Journal of Industrial and Engineering Chemistry, Vol.84, 202-216, April, 2020
Influence of synthesis parameters on composition and morphology of electrodeposited Zn-Sb thin films
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The influence of bath concentration, electrodeposition potential, and hydrodynamic conditions in the electrolytic cell on the morphology, chemical composition, and crystal structure of synthesized Zn, Sb, and Zn-Sb thin films was demonstrated based on FE-SEM, EDS, XRD, and Raman measurements. It was found that an increase in the working electrode potential leads to the formation of thin films with a higher atomic percentage (at.%) of zinc. Contrary, increasing SbCl3 concentration in the citrate bath and application of electrolyte stirring, lead to the preferential electrodeposition of thin films containing a higher content of antimony. From the point of view of thermoelectric applications, the most promising material was that containing the ZnSb crystal phase with the Zn/Sb atomic ratio of 1. The best results for electrodeposition of Zn-Sb thin films were observed at -1.5 V vs. Ag/AgCl (3 M KCl) in the citrate bath containing 0.045 M ZnCl2 and 0.045 M SbCl3 in the absence of electrolyte stirring. As a result, an amorphous ZnSb thin film with the Zn/Sb atomic ratio of 1.03 was obtained. The sample with a composition very close to stoichiometric ZnSb was annealed in an inert atmosphere in order to transform it into a crystalline thin film.
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