Low-cost one-pot synthesis of hydrophobic and hydrophilic monodispersed iron oxide nanoparticles

Abstract

The synthesis of Superparamagnetic Iron Oxide Nanoparticles (SPIONs) with size and shape tunability, which is also industrially scalable, remains challenging. Surface functionalization of the nanoparticles is yet another active research subject. Although a variety of inorganic and organometallic precursors have been tried, which are demanding in terms of both cost and effort, the use of iron hydroxide, a simple and cheap iron precursor, has not been explored in detail for the synthesis of SPIONs following a thermal decomposition route. Here, we outline a simple one-pot thermal decomposition route that avoids separate precursor preparation and purification steps and, consequently, is easily scalable. The method involves the alcoholic hydrolysis of a simple iron salt into iron hydroxide, which, on addition of oleic acid, forms the precursor oleate complex in situ, which is subsequently thermally decomposed to produce monodispersed SPIONS. Minor modifications allow for particle dimensions (5–20 nm) and morphology (spheroid or cuboid) to be controlled. Additionally, we explored a simple ligand exchange process for rendering the hydrophobic nanoparticles hydrophilic. Trisodium nitrilotriacetate (NTA), a readily available polycarboxylate, can efficiently transfer the oleate-coated SPIONs to water without the need for separation from the crude reaction mixture. X-ray Rietveld refinement showed that particles obtained by this method had both the magnetite and wustite phases of iron oxide present. Magnetic measurements confirm that the iron oxide particles are superparamagnetic at room temperature, with typical blocking temperatures of 183 K for the spherical and 212 K for the cuboid ones.