Layered double hydroxide (LDH) thin films with different chemical compositions (MgZnAl, MgZnGa, MgGaAl) and varying thicknesses were easily prepared by sol-gel method followed by dip-coating. Films were chemically uniform, transparent and well adhered to a conductive indium tin oxide (ITO) substrate. Structure, chemical composition and morphology of the thin films were characterized by XRD-GADDS, SEM-EDS and AFM. Additionally, the semiconducting properties of all the prepared films were studied through the Mott-Schottky relationship; such properties were closely related to the chemical compositions of the film. The films were characterized after electrochemical treatment and important modifications regarding surface morphology, particle and crystal sizes were observed. An in-depth study was conducted in order to investigate the effect of several different electrochemical treatments on the morphology, particle size distribution and crystal size of LDH thin films. Upon electrochemical treatment, the films' surface became smooth and the particles forming the films were transformed from flaky open LDH platelets to uniformly distributed close-packed LDH nanoparticles. (C) 2014 Elsevier B.V. All rights reserved.