Small angle X-ray scattering of particle growth and structure in spray flame synthesis

Abstract

Customized metal oxide nanoparticles are on increasing demand due to their high specific surface area coupled with their material properties. Spray flame synthesis (SFS) is able to produce such particles in high quantity and purity. However, the turbulent flame including droplets is a complex system. The analysis of the product is challenging due to the broad size distribution of the aggregated primary particles. Thus, this study combines small angle X-ray scattering (SAXS) with transmission electron microscopy (TEM) in order to gain valuable information about primary particle sizes and fractal properties. Insights about the particle formation is obtained by comparing the SAXS data of titanium oxide and iron oxide particles produced with a variety of precursors in different concentrations using two burner setups. Remarkably, all presented systems show a size distribution of the primary particle with two size fractions. The differences in the sizes and consequences for the gained information about the fractal dimensions are discussed in detail. This includes the overlap of scattering information and resolution limits. All particle structures include small particles of 5–8 nm pointing to a gas-to-particle pathway. The large particle fraction ranges from 35 to 320 nm depending on precursor composition and concentration. Their formation is likely linked to hydrolysis reactions of the precursor in spray droplets. For the aggregates, the fractal dimension of mass with values 1.6–1.8 point to diffusion-limited cluster aggregation which is typical for flame-made products. The evaluation of in situ studies with synchrotron radiation confirms the gas-to-particle pathway.