One challenge in the production of nanometer-sized objects with given properties is to control their growth at a macroscopic scale in situ and in real time. A dedicated ultrahigh-vacuum grazing-incidence small-angle x-ray scattering setup has been developed, yielding high sensitivity and dynamics. Its capabilities to derive the average particle shape and size and the film growth mode and ordering and to probe both surfaces and buried interfaces are illustrated for two prototypical cases: the model catalyst Pd/MgO(100) and the self-organized Co/Au(111) system. A wide range of technologically important systems can potentially be investigated in various gaseous environments.

Using grazing-incidence x-ray diffraction, the $p(2\times 2)$ surface structures of the single crystal NiO(111) and a 5 monolayer thick NiO(111) film on Au(111) were both shown to exhibit locally the theoretically predicted octopolar reconstruction, with some important differences. The single crystal exhibits a single Ni termination with double steps. The thin film exhibits both possible terminations (O and Ni) and single steps. These surfaces were found to be nonreactive with respect to hydroxylation.

The growth of hexagonal aluminum nitride directly on (111) silicon has been studied by grazing incidence x-ray diffraction and high resolution electron microscopy as a function of film thickness. Two epitaxial relationships were observed: (1) AlN (0001) $\text{[2}\overline{11}\text{0]//}\mathrm{Si}\text{(111)}$ [022̄], which prevails at deposition temperatures larger than 650 °C, and (2) AlN (0001) [101̄0]//Si(111) [022̄]. For a 40 Å thick layer, the average in-plane crystallite size is 162 Å, the in-plane rotation is $\text{∼2°}$ and the dislocations induce an average strain distribution of 0.8%. The Si/AlN interface is very sharp and complete relaxation (down to $\text{∼0.2\%}$ ) occurs within one bilayer. No long range order was observed at the interface. This implies a low mobility of the AlN species on Si, inhibiting any structural rearrangement. In particular the in-plane rotations originate from the early stage of the layer growth and decrease with the layer thickness, especially for thicknesses larger than 250 Å.