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Romanticism and administration mining, galvanism and oversight in Alexander von Humboldt's global physics.
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Rapid Quantification of Film Thickness and Metal Loading for Electrocatalytic Metal Oxide Films
The thicknesses and metal loadings
of amorphous nickel, iron, and
iridium oxide films widely used for solar fuel electrocatalysis were
determined by cross-sectional scanning electron microscopy (SEM) and
X-ray fluorescence (XRF) spectroscopy measurements. The thicknesses
for a series of films, which were systematically varied from 10 to
400 nm using photodeposition techniques, were accurately measured
by cross-sectional SEM using a protocol that successfully resolves
the relevant catalyst layers. XRF measurements recorded on each of
the films provided a strong linear correlation (<i>R</i><sup>2</sup> > 0.97) with the thicknesses determined by cross-sectional
SEM. The electrochemical surface areas (ECSAs) determined by double-layer
capacitance measurements, a technique widely used in the electrocatalysis
community, showed a linear relationship for iridium oxide film thicknesses
but not with those consisting of nickel and iron. These results highlight
the limitations of using ECSA to determine catalyst film thicknesses
and metal loadings. The noninvasive XRF technique is demonstrated
to be a far superior method for reporting on the thickness and loadings
of thin metal oxide films