Electrochemical Techniques for Nanomaterials: A Critical Review of Production, Characterisation and Application
Ahmed M. Awad Abouelata *
Department of Chemical Engineering and Pilot Plant, Engineering Research and Renewable Energy Institute, National Research Center, Dokki 12622, Giza, Egypt.
*Author to whom correspondence should be addressed.
Abstract
Electrochemical techniques occupy an unusual position in nanomaterials science because the same interfacial phenomena can be used to manufacture nanoscale matter, interrogate its physicochemical behaviour and drive the reactions for which it is ultimately applied. This critical narrative review examines electrochemical routes for producing nanomaterials, the electrochemical methods used to characterise them, and the extent to which these approaches generate reliable structure-property-performance relationships. Literature published principally from 1 January 2000 to 30 June 2026 was critically synthesised, with seminal earlier studies included where necessary to establish mechanistic foundations. Electrodeposition, template-assisted growth, anodic self-organisation, electrochemical exfoliation, electrochemical dealloying and continuous particle electrosynthesis are compared in terms of controllability, throughput, defect generation, substrate dependence and scalability. Cyclic voltammetry, transient methods, electrochemical impedance spectroscopy, electrochemical quartz crystal microbalance measurements and scanning electrochemical cell microscopy are then evaluated according to what they directly measure and what is too often inferred from them. The evidence shows that electrochemical synthesis can provide strong control over local composition and morphology under relatively mild conditions, but nominal process variables are strongly coupled through mass transport, interfacial chemistry, nucleation and evolving surface area. Consequently, apparent performance gains in electrocatalysis, energy storage, sensing and separations may reflect accessibility, loading, wetting, transport or normalisation choices rather than intrinsic nanoscale activity. Scale-up remains possible, as demonstrated by continuous electrodeposition and industrially compatible anodisation concepts, but reproducibility, precursor utilisation, electrolyte management, metrology and device-level validation remain uneven. The most productive future direction is therefore not simply finer morphology control, but integrated electrochemical manufacturing with operando characterisation, statistically defensible benchmarking and process metrics that connect nanoscale design to durable, scalable function.
Keywords: Electrodeposition, anodisation, electrochemical exfoliation, dealloying, electrochemical impedance spectroscopy, nanostructures, electrocatalysis, operando characterisation