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Morphological and chemical dynamics upon electrochemical cyclic sodiation of electrochromic tungsten oxide coatings extracted by in situ ellipsometry

Alexandre Zimmer, Mickaël Gilliot, Laurent Broch, Clotilde Boulanger, Nicolas Stein, and David Horwat

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Abstract

The sodiation–desodiation process of sputtered amorphous electrochromic tungsten oxide coatings in an aqueous-based medium was simultaneously monitored over 99 cycles by cyclic voltammetry and in situ spectroscopic ellipsometry. This allowed extracting the evolution of optical and geometrical parameters upon cycling. The resulting electrochemical coloring-bleaching process was dynamically fitted in the 1.8–2.8 eV optical range with a four-phase model including a constrained spline parametrization of the dielectric function. This allows real time access to thickness, surface roughness, and dielectric function of ${{\rm Na}_x}\!{{\rm WO}_3}$. The temporal evolution of the latter in the fully colored state was used to highlight the porosity extent of the probed coating of opened morphology. The designed spectroelectrochemical approach was applied to map the temporal evolution of the $\rm Na$ content (${x}$ in ${{\rm Na}_x}\!{{\rm WO}_3}$) during and between cycles, taking into account the intricate interplay between charge density, thickness, and electrolyte uptake.

© 2020 Optical Society of America

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Supplementary Material (11)

NameDescription
Visualization 1       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 5th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 2       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 10th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 3       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 20th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 4       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 30th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 5       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 40th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 6       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 50th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 7       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 60th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 8       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 70th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 9       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 80th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 10       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 90th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.
Visualization 11       Best-fitted evolution of the imaginary part of the pseudo-dielectric function for a representative sputtered amorphous WO3 coating during the 99th cycle of sodiation-desodiation. The video is accelerated 3.5 times. Total cycle duration: ca. 88 s.

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Figures (7)

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Equations (8)

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