Multipulse electrodeposition of Ag nanoparticles on HOPG monitored by in-situ by Small-Angle X-ray Scattering

A new experimental approach to study nanoparticle size distributions in electrochemical deposition processes by in-situ Small Angle X-ray Scattering (SAXS) is presented. A specifically designed flow cell was used to acquire SAXS frames after different nucleation and growth pulses in a potentiostatic multiple pulse approach. Measurements show that after a correct background subtraction, scattered intensity variations are only caused by electrodeposited silver nanoparticles and that size distribution evolution derived after modeling the SAXS data is in agreement with electrochemical particle growth.