The combination of a flow reactor with microwave heating enabled a robust process for the fast precipitation of magnetic nanoparticles.
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Controllable and reproducible synthesis of multicore iron oxide nanoparticles was achieved.
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Reactor scale-up by an order of magnitude was demonstrated.
Abstract
Coprecipitation is by far the most common synthesis method for iron oxide nanoparticles (IONPs). However, reproducibility and scalability represent a major challenge. Therefore, innovative processes for scalable production of IONPs are highly sought after. Here, we explored the combination of microwave heating with a flow reactor producing IONPs through coprecipitation. The synthesis was initially studied in a well-characterised microwave-heated flow system, enabling the synthesis of multicore IONPs, with control over both the single core size and the multicore hydrodynamic diameter. The effect of residence time and microwave power was investigated, enabling the synthesis of multicore nanostructures with hydrodynamic diameter between ∼35 and 70 nm, with single core size of 3–5 nm. Compared to particles produced under conventional heating, similar single core sizes were observed, though with smaller hydrodynamic diameters. The process comprised of the initial IONP coprecipitation followed by the addition of the stabiliser (citric acid and dextran). The ability of precisely controlling the stabiliser addition time (distinctive of flow reactors), contributed to the synthesis reproducibility. Finally, scale-up by increasing the reactor length and using a different microwave cavity was demonstrated, producing particles of similar structure as those from the small scale system, with a throughput of 3.3 g/h.
