ORIGINAL PAPER Combining imaging ellipsometry and grazing incidence small angle X-ray scattering for in situ characterization of polymer nanostructures Volker Körstgens & Johannes Wiedersich & Robert Meier & Jan Perlich & Stephan V. Roth & Rainer Gehrke & Peter Müller-Buschbaum Received: 28 May 2009 / Revised: 22 July 2009 / Accepted: 23 July 2009 / Published online: 14 August 2009 # Springer-Verlag 2009 Abstract A combination of microbeam grazing incidence small angle X-ray scattering (μGISAXS) and imaging ellipsometry is introduced as a new versatile tool for the characterization of nanostructures. μGISAXS provides a local lateral and depth-sensitive structural characterization, and imaging ellipsometry adds the position-sensitive determination of the three-dimensional morphology in terms of thickness, roughness, refractive index, and extinction coefficient. Together μGISAXS and imaging ellipsometry enable a complete characterization of structure and morphology. On the basis of an example of buildup of nanostructures from monodisperse colloidal polystyrene nanospheres on a rough solid support, the scope of this new combination is demonstrated. Roughness is introduced by a dewetting structure of a diblock copolymer film with one block being compatible with the colloidal nanoparticles and one block being incompatible. To demonstrate the potential for kinetic investigations, μGISAXS and imaging ellipsometry are applied to probe the drying process of an aqueous dispersion of nanospheres on such a type of rough substrate. Keywords Interface/surface analysis . Diffraction methods (low-energy electron diffraction|X-ray) . Nanoparticles/ nanotechnology . Microbeam grazing incidence small angle X-ray scattering . Imaging ellipsometry . Self-assembly A new combined technique For many nanostructured systems in materials of natural origin as well as in artificial materials developed with bottom-up techniques, nanostructures are not homogeneously distributed. Often structures on the nanoscale are a substruc- ture of structures in the mesoscopic or macroscopic regime. In such cases, the nanostucture is only one of all the structural length scales that are responsible for the overall material properties of these hierarchically ordered systems [1–3]. Thus, an ideal characterization technique for nano- structures should not just offer the opportunity to investigate larger sample areas to depict heterogeneities, but the widest possible range of length scales should be addressable. So far, to a large extent the characterization of nano- structures has been successfully carried out with real space characterization techniques such as atomic force microsco- py (AFM) and scanning electron microscopy [4–6]. Being extensively used, however, these techniques might only offer information on a limited observation area if not different areas are probed. As a consequence, in the case of macroscopic samples the structural information obtained risks having an insufficient statistical representative mean- ing. Such problems are overcome with the application of surface-sensitive scattering techniques, which allow large sample areas to be probed and yield structural information about nanoscopic objects with high statistical relevance. However, due to the beam size used in such scattering V. Körstgens : J. Wiedersich : R. Meier : J. Perlich : P. Müller-Buschbaum (*) Physik-Department E13, Technische Universität München, James-Franck-Str. 1, 85747 Garching, Germany e-mail: muellerb@ph.tum.de S. V. Roth : R. Gehrke HASYLAB at DESY, Notkestr. 85, 22603 Hamburg, Germany Anal Bioanal Chem (2010) 396:139–149 DOI 10.1007/s00216-009-3008-1