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Synchrotron radiation experiments were carried out during the in situ growth of ZnO nanoparticles by the aqueous chemical growth technique. The first results of this exploratory in situ grazing-incidence diffraction (GID) experiment are reported, with emphasis on the difficulties encountered. In particular, it is shown that, when in situ GID experiments are carried out in a 25 mm-long cell, scattering by the solvent dominates. This impedes the observation of the formation of ZnO nanoparticles during the early stages of the growth process. Nevertheless, it is clearly shown that the wurzite hexagonal structure is present in the solution. At a specific concentration, it is shown how the peak intensities and widths of the Bragg peaks evolve as a function of time.

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