Rapid growth in nanomaterial applications highlight limitations of available physicochemical characterization methods. An in situ electrochemical small-angle neutron scattering (eSANS) meth-odology was devised that enables direct measurements of nano-material dispersion structure while undergoing reduction-oxidation (redox) reactions at the vitreous carbon electrode. Further, these porous electrodes are amenable to contrast-variant neutron scattering strategies to measure nanoparticle structure and polymer conformation in multi-component systems. The eSANS method was tested for feasibility by characterizing ZnO nanoparticles in 50 mmol/L NaCl deuterium oxide solution un-dergoing bulk electrolysis at negative potentials. Irreversible nanoparticle structural changes are observed during the potential cycle. The complete reduction of Zn2+ to Zn0 nanoparticles is unlikely, but an increase in the correlation length occurs as a pre-cursor to substantial redox bias and reduced correlation length.
Citation: Journal of the American Chemical Society
Pub Type: Journals
nanoparticle, electrochemical, neutron scattering, toxicity, redox