Sodium vanadium phosphate composite cathode material and preparation method thereof
A composite cathode material, sodium vanadium phosphate technology, applied in the direction of positive electrodes, electrode manufacturing, phosphorus compounds, etc., can solve the problems of high cost of redox graphene, expensive spray pyrolysis equipment, and can not meet the batch demand, etc., to achieve the best capacity and cycle stability, excellent cycle stability, and excellent electrochemical performance
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[0030] A method for preparing a sodium vanadium phosphate composite positive electrode material provided in a typical embodiment of the present invention is characterized in that it comprises:
[0031] Step 1: Mix ammonium metavanadate, ammonium dihydrogen phosphate, sodium carbonate and sucrose uniformly in an agate ball mill jar in proportion, add ethanol solution and put the mixture into a planetary ball mill, the ball mill speed is 450-2850 rpm, ball mill 1.5-72 hours to obtain the precursor slurry of sodium vanadium phosphate composite, dry the precursor slurry at 55-135° C. for 2-64 hours in a vacuum oven, vacuumize it and dry it for 2-18 hours, Obtain the first precursor.
[0032] In this step, preferably, the molar ratio of ammonium metavanadate, ammonium dihydrogen phosphate, sodium carbonate and sucrose is 4:6:3:2. Taking ammonium metavanadate (4 mmol), ammonium dihydrogen phosphate (6 mmol), sodium carbonate (3 mmol) and sucrose (2 mmol) as examples, add 5-95 mL of...
Embodiment 1
[0046] (1) Preparation of sodium vanadium phosphate composite cathode material
[0047] Step 1, weigh ammonium metavanadate (4 mmol), ammonium dihydrogen phosphate (6 mmol), sodium carbonate (3 mmol) and sucrose (2 mmol) into the agate ball mill jar, add 24 mL ethanol solution, and mix well mix. The ball milling speed was 1000 rpm, and the ball milling time was 36 hours to obtain a light blue sodium vanadium phosphate composite precursor slurry. It was dried in an oven at 115°C for 2 hours, and dried in a vacuum oven at 115°C for 8 hours to obtain a blue / light blue sodium vanadium phosphate precursor powder, that is, the first precursor.
[0048] Step 2, weigh 20 g of the first precursor and place it in a 100 ml beaker, and add 64 ml of deionized water. Add 244ml deionized water to the nano spray tank. Transfer the evenly mixed liquid to the reaction site, set the mist volume to 2 gears, and after 5.5 hours of reaction time, take out the atomized material and place it in a ...
Embodiment 2- Embodiment 7
[0054] Embodiment 2-Embodiment 7 differs from Embodiment 1 only in the rotational speed / time of ball milling, the spraying time in step 2 and the solid-phase sintering temperature in step 3, as shown in Table 1. The corresponding charge and discharge data and cycle performance data can be obtained by performing a performance test on the obtained button-type sodium-ion battery, which corresponds to the performance of the sodium-ion battery of the sodium vanadium phosphate material.
[0055]
[0056] to combine Figure 1-Figure 8 , figure 1 It shows that when the sintering temperature is 660 ℃ (NVP / C-660, Example 6), the obtained sodium vanadium phosphate composite material is used as the positive electrode material of the sodium ion battery, and the battery voltage platform is unstable and the polarization is very large. At a current density of 100 mA / g, the specific capacity is only 87.7mA h / g, which does not improve the conductivity much. figure 2 It shows that when the...
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