 0.8≤x≤1.2, 0.5≤y≤1.0, preferably 0.85≤x≤1.15, 0.6≤y≤1.0, more preferably 0.9≤x≤1.1, 0.8≤y≤1.0; M is Fe, Co, Ni, At least one metal element of Zn, Cu, Al, Mg, Ti, Zr, Sn, V, Nb, W, La, C...
Embodiment 1
[0054] Measure 150ml of 1M phosphoric acid aqueous solution, add it to 600ml polyethylene glycol 400, and mix well. Then add 300ml, 0.5M MnSO 4 aqueous solution, and stir well. Then, 450 ml of 1M LiOH aqueous solution was added to the above solution. After mixing evenly, the above solution was transferred into a closed stainless steel reactor lined with polytetrafluoroethylene, heated to 180°C and kept for 12 hours. After cooling to room temperature, washing with deionized water and drying to obtain lithium manganese phosphate nanomaterials. Elemental analysis results show that the product has LiMnPO 4 chemical formula. The X-ray diffraction pattern of the product is as figure 1As shown, the product is shown to be a pure lithium manganese phosphate phase. The shape of the product is as figure 2 As shown, they are all in the shape of nanorods, and the size distribution is uniform. The length of the nanorods is 100-500nm, and the width is about 50-100nm.
Embodiment 2
[0056] Measure 150ml of 1M phosphoric acid solution, add it to 600ml polyethylene glycol 400, and mix well. Then add 450ml, 1M LiOH solution, and stir well. Then add 300ml, 0.5M MnSO to the above solution 4 solution. After mixing evenly, the above solution was transferred into a closed stainless steel reactor lined with polytetrafluoroethylene, heated to 140°C and kept for 10 hours. After cooling to room temperature, washing with deionized water and drying to obtain lithium manganese phosphate nanomaterials. Elemental analysis results show that the product has LiMnPO 4 chemical formula. The shape of the product is as image 3 As shown, it is a monodisperse nanosheet with a diameter of about 100 nm and a thickness of less than 30 nm.
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