Abstract
We demonstrate quantification of porosity, nanopore tortuosity, and electrical connectivity at the single-nanoparticle (NP) level for NPs synthesized by nanodroplet-mediated electrodeposition. Focused ion beam nanoslice tomography was used to slice NPs with ca. 10 nm slice resolution followed by imaging using scanning electron microscopy (SEM), allowing measurement of these parameters on NPs not amenable to transmission electron microscopy. Slices were reconstructed in three dimensions and revealed pores with an average size of 3 ± 2 nm and relative nanopore tortuosity of 46.8 ± 24.5. We also demonstrate a new technique to evaluate electrical connectivity at the single-NP level by taking advantage of material-selective electrodeposition. The rate of Cu electrodeposition differs significantly on Pt compared to carbon, implying Cu can be selectively electrodeposited onto Pt NPs adsorbed onto a carbon support. Following the Cu electrodeposition step, NP connectivity was determined by the presence of Cu on Pt...
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