Iron oxide nanoparticles were synthesized in a liquid flame spray process from iron(III) nitrate. The choice of chemicals and all other process parameters affects the crystallographic phase composition and the quality of the material. Adjustment of the solvent composition and the gas flow rates was used to control the phase composition of the produced particles. All samples consisted of pure maghemite (γ-Fe 2 O 3 ) or a mixture of maghemite and hematite (α-Fe 2 O 3 ). When using pure alcohols as solvents, the maghemite/hematite phase ratio could be adjusted by changing the equivalence ratio that describes the oxidation conditions in the flame zone. A large residual particle mode formed in the size range of ~20-700 nm along with a dominant very fine particle mode (2-8 nm). Both phases seemed to contain large particles. A partial substitution of methanol with carboxylic acids turned the hematite phase into maghemite completely, even though some of particles were possibly not fully crystallized.Residual particles were still present, but their size and number could be decreased by raising the heat of combustion of the precursor solution. 30 vol-% substitution of methanol with 2-ethylhexanoic acid was adequate to mostly erase the large particles.
K E Y W O R D Siron/iron compounds, liquid flame spray, nanoparticles, synthesis
This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO2 nanoparticles with diameters in the range 4–35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO2: anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO2 nanoparticles.
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