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. 2021 Dec 20;7(1):761-772.
doi: 10.1021/acsomega.1c05293. eCollection 2022 Jan 11.

Reaction Mechanisms of the Electrosynthesis of Magnetite Nanoparticles Studied by Electrochemical Impedance Spectroscopy

Rubí Reséndiz-Ramírez  1 , Aarón Rodríguez-López  2 , Jesús A Díaz-Real  1 , Humberto F Delgado-Arenas  1 , Azucena Osornio-Villa  1 , Rosalba Hernández-Leos  3 , Vincent Vivier  4 , René Antaño-López  1
Affiliations

Reaction Mechanisms of the Electrosynthesis of Magnetite Nanoparticles Studied by Electrochemical Impedance Spectroscopy

Rubí Reséndiz-Ramírez et al. ACS Omega. .

Abstract

This work presents a mechanistic study of the electrochemical synthesis of magnetite nanoparticles (NPs) based on the analysis of the electrochemical impedance spectroscopy (EIS) technique. After a discussion of the mechanisms reported in the literature, three models are devised and a prediction of their EIS spectra is presented. The approach consisted of the simulation of EIS spectra as a tool for assessing model validity, as EIS allows to characterize the relaxation of adsorbed intermediates. The comparison between the simulated impedance spectra and the experimental results shows that the mechanisms proposed to date do not explain all of the experimental results. Thus, a new model is proposed, in which up to three adsorbed intermediate species are involved. This model accounts for the number of loops found in experimental impedance data. The closest approximation of the features found in the experimental spectra by this proposed model suggests a better representation of the reaction mechanism within the evaluated potential range.

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Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
Equivalent circuit representing the total impedance for the system.
Figure 2
Figure 2
Nyquist diagrams of EIS response simulated for model I for different values of E: (a) 0, (b) 50 mV, (c) 100 mV, (d) 150 mV, (e) 200 mV, and (f) variation of θ1 and θ2 with E. Parameters used for these simulations are summarized in Table 1.
Figure 3
Figure 3
Nyquist diagrams of EIS response simulated for model II for different values of E: (a) 0, (b) 50 mV, (c) 100 mV, (d) 150 mV, (e) 200 mV, and (f) variation of θ1 with E. Parameters used for these simulations are summarized in Table 3.
Figure 4
Figure 4
Nyquist diagrams of EIS response simulated for model III for different values of E: (a) 0, (b) 50 mV, (c) 100 mV, (d) 150 mV, (e) 200 mV, and (f) variation of θ1 with E. Parameters used for these simulations are summarized in Table 5.
Figure 5
Figure 5
(a) Experimental Nyquist diagrams at different potentials of anodic polarization (−880, −860, −840, −820, −760, and −740 vs Hg|Hg2SO4) in 0.1 M K2SO4 using a 98% purity iron bar as the working electrode. (b) Magnification of the shaded area in (a). (c) Single response for −840 mV vs Hg|Hg2SO4. (d) Magnification of the shaded area in (c).
Figure 6
Figure 6
Nyquist diagrams showing experimental data compared with the simulated one for the proposed model at different values of E: (a) 60 and (b) 80 mV. Parameters used for these simulations are summarized in Table 8.
See this image and copyright information in PMC

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