Evaporation of colloidal nanoparticle solutions is known to produce ordered monolayers of nanoparticles, self-assembled arrays of magnetic nanoparticles being of special importance for applications. The in situ time-resolved grazing-incidence small-angle x-ray scattering with the temporal resolution down to $100\mathrm{ms}$ was employed to study the self-assembling process of iron oxide nanoparticles after a colloidal drop was applied on a silicon substrate. The x-ray scattering contributions from the evaporating drop volume, drop surface, and substrate surface were monitored and separated. The x-ray scattering from the drop for the distances from the substrate surface larger than $\approx 80\mu \mathrm{m}$ shows the absence of self-assembled clusters in the drop volume or self-assembled domains on the drop surface. These results indicate that the nanoparticle self-assembling occurs in the vicinity of the three-phase drop contact line. The ordered nanoparticle monolayer exhibits hexagonal close-packed arrangement.

• Received 26 March 2007

DOI:https://doi.org/10.1103/PhysRevB.76.195432