Influence of hydrothermal synthesis conditions on size, morphology and colloidal properties of Hematite nanoparticles

The synthesis, morphological characterization, and colloidal properties of Hematite nanoparticles (hemNP) with different sizes and shapes were presented. To prepare hemNP we used hydrothermal synthesis with different combinations of reaction conditions. Various characterization techniques involving XRD, TEM, AFM and DLS were employed to describe the dependence of the hemNP size, charge and morphology on different synthesis conditions. Spheroidal Hematite nanoparticles from 20 to 60 nm were obtained by varying the rate of addition of iron precursor solutions and the aging time (Δt) at ca. 100°C. The transformation from Ferrihydrite to Hematite (α-Fe2O3) started with a burst nucleation of nanosized crystallites, followed by a first-order kinetic growth of primary grains up to a final threshold size of ca 30 nm. Colloidal behavior was also checked at pH 4 and 7, finding interparticle aggregation at circumneutral pH only for hemNP obtained for Δt<2 h. Electrophoretic ζ potential measurements yield positive values at pH 4 and negative at pH 7. The shifts in (IEP) at lower values depended on the adsorption of appreciable counterions on the particle surface and reduced at pH 7 the charge-charge repulsion, whereas the attractive forces became predominant. The results confirmed that the particle size of the Hematite nanoparticle critically affected their colloidal behavior with significant consequences for sorption and aggregation processes. Particularly for low particle sizes of the order of 10-20 nm, the surface charge and surface reactivity also could differ in important ways compared to 40-60 nm size particles.