Publication date: 10th April 2024
Recently, fluoride ion (F-) conducting ceramics attract attention as solid electrolytes to be used in fluoride batteries. In the present study, fluoride ion conducting behavior in ceramics, MSnF4 (M = Pb, Ba) with the fluorite-type-related structure was investigated in order to think of a strategy for the development of fast ion conductors. Especially, enhancing the ionic conductivity by using a mechanochemical synthesis was examined. A pellet was prepared by employing a mechanical milling (MM) process using MF2 (M = Pb, Ba) and SnF2 powders, followed by the post-annealing. These electrical conductivities were evaluated by an impedance method. First, (Ba1-xSnx)F2 (BSF) fluorides were prepared via a MM process by changing chemical composition, impurity element concentration, milling media, weight ratios of ball to powder (B/P), and milling time. We succeeded in obtaining the highest conductive BSF. These BaF2-based electrolytes are successful candidates for the electrolyte materials in high performance fluoride batteries. In addition, ion conducting behavior of the well-known highest fluoride ion conductor: PbSnF4 (PSF) was reinvestigated. In the study, PSF specimens were obtained via two kinds of the firing process under (i) Ar-flowing or (ii) Ar-atmosphere gas-tight conditions. In addition, low-temperature annealing just after the milling process was also considered. X-ray diffraction (XRD) patterns of PSF samples via MM, followed by the post-annealing show that a tetragonal PSF phase was mainly obtained. Electrical conductivities were high enough to be applied to a solid electrolyte of room temperature-operating fluoride battery. We found that the low-temperature annealing was effective to enhance the conductivity of the PSF specimens. In a closer look at the XRD patterns, the relative intensity for the reflection peak of 00ℓ planes seems to be related to its conductivity. The conductivity increases with decrease in the ratio of the peak intensity of 00ℓ planes to that of the main peak. The reason for this needs to be clarified in the near future by using the detailed crystal structure refinement.
This work was supported by a project, JPNP21006, commissioned by the New Energy and Industrial Technology Development Organization (NEDO).
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