Porous manganese vanadium lithium lithium phosphate composite cathode material and preparation method thereof
A composite positive electrode material, lithium manganese vanadium phosphate technology, applied in phosphorus compounds, chemical instruments and methods, battery electrodes, etc., can solve the problems of uneven pore size distribution of porous materials, reduce material uniformity, etc., and achieve low reaction temperature , excellent electrochemical performance, and wide source of raw materials
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Embodiment 1
[0034] (1) Weigh 2.45g (10mmol) of manganese acetate tetrahydrate, 4.68g (40mmol) of ammonium metavanadate, and 7.27g (70mmol) of lithium dihydrogen phosphate, add them to 0.1L deionized water, and then add 10.59 g of oxalic acid dihydrate g (84mmol), placed in a stirred reactor equipped with an ultrasonic device, at an ultrasonic frequency of 30kHz and a stirring speed of 250r / min, stirred and reacted for 1h to obtain a mixed solution;
[0035] (2) Place the mixed solution obtained in step (1) in a vacuum freeze dryer, and freeze-dry in vacuum for 24 hours at -30°C and a vacuum degree of 15Pa to obtain a solid powder;
[0036] (3) The solid powder obtained in step (2) was roasted at 725°C for 8 hours under the protection of high-purity argon, and then cooled to room temperature with the furnace to obtain the porous manganese vanadium lithium phosphate composite positive electrode material Li 2.33 mn 0.33 V 1.33 (PO 4 ) 2.33 .
[0037] Depend on figure 1 The transmission...
Embodiment 2
[0041] (1) Weigh 9.80g (40mmol) of manganese acetate tetrahydrate, 14.02g (120mmol) of ammonium metavanadate, 5.27g (220mmol) of lithium hydroxide, 25.3g (220mmol) of ammonium dihydrogen phosphate, and add them into 0.6L to remove Then add 30.26g (240mmol) of oxalic acid dihydrate into ionized water, place it in a stirred reactor equipped with an ultrasonic device, and stir for 0.5h at an ultrasonic frequency of 20kHz and a stirring speed of 50r / min to obtain a mixed solution;
[0042] (2) Place the mixed solution obtained in step (1) in a vacuum freeze dryer, and freeze-dry it for 12 hours at -5°C and a vacuum degree of 5 Pa to obtain a solid powder;
[0043] (3) Under the protection of high-purity hydrogen / argon mixed gas (hydrogen volume concentration is 5%), the solid powder obtained in step (2) is roasted at 500 ° C for 6 hours, and then cooled to room temperature with the furnace to obtain porous manganese vanadium lithium phosphate Composite cathode material Li 2.2 mn ...
Embodiment 3
[0047] (1) Weigh 0.35g (2mmol) of manganese oxalate dihydrate, 50.54g (432mmol) of ammonium metavanadate, 67.54g (650mmol) of lithium dihydrogen phosphate, add them to 0.66L deionized water, and then add 119.80g of oxalic acid dihydrate g (950.3mmol), placed in a stirring reactor equipped with an ultrasonic device, at an ultrasonic frequency of 40kHz and a stirring speed of 400r / min, stirred and reacted for 2h to obtain a mixed solution;
[0048] (2) Place the mixed solution obtained in step (1) in a vacuum freeze dryer, and freeze-dry in vacuum for 36 hours at -50°C and a vacuum degree of 30Pa to obtain a solid powder;
[0049] (3) The solid powder obtained in step (2) was roasted at 800°C for 10 hours under the protection of high-purity nitrogen, and then cooled to room temperature with the furnace to obtain the porous manganese vanadium lithium composite positive electrode material Li 2.98 mn 0.009 V 1.98 (PO 4 ) 2.98 .
[0050] Battery assembly: Weigh 0.4g of the obta...
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