The synthesis of pure and Sb₂O₃ ( 0 to 5% molar fraction ) doped ZnO has been realized by sublimation-condensation method in a solar furnace. The characterization of the initial and final powders was done by means of XRD and PL techniques.

The XRD obtained results showed: the formation of a new phase Zn₇O₂Sb₁₂ in the micropowders which disappears in the nanopowders. These results showed also a small increase of the grain size as a function of Sb₂O₃ concentration in the nanopowders. The analysis of the photoluminescence spectra allowed us to establish the following features: a decrease of D°X and D⁺X and an increase of A°X peaks when the Sb₂O₃ concentration increases for the micropowders and an increase of D⁺X and no change in A°X and no peak shift and a disappearance of X peak as far as nanopowders are concerned for all considered compositions.

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