Flow cell coupled dynamic light scattering for real-time monitoring of nanoparticle size during liquid phase bottom-up synthesis

To tailor the properties of nanoparticles and nanocomposites, precise control over particle size is of vital importance. Real-time monitoring of particle size during bottom-up synthesis in liquids would allow a detailed study of particle nucleation and growth, which provides valuable insights in the mechanism of formation of the nanoparticles. Furthermore, it facilitates a rational scale-up, and would enable adequate intervention in the production process of nanoparticle dispersions to minimize the number of off-spec batches. Since real-time monitoring requires particle size measurements on dispersions in flow, conventional dynamic light scattering (DLS) techniques are not suited: they rely on single scattering and measure the Brownian motion of particles dispersed in a liquid. Here, we present a set-up that allows accurate measurements in real-time on flowing dispersions using a DLS technique based on modulated 3D cross-correlation. This technique uses two simultaneous light scattering experiments performed at the same scattering vector on the same sample volume in order to extract only the single scattering information common to both. We connected the reactor to a flow-cell in the DLS equipment using a tailor-made analysis loop, and successfully demonstrated the complete set-up through monitoring of the size of spherical silica nanoparticles during Stober synthesis in a water-alcohol mixture starting from the molecular precursor tetraethyl orthosilicate.