Polycrystalline Ca beta''-alumina was produced in a relatively gentle
way by increasing stepwise the Ca content of (Na, Ca) beta''-alumina i
n suitable mixtures of molten salts (Ca(NO3)(2) and CaCl2). When deter
mining the conductivity of Ca beta''-alumina as a function of temperat
ure by the four-probe technique, an irreversible decrease of the condu
ctivity was observed in subsequent measurements if the temperature dur
ing the first conductivity measurement was extended beyond 600 degrees
C. Impedance measurements on such samples demonstrated that the condu
ctivity decrease was due to an increase of the contribution of the gra
in boundary resistivity to the total specific resistivity.