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The critical process conditions for controlled growth of iron oxide nanoparticles synthesized using continuous hydrothermal synthesis
Kriedemann, Brett Craig
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Iron oxide nanoparticles have recently become attractive for use in gas sensing, as catalysts and have also shown promise in other fields, such as biomedicine, for targeted drug delivery and cancer treatment. Despite these growing applications, the ability to produce iron oxide and one dimensional (1D) iron oxide nanoparticles on an industrial scale has proven to be a challenge. The continuous hydrothermal synthesis, (CHS), method has been proposed as the most promising method, yet the effect of the operating parameters on particle characteristics are still widely contested in the literature. One such parameter, temperature, is still widely contested on its effect on APS. To address this issue, a CHS pilot plant was constructed and commissioned. The inability to isolate certain parameters in CHS is a common shortcoming. Parameters such as temperature and flow rate are prime examples, as changing the temperature has several effects on the system resulting in a change in reaction rate, a change in density and a change in the reactor residence time while the flow rate is closely linked to the residence time and mixing conditions. A 3-level Box-Behnken factorial design method was used to statistically analyze the correlations and interactions between operating parameters (temperature, concentration and flow rate) in CHS and evaluate their resulting effect on particle characteristics, with focus on morphology. All particles were characterized by X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). Reactions in the presence of solvents or surfactants proved incapable of modifying particle morphology, although significant particle size reduction revealed that they were actively involved in particle growth and may be used as a further tool for controlling particle characteristics. The concentration was found to have the greatest effect on particle characteristics including a slight alteration of particle shape and a massive influence on the average particle size. The interactions between operating parameters were significant, especially in the case of temperature and concentration. The temperature and concentration were found to interact revealing three different trends on APS, offering a solution to conflicting reports in the literature. The temperature was also observed to interact favourably with the flow rate, presenting a method of increasing the PY and RC, with little change in APS and PSD. This knowledge will prove invaluable for the design of future experiments in CHS.