In situ XAFS experiments using a microfluidic cell: application to initial growth of CdSe nanocrystals

The design and performance of a compact fluorescense XAFS apparatus equipped with a microfluidic cell for in situ studies of nanoparticles are described. CdSe nanoparticles were prepared by solution reaction starting from trioctylphosphine-Se. Time-resolved experiments were performed by precisely controlling the reactor coordinates (x,y), allowing the synchrotron X-ray beam to travel along a reactor channel, covering nucleation and initial growth of nanoparticles. Detailed analysis of EXAFS data combined with UV-vis spectra allow reliable estimation of particle size and density in the initial growth that cannot be accessible by conventional optical techniques based on a long-range order. The Se K-XANES spectra are interpreted by multi-scattering calculations providing bond formation kinetics consistent with the EXAFS data.