The NASICON-type compound La1/3Zr2(PO4)3 has been studied by thermal X-ray diffraction. It was
found to exhibit, around 1000 °C, a reversible phase transition from P3̄ to P3̄c1 due to a modification of
the lanthanum distribution in the [Zr2(PO4)3]- network. This evolution was confirmed by 31P NMR experiments performed on quenched La1/3Zr2(PO4)3 samples (T = 700 and 1000 °C) and compared to room-temperature results. To complete this study, impedance spectroscopy measurements were carried out
between 330 and 730 °C, confirming the La3+ mobility in the NASICON network.
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