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Influence of synthesis parameters on composition and morphology of electrodeposited Zn-Sb thin films
Journal of Industrial and Engineering Chemistry ( IF 5.9 ) Pub Date : 2020-04-01 , DOI: 10.1016/j.jiec.2019.12.035
Dominika Rajska , Kacper Motyka , Marcin Kozieł , Damian Chlebda , Agnieszka Brzózka , Grzegorz D. Sulka

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:

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。
更新日期:2020-04-01
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