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.