In situ Electrochemical Small-Angle Neutron Scattering (eSANS) for Quantitative Structure and Redox Properties of Nanoparticles.

The rapid growth in nanomaterial applications have revealed limitations in available physicochemical characterization methods. An in situ electrochemical small-angle neutron scattering (eSANS) methodology was devised that enables direct measurements of nanomaterial dispersion structure while undergoing reduction-oxidation (redox) reactions at the vitreous carbon electrode. Furthermore, these porous electrodes are amenable to contrast-variant neutron scattering strategies to measure nanoparticle structure and polymer conformation in multicomponent systems. The eSANS method was tested for feasibility by characterizing ZnO nanoparticles in 50 mmol/L NaCl deuterium oxide solution undergoing bulk electrolysis at negative potentials. Irreversible nanoparticle structural changes are observed during the potential cycle. The complete reduction of Zn(2+) to Zn(0) nanoparticles is unlikely, but a peak in the characteristic correlation length occurs during the redox bias with reduced average characteristic size.