Electrical materials incorporating lanthanide ions have great potential as electro-optical multifunctional systems. Polycrystalline NASICON (sodium silicon conductor) fast-ion conductors (Na5LnSi4O12, Ln = Eu, Tb) have been prepared via solid-state synthesis. These materials have been characterized by photoluminescence spectroscopy, including steady-state emission and excitation spectra, and measurement of the lifetimes of the excited states. Two Eu3+ sites have been detected: (i) in regular framework positions, and (ii) replacing Na+ ions in the tunnels. Samples containing only Eu3+ or Tb3+ emit mainly from one transition, respectively, 5D0
→
7F2 (610 nm, red) and 5D4
→
7F5 (550 nm, green). Mixed lanthanide samples, Na5Eu0.75Tb0.25Si4O12 and Na5Eu0.25Tb0.75Si4O12, have also been prepared and efficient Tb → Eu energy transfer has been observed for the latter.
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