A series of nine bulk crystals of the Zn4 - xCd xSb3 compounds (x = 0-2.00 with 0.25 step) has been successfully synthesized and the detailed crystal structure has been refined by powder XRD study using the Rietveld method including the quantitative analysis. The substitution limit of the Cd atoms for the Zn4 - xCd xSb3 system has been extended to x = 2.00 by employing the vacuum casting method without annealing. The purities and densities of the bulk crystals exceeded approximately 96 mass% and 95% of XRD density, respectively. The lattice parameters of the a and c-axes in the system increase linearly with increasing Cd content x with obeying the Vegard law.
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