For very fast synthesis of particle , the structural and kinetic information is not accessible in situ by conventional characterization methods. In our present work, an experiment setup based on rapid mixing of the reactants through a continuous millifluidics flow which transforms the space resolution in a time resolution has been built. It enables us to perform in situ UV and SAXS measurements during the continuous synthesis of gold nanoparticles. A synthesis of gold nanoparticles using ascorbic acid has been adapted to this microfluidic device. A series of experiments was performed in which pH of the ascorbic acid, ratio, and precursor concentrations were varied. In a first experiment on SWING(SOLEIL) on this system, the full kinetics was followed by in situ UV and SAXS. The number density, sizes, size distributions and volume fraction of AuNP have been obtained through the quantitative analyze of the SAXS data on an absolute scattering scale. The disappearance of the Au(III) and ascorbic acid species was obtained from their UV signature. – The combined in situ chemical speciation of Au(III) and in situ nanoparticles formation were identified to fully understand the influences on the nucleation and growth.
References:
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[3]F.Hubert et al. Langmuir 24 (17) 9219–9222 2008
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