Preparation method for solid fluoride ion battery at room temperature based on tin-based fluoride MSnF4 laminated fluoride ion electrolyte
A technology of fluoride ions and electrolytes, applied in battery electrodes, secondary batteries, circuits, etc., to achieve the effects of solving high working temperature, simplifying the preparation process, and simple preparation process
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Embodiment 1
[0028] Weigh 5.2805g BaF respectively 2 and 4.7195g SnF 2 , under the protection of argon, the ball milling speed is 600rpm, the ball milling time is 20h, and the obtained ball milling product is dried at 80°C for 10h. figure 1 (a) BaSnF prepared by high energy ball milling method in this example 4 XRD pattern of the precursor powder. The obtained dry product was sintered under the protection of nitrogen gas, the sintering temperature was 300 °C, and the heating rate was 6 °C min -1 , the sintering time is 3h, and the BaSnF 4 Electrolyte powder. figure 1 BaSnF prepared before and after sintering for this example4 XRD pattern of electrolyte powder. BaSnF before sintering 4 Electrolyte powder XRD ( figure 1 (a)) at 2θ = 24.84°, 28.88°, 41.44° and 48.91° represent (102), (110), (200) and (212) characteristic peaks, respectively, which indicates that the BaSnF before sintering 4 The electrolyte powder has a cubic phase structure. Sintered BaSnF 4 Electrolyte powder XRD (...
Embodiment 2
[0030] Weigh 6.0889g PbF respectively 2 and 3.9112g SnF 2 , under the protection of nitrogen, the ball milling speed was 800rpm, the ball milling time was 15h, and the obtained ball milling product was dried at 60°C for 14h. figure 2 (a) is the PbSnF prepared by the high energy ball milling method in this embodiment 4 XRD pattern of the precursor powder. The obtained dry product was sintered under the protection of argon gas, the sintering temperature was 450 °C, and the heating rate was 3 °C min -1 , the sintering time is 2h, and the PbSnF 4 Electrolyte powder. figure 2 (b) is the PbSnF prepared after sintering of the present embodiment 4 XRD pattern of electrolyte powder. PbSnF before and after sintering 4 The XRD pattern performance of electrolyte powder and BaSnF 4 The same characteristic peak differentiation of electrolyte powder, compared with the standard card, shows that PbSnF 4 The electrolyte powder is a tetragonal phase before sintering and an orthorhombi...
Embodiment 3
[0032] Weigh 0.8g BiF respectively 3 , 0.2g carbon nanotubes and 1.0g BaSnF 4 or PbSnF 4 , under the protection of nitrogen, the ball milling speed is 200rpm, the ball milling time is 2h, and the obtained ball milling product is dried at 60°C for 3h to prepare BiF 3 Composite cathode material. in image 3 (a) is BiF of this embodiment 3 / BaSnF 4 / SEM image of carbon nanotube composite cathode material, image 3 (d) is BiF of this embodiment 3 / PbSnF 4 / SEM image of carbon nanotube composite cathode material. SEM images show that the electrolyte, electrode materials, and carbon nanotubes are evenly distributed. Weigh 1.0g Sn, 0.2g carbon nanotube and 0.8g BaSnF 4 or PbSnF 4 , under the protection of argon, the ball milling speed was 150rpm, the ball milling time was 4h, and the obtained ball milling product was dried at 70°C for 2h to prepare the Sn composite negative electrode material. in image 3 (c) is the Sn / BaSnF of this embodiment 4 / SEM image of carbon nan...
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