The influence of annealing on the microstructure and electrical properties of undoped polycrystalline ZnSb samples has been investigated by different experimental techniques. In situ XRD in an argon at- mosphere showed that ZnSb powders decompose at 300 C, which is attributed to Zn evaporation. In situ SEM in a moist atmosphere showed fast surface deterioration at 450 C and above, reflecting decom- position of ZnSb and the formation of metallic Sb precipitates. The rate of Zn loss in a reducing atmo- sphere was determined by thermogravimetry and related to the Zn partial vapor pressure. The increase of the hole carrier concentration of ZnSb measured at room temperature after heat treatment was correlated with Zn evaporation at elevated temperature. The carrier concentration after annealing at 400 C is consistent with an activation energy for Zn vacancy formation of 0.4 eV and a maximum Zn deficiency x of Zn1-xSb of 1 10 3.
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