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.

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► We study nanoparticle electrodeposition by in-situ Small Angle X-ray Scattering.
► Electrodeposition of Ag nanoparticles on HOPG in a specifically designed flow cell.
► Nanoparticle size distributions are obtained after correct treatment of SAXS data.
► Particle sizes derived from SAXS are in agreement with electrochemical measurements.
► In-situ SAXS is proven to be very promising to study nanoscale electrodeposition.