Volume 86
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Aßmann, S., Huber, F. J. T., & Will, S. (2024). In situ characterization of particle formation in spray flame synthesis using wide-angle light scattering. Particuology, 86, 304-312. https://doi.org/10.1016/j.partic.2023.07.013
In situ characterization of particle formation in spray flame synthesis using wide-angle light scattering
Simon Aßmann a b c, Franz J.T. Huber a b c *, Stefan Will a b c
a Lehrstuhl für Technische Thermodynamik (LTT), Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), Erlangen, 91058, Germany
b Erlangen Graduate School in Advanced Optical Technologies (SAOT), Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), Erlangen, 91052, Germany
c Competence Unit Engineering of Advanced Materials (EAM), Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), Erlangen, 91052, Germany
10.1016/j.partic.2023.07.013
Volume 86, March 2024, Pages 304-312
Received 31 January 2023, Revised 23 June 2023, Accepted 22 July 2023, Available online 28 July 2023, Version of Record 5 August 2023.
E-mail: franz.huber@fau.de

Highlights

• In situ characterization of spray flame synthesis using wide-angle light scattering.

• Distinction between scattering of droplets and nanoparticles of different morphology.

• Observation of different morphologies for titania and iron oxide nanoparticles.


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.

Graphical abstract
Keywords
Spray flame synthesis; Metal oxide particles; Elastic light scattering; Droplet size distribution; Nanoparticle morphology; Particle size distribution