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All pellets were prepared by first grinding the samples into a homogeneous powder with a mortar and pestle. The powders (0.3 g) were then added to a standard 13 mm die, sandwiched between two porous carbon electrodes (Sigracet, GDL 10 BB, 1.222 cm diameter) and pressed at 5,000 kg for 2 min. All pellets were 13 mm in diameter and ranged in thickness from 1.30 to 1.38 mm. Measurements were performed using an impedance and gain-phase analyser (SI model 1260), 1 Hz¨C1 MHz, with a two-probe electrochemical cell equipped with platinum current collectors and an applied a.c. voltage of 10¨C100 mV (unless otherwise stated). Measurements were taken in the temperature range of 23 to 150 ¡æ in either an anhydrous H2 or D2 atmosphere.
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