Electrodeposition of Versatile Nanostructured Sb/Sb₂O₃ Microcomposites: A Parameter Study

Abstract

Antimony (Sb) and its oxides are considered to be promising materials for numerous applications, such as secondary batteries, catalysis, and thermoelectrics. Recent studies show that Sb/Sb2O3 composites can easily be prepared by electrochemical deposition. In the present work, the impact of process parameters, such as flow conditions, substrate roughness, and current‐potential modulations, on the properties of the Sb/Sb2O3 deposits are investigated. The deposits are characterized by electron microscopy including energy‐dispersive X‐ray spectroscopy analysis as well as X‐ray diffraction and Raman spectroscopy. The systematic investigations on the process parameters reveal that the size, morphology, and composition of the resulting Sb/Sb2O3 composites can be adjusted in a wide range. The insights of this parameter study imply a huge design freedom for the electrochemical formation of nanostructured Sb/Sb2O3 composites, allowing straightforward implementation of rational designs depending on a desired application.

In situ electrogenerated Cu(III) triggers hydroxyl radical production on the Cu-Sb-SnO 2 electrode for highly efficient water decontamination

“…As shown in Fig. 2 D , there were characteristic peaks of Sn-O and Sb-O vibration mode in the Raman spectra of the electrodes ( 39 – 41 ). A new Raman peak corresponding to Cu-O vibration appeared at approximately 628 cm −1 after Cu doping ( 42 ).…”

Structural Control of Electrodeposited Sb Anodes through Solution Additives and Their Influence on Electrochemical Performance in Na-Ion Batteries

“…53 Despite the tunability that can be acheived through these organic additives, there are few publications reporting the tunability of electrodeposited Sb anodes for battery applications using solution additives. 7,54 Herein we report the effect of solution additives, such as CTAB and SPS, on the electrodeposition of Sb anodes in aqueous-based electrolyte baths and the subsequent impacts on the electrodes electrochemical performance in a sodium-ion battery (NIB). We report that both CTAB and SPS can dramatically influence the morphology and crystallinity of the deposited films.…”

“…As a result, brighteners can also help level the micro profile of the electrode surface without the need for polishing after the deposition. , Additives, such as bis­(3-sulfopropyl) disulfide (SPS) that acts a brightner, − and sodium gluconate, , are typically used in copper and nickel plating baths, respectively, and an extensive library of additives have been investigated for other metal depositions. ,, Surfactants, such as cetyltrimethylammonium bromide (CTAB), have also been used in deposition baths due to their potential to affect the surface tension between the electrolyte and the electrode and can have effects on coating adhesiveness and morphology at varying concentrations. , Depending on the interactions of CTAB with the substrate or the active metal being deposited, it may act as a leveling or brightening agent. − Additonally, CTAB can interact directly with the deposited metal instead of the substrate and has been used to cap the growth of particles as demonstrated in nanoparticle synthesis − and also has the potential to act as a corrosion inhibitor . Despite the tunability that can be acheived through these organic additives, there are few publications reporting the tunability of electrodeposited Sb anodes for battery applications using solution additives. , …”

“…Antimony (Sb) anodes for both sodium-ion and lithium-ion batteries have been extensively studied due to its high theoretical capacity (660 mAh/g) and electronic conductivity. − Studies have reported high reversible capacities and have implemented the use of conductive additives − and nanostructuring , to overcome issues related to mechanical stability, induced by volume expansion that occurs when Sb alloys with either sodium or lithium. To test and optimize the properties and performance of Sb, a variety of synthetic and fabrication techniques have been utilized.…”

“…A less prevalent technique previously reported by our group utilizes electrodeposition to synthesize Sb based anodes. ,− Through electrodeposition, Sb ions are plated electrochemically from solution onto a charged substrate. , This technique does not require binders and additives, which are necessary in slurry casted films, and vastly simplifies the understanding of the inherent properties of Sb anodes by removing the need to deconvolute the role of binders and additives . In addition, electrodeposition has been found to be a valuable technique to control composition, film thickness, crystallinity, and morphology of the deposited metal. ,− This control can be accomplished by a multitude of experimental parameters (temperature, bath composition, current density, etc.) as well as the use of different solution additives …”