Scalable fractionation of iron oxide nanoparticles using a CO₂ gas-expanded liquid system

Iron oxide nanoparticles exhibit highly size-dependent physicochemical properties that are important in applications such as catalysis and environmental remediation. In order for these size-dependent properties to be effectively harnessed for industrial applications scalable and cost-effective techniques for size-controlled synthesis or size separation must be developed. The synthesis of monodisperse iron oxide nanoparticles can be a prohibitively expensive process on a large scale. An alternative involves the use of inexpensive synthesis procedures followed by a size-selective processing technique. While there are many techniques available to fractionate nanoparticles, many of the techniques are unable to efficiently fractionate iron oxide nanoparticles in a scalable and inexpensive manner. A scalable apparatus capable of fractionating large quantities of iron oxide nanoparticles into distinct fractions of different sizes and size distributions has been developed. Polydisperse iron oxide nanoparticles (2–20 nm) coated with oleic acid used in this study were synthesized using a simple and inexpensive version of the popular coprecipitation technique. This apparatus uses hexane as a CO₂ gas-expanded liquid to controllably precipitate nanoparticles inside a 1L high-pressure reactor. This paper demonstrates the operation of this new apparatus and for the first time shows the successful fractionation results on a system of metal oxide nanoparticles, with initial nanoparticle concentrations in the gram-scale. The analysis of the obtained fractions was performed using transmission electron microscopy and dynamic light scattering. The use of this simple apparatus provides a pathway to separate large quantities of iron oxide nanoparticles based upon their size for use in various industrial applications.