In situ characterization of particle formation in spray flame synthesis using wide-angle light scattering

Abstract

Wide-angle light scattering (WALS) was used for in situ measurements of droplet and nanoparticle size distributions during the synthesis of titania and iron oxide particles from liquid precursor solutions in the standardized SpraySyn burner for spray flame synthesis. Titania was synthesized from titanium tetraisopropoxide (TTIP) and iron oxide from iron(III) nitrate nonahydrate (INN) using ethanol (EtOH) as solvent. Scattering images were taken at heights up to 120 mm above the burner surface and classified into droplet and particle scattering. Droplet size distributions were derived from a sequential analysis of scattering data containing the oscillating Mie pattern, the lognormal size distribution parameters for spherical and fractal particle fractions from a multivariate approach on averaged particle scattering data. The results show that the precursor addition leads to altered evaporation behavior and even droplet disruption probably induced by puffing or micro-explosions compared to pure EtOH. In the case of TTIP (a hygroscopic alkoxide), the synthesis of a large fraction of spheres was observed, while the nitrate INN leads to the formation of mostly fractal aggregates.