Abstract 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.

中文翻译：

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合成参数对电沉积Zn-Sb薄膜组成和形貌的影响

摘要 基于 FE-SEM、EDS、XRD 证明了电解槽中电解液浓度、电沉积电位和流体动力学条件对合成的 Zn、Sb 和 Zn-Sb 薄膜的形貌、化学成分和晶体结构的影响。 ，和拉曼测量。发现工作电极电位的增加导致形成具有更高原子百分比 (at.%) 锌的薄膜。相反，增加柠檬酸盐浴中 SbCl3 的浓度和应用电解液搅拌，导致含有较高锑含量的薄膜优先电沉积。从热电应用的角度来看，最有前途的材料是含有 ZnSb 晶相且 Zn/Sb 原子比为 1 的材料。在没有电解液搅拌的情况下，在含有 0.045 M ZnCl 2 和 0.045 M SbCl 3 的柠檬酸盐浴中，Zn-Sb 薄膜电沉积的最佳结果是在 -1.5 V vs. Ag/AgCl (3 M KCl) 下观察到的。结果，获得了Zn/Sb原子比为1.03的非晶ZnSb薄膜。成分非常接近化学计量的 ZnSb 的样品在惰性气氛中退火，以将其转变为结晶薄膜。