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ElsevierGiner Sanz, JJ.; Ortega Navarro, EM.; Pérez-Herranz, V. (2015). Total harmonic distortion based method for linearity assessment in electrochemical systems in the context of EIS. Electrochimica Acta. 186:598-612. doi:10.1016Acta. 186:598-612. doi:10. /j.electacta.2015 Electrochemical Impedance Spectroscopy (EIS) is a widely used electrochemical measurement technique that has been used in a great spectrum of fields since it allows deconvolving the individual physic-chemical processes that take place in a given system. Ohm's generalized law, and thus the impedance concept, are only valid if 4 conditions are fulfilled: causality, finiteness, stationarity and linearity. In the case that any of these conditions is not achieved, the obtained impedance spectra will present distortions that may lead to biased or even erroneous results and conclusions. For this reason it is crucial to verify if the 4 conditions are fulfilled, before accepting the results extracted from impedance spectra. In this work, a linearity assessment quantitative method based in the total harmonic distortion (THD) parameter is presented and verified experimentally. The experimental validation of the implemented method showed that the implemented method is able to assess quantitatively the linearity of the system. In addition, it is also able to determine the threshold frequency above which the system will not present significant nonlinear effects even for large perturbation amplitudes. It was observed that the THD method is more sensitive to nonlinear effects than the spectra themselves.

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Three-dimensional (3D) porous nickel structures were fabricated via a double-template electrochemical deposition process. The construction of the foam structures was achieved by means of a hydrogen bubble dynamic template, prepared from Cu electrodeposition at high current densities. Subsequently, a Ni layer was electrodeposited on the Cu 3D template. During the nickel coating, the typical fingerlike microstructure of the Cu foam becomes denser and changes to a cauliflower microstructure. The hydrogen evolution reaction (HER) on these macroporous Ni electrodes was evaluated in 30 wt.% KOH solution by means of polarization curves and electrochemical impedance spectroscopy (EIS). Results demonstrate greater apparent activity of the developed electrodes towards HER in comparison with commercial smooth Ni electrode. The 3D porous Ni electrocatalyst obtained from Cu templates synthesized at the lowest current density and the highest electrodeposition time yielded the best electrochemical activity for HER.