Electrochemical impedance spectroscopy in the presence of non-linear distortions and non-stationary behaviourPart I: theory and validation

Gheem, Els Van; Pintelon, Rik; Vereecken, Jean; Schoukens, Joannes; Hubin, Annick; Verboven, Peter; Blajiev, Orlin

doi:10.1016/s0013-4686(04)00558-4

Cited by 23 publications

(25 citation statements)

References 26 publications

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“…A great number of works have studied the effects of the non-fulfilment of the linearity condition: some examples of these works are the works of Darowicki and co-workers [51,[57][58][59]; the works of Diard and co-workers [60][61][62][63][64][65]; and the works of Van Gheem's team [66][67]. It has been shown that the main effect of nonlinearity is the generation of non-fundamental harmonics in the output signal [68].…”

Section: Introductionmentioning

confidence: 99%

Harmonic analysis based method for linearity assessment and noise quantification in electrochemical impedance spectroscopy measurements: Theoretical formulation and experimental validation for Tafelian systems

Giner-Sanz

Ortega

Pérez-Herranz

2016

Electrochimica Acta

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ElsevierGiner-Sanz, JJ.; Ortega Navarro, EM.; Pérez-Herranz, V. (2016). Harmonic analysis based method for linearity assessment and noise quantification in electrochemical impedance spectroscopy measurements: Theoretical formulation and experimental validation for Tafelian systems. Abstract:Electrochemical Impedance Spectroscopy (EIS) is an electrochemical measurement technique that has been applied to a broad range of applications. Three conditions must be fulfilled in order to obtain valid EIS measurements: causality, linearity and stationarity. The non fulfilment of any of these conditions may lead to distorted and biased EIS spectra. Consequently, the verification of the four fundamental conditions is mandatory before accepting any results extracted from an EIS spectrum. In this work, a harmonic analysis based method for linearity assessment and noise quantification in EIS measurements is presented, and validated both from an experimental point of view and from a theoretical point of view, for Tafelian systems. It was shown that the presented method was able to quantitatively assess the nonlinearity of the system; and to quantify and characterize the noise. Moreover, the presented method is able to determine the threshold frequency of the system above which the system does not present significant nonlinear effects even for very large perturbation amplitudes.

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Section: Introductionmentioning

confidence: 99%

Harmonic analysis based method for linearity assessment and noise quantification in electrochemical impedance spectroscopy measurements: Theoretical formulation and experimental validation for Tafelian systems

Giner-Sanz

Ortega

Pérez-Herranz

2016

Electrochimica Acta

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“…There is a large number of works in literature that show that the non-fulfilment of the linearity condition leads to the generation of non-fundamental harmonics in the output signal. Some of such works are the works of Darowicki and co-workers [53,[55][56], Victoria and Ramanathan [57], Diard and co-workers [58][59][60][61][62][63], and Van Gheem's team [64][65]. When a mono-frequency sinusoidal perturbation signal is applied to a linear system, a mono-frequency output signal of same frequency is obtained [66].…”

Section: Introductionmentioning

confidence: 99%

Application of a Montecarlo based quantitative Kramers-Kronig test for linearity assessment of EIS measurements

Giner-Sanz

Ortega

Pérez-Herranz

2016

Electrochimica Acta

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Electrochemical Impedance Spectroscopy (EIS) is a very powerful tool to study the behaviour of electrochemical systems. Three conditions must be fulfilled during EIS measurements: causality, linearity, and stability. If any of these conditions is not achieved, then the conclusions obtained from the analysis of the measured spectra may be biased, or even misguided. For this reason, the verification of the compliance of these conditions is critical before accepting any analysis performed on an experimental spectrum. In a previous work, an experimental spectrum quantitative validation technique based on Kramers-Kronig relations was presented. The validation method consists in a Kramers-Kronig (KK) validation test, by equivalent electrical circuit fitting, coupled with a Montecarlo error propagation method. The validation technique builds a consistency region for a given confidence level that allows to discriminate between the individual points of the EIS spectrum that are consistent with the four fundamental hypotheses, and the inconsistent ones. The aim of this work is to validate experimentally if the quantitative validation technique is able to detect nonlinearities. In order to achieve this goal, the EIS spectrum of a markedly nonlinear system was measured experimentally using different perturbation amplitudes. The validation technique was applied to each one of the measured spectra. The method successfully managed to identify large nonlinearities; but did not detect slight ones.

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“…For most of the samples, after longer immersion periods, the LF impedance decrease is accompanied by oscillations in the phase angle. This can be associated with the onset of localized corrosion, the potential spikes characteristic of this type of corrosion leads to a nonstationary transient behaviour leading to a distortion in the impedance spectrum . The extent of the LF impedance drop with immersion time was different among the samples, indicating different protective properties of the precipitated products.…”

Section: Eis Measurementsmentioning

confidence: 99%

EIS investigation of a Ce‐based posttreatment step on the corrosion behaviour of Alclad AA2024 anodized in TSA

Ramirez

Queiroz

Terada

et al. 2019

Surface & Interface Analysis

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In the aircraft industry, anodizing and posttreatment steps use Cr (VI) compounds, which, despite offering good corrosion resistance and self‐healing properties, are highly toxic and carcinogenic. Ce compounds are recognized as efficient corrosion inhibitors for Al alloys, and several works report self‐healing ability for these chemicals. In this investigation, the corrosion resistance of Alclad AA2024‐T3 alloy anodized in tartaric‐sulphuric acid (TSA) bath and posttreated in a solution comprising cerium nitrate without and with hydrogen peroxide was evaluated. The purpose is to investigate the potentiality of using hydrothermal treatment in Ce nitrate solution as candidate to replace Cr (VI) posttreatment. The aim is to provide a posttreatment step which, while improving the corrosion resistance, does not plug the mouths of the pores maintaining the adhesion properties of the porous anodic layer. Microstructural characterization was carried out by SEM‐EDS whereas corrosion resistance was evaluated by EIS. The surface analysis showed that the posttreatments, all performed at 50°C, kept the open structure of the pores. EIS analysis showed that the posttreatments performed in the H2O2 solution for short immersion times were the most effective in improving the corrosion resistance of the samples, whereas electrical equivalent circuit (EEC) fitting of the data indicated sealing of the porous layer during the immersion of the different samples in the test solution. SEM‐EDS analysis of the samples posttreated in the H2O2 containing solution, prior and after the corrosion test, showed the presence of Ce oxy‐hydroxide randomly deposited on the sample surface, indicating that Ce could be incorporated/stored in the anodic layer.

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Electrochemical impedance spectroscopy in the presence of non-linear distortions and non-stationary behaviourPart I: theory and validation

Cited by 23 publications

References 26 publications

Harmonic analysis based method for linearity assessment and noise quantification in electrochemical impedance spectroscopy measurements: Theoretical formulation and experimental validation for Tafelian systems

Harmonic analysis based method for linearity assessment and noise quantification in electrochemical impedance spectroscopy measurements: Theoretical formulation and experimental validation for Tafelian systems

Application of a Montecarlo based quantitative Kramers-Kronig test for linearity assessment of EIS measurements

EIS investigation of a Ce‐based posttreatment step on the corrosion behaviour of Alclad AA2024 anodized in TSA

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