The purpose of this study was to investigate the synthesis of iron oxide nanoparticles under two different conditions, namely high and low gas flow rates, using laser pyrolysis and to examine the influence of laser power. The attained nanoparticles have been characterised regarding their stability and hydrodynamic dimensions by dispersive light scattering analysis (DLS), structure–X-ray diffraction (XRD), elemental composition–energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS), and morpho-structural characterisation achieved by transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). For a better understanding of the laser power influence, the residence time was also calculated.
The laser pyrolysis technique was used in the synthesis of magnetic iron oxide nanopowders in the presence of ethanol vapors as a sensitizer. This technique uses the energy from a continuous-wave CO2 laser operating at a 9.25 μm wavelength, which is transferred to the reactive precursors via the excited ethanol molecules, inducing a rapid heating of the argon-entrained Fe(CO)5 vapors in the presence of oxygen. For a parametric study, different samples were prepared by changing the percentages of sensitizer in the reactive mixture. Moreover, the raw samples were thermally treated at different temperatures and their morpho-structural and magnetic properties were investigated. The results indicated a high degree of crystallinity (mean ordered dimension) and enhanced magnetic properties when high percentages of ethanol vapors were employed. On the contrary, at low ethanol concentrations, due to a decrease in the reaction temperature, nanoparticles with a very low size were synthesized. The raw particles have a dimension in the range of 2.5 to 10 nm (XRD and TEM). Most of them exhibited superparamagnetic behavior at room temperature, with saturation magnetization values up to 60 emu/g. The crystalline phase detected in samples is mainly maghemite, with a decreased carbon presence (up to 8 at%). In addition to the expected Fe-OH on the particles surfaces, C (and O) bearing functional groups such as C-OH or C=O that act as a supplementary hydrophilic agent in water-based suspension were detected. Using the as-synthesized and thermally treated nanopowders, water suspensions without or with hydrophilic agents (CMCNa, L-Dopa, chitosan) were prepared by means of a horn ultrasonic homogenizer at 0.5 mg/mL concentrations. DLS analyzes revealed that some powder suspensions maintained stable agglomerates over time, with a mean size of 100 nm, pH values between 4.8 and 5.3, and zeta-potential values exceeding 40 mV. All tested agents greatly improved the stability of 250–450 °C thermally treated NPs, with L-Dopa and Chitosan inducing smaller hydrodynamic sizes.
The present study investigates the synthesis and dispersibility process of iron oxide nanoparticles using laser pyrolysis with isopropanol vapors as a sensitizer agent. Similar to previous experiments (iron oxide nanoparticles synthesized by laser pyrolysis using ethylene as sensitizer gas), iron pentacarbonyl (Fe(CO)5) was employed as an iron precursor; however, instead of the classic ethylene, isopropanol was chosen as a sensitizer, which indicated beneficial features (especially enhanced dispersibility in water) in the as-synthesized nanoparticles. Structural and elemental analysis confirmed the size range of the nanoparticles (nanometric), with crystallite sizes under 10 nm. Both raw nanoparticles, as well as the oleic acid stabilized ones, exhibited excellent colloidal stability in both water and organic fluids (Toluene, Chloroform, and DMSO): around 100 nm hydrodynamic diameter and more than 40 mV for zeta potential. The study highlights the advantages of using isopropanol as a sensitizer in the production of high-purity iron oxide nanoparticles from laser pyrolysis, particles that showcase superior dispersibility and functionalization potential.