Maghemite nanoparticles synthesis via spray flame synthesis and particle characterization by hole in a tube sampling and scanning mobility particle sizing (HIAT-SMPS)

Abstract

In order to standardize spray flame synthesis (SFS) studies, intensive work has been done in recent years on the design of burner types. Thus, in 2019, the so-called SpraySyn1 burner was introduced (SS1), which was subsequently characterized in numerical and experimental studies. Based on this research, a modification of the nozzle design was proposed, which has now been considered in the successor model, SpraySyn2 (SS2). As little is known about the effect of the nozzle adaptation on the particle formation, we operated both burners under identical operating conditions to produce maghemite. The final powder comparison showed that SS2 yielded considerable higher specific surface areas (associated with smaller primary particle sizes), lower polydispersity, and higher phase purity. To obtain further information on the size distributions of aggregates and agglomerates generated by SS2, aerosol samples were extracted by hole in a tube (HIAT) sampling and characterized by scanning mobility particle sizing (SMPS). Samples were extracted along the centerline at different heights above the burner (HAB) above the visible flame tip (>7 cm), and quenching experiments were performed to extract the aerosol samples at different dilution rates. Thereby, it was demonstrated that performing detailed quenching experiments is crucial for obtaining representative HIAT-SMPS data. In particular, agglomerates/aggregate sizes were overestimated by up to ∼70 % if samples were not sufficiently diluted. If sufficient dilution was applied, distribution widths and mean particle mobility diameters were determined with high accuracy (sample standard derivation <5 %). Our data suggested the evolution of primary particle sizes was mostly completed <7 cm HAB and it was shown aggregates/agglomerates present above the visible flame were compact in structure (non-fractal). The mean diameter of the particle ensemble grew along the centerline from 6.9 nm (7 cm) to 11.4 nm (15 cm), while distribution widths grew from 1.42 to 1.52.