“…A bulky quantity of nanomaterials is, however, not necessary for many applications. For example, in surface-enhanced Raman spectroscopy (SERS) and in many catalysis-related applications, no more than a monolayer of nanoparticles is required. ,, Electrochemical (EC) methods represent one of the promising approaches to the additive-free synthesis of a dispersed monolayer of shape- and size-controlled crystalline nanoparticles in aqueous phase under ambient conditions. − In EC-based methods, both the thermodynamics and kinetics of the particle nucleation and growth are controllable via adjusting deposition potential, current, and/or their time-gauged variation in pulse forms. − Compared with many other routinely used EC methods, square-wave voltammetry (SWV) is a much less studied technique in the electrocrystallization of nanomaterials, despite its extensive applications in the electroanalysis for sensitivity enhancement. − SWV was employed recently in the fabrication of Pt nanocrystals and nanothorns, , Pd nanothorns, Ag dendrites, Au microflowers, and Zn and Cu nano-/microstructures. , Neither the effects of individually adjustable parameters in SWV to the structure of fabricated nanocrystals nor the comparison with other conventional nonpulsed and pulsed voltammetric and amperometric techniques were reported.…”