The polycrystals of CdCl2-PbCl2 (CCPC) were prepared by the high temperature method in the horizontal tubular furnace of variable temperature zone. The cell parameters were determined through proszki software using powder XRD data where the crystal system was found to be monoclinic with a=15.328(+/-0.005), b=5.920(+/-0.011), c=9.728(+/-0.004) Angstrom and alpha=90degrees, beta=106.010(+/-0.037)degrees, gamma=90degrees, V=848.61 Angstrom(3). The TG analysis showed that it melts at 773 K and volatizes thereafter. The endothermic and exothermic peaks at 523 and 623 K, respectively, in DSC are due to structural change in the crystals during heating. The cell parameter of the crystal heated at 523 and 623 K and cooled to room temperature was found to be monoclinic with the same parameters given above. The temperature variation electrical conductivity of the sample in the temperature range (323-473 K) showed that there was a sudden increase in the current at 465 K and the activation energy of CCPC was found to be 0.53 eV. (C) 2003 Elsevier Science B.V. All rights reserved.