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In order to perform a complete integration of reflection intensities, PED can be coupled with ADT (Mugnaioli et al. 2009). The resulting data sets proved to be of extremely high quality and in the last 2 years a number of complicate structures have been solved ab initio by direct methods with a fully kinematic assumption (Birkel et al. 2010; Kolb et al. 2010, 2011; Rozhdestvenskaya et al. 2010; Andrusenko et al. 2011; Denysenko et al. 2011). In this chapter we show how ADT/PED data can be used for routine analysis of nano crystalline inorganic materials.
2 Experimental For TEM and ADT investigations samples were dispersed in ethanol using ultrasonic bath and sprayed on a carbon-coated copper grid (Mugnaioli et al. 2009). TEM, STEM and ADT were carried out with a FEI TECNAI F30 S-TWIN transmission electron microscope working at 300 kV. TEM images and electron diffraction patterns were acquired with a CCD camera (14-bit GATAN 794MSC). STEM images were acquired by a FISCHIONE HAADF detector. For structure analysis electron diffraction data were collected using ADT module (Kolb et al.
Under these conditions, nearly all organic and most of inorganic materials suffer a fast deterioration due to beam damage. The necessity to orient the particle in order to record meaningful HRTEM images further increases the exposure time. This may lead to a modification of the crystalline structure or to complete amorphization or sublimation of the sample (Spence 2003; Reimer and Kohl 2008; Kolb et al. 2010). On the contrary, electron diffraction can deliver structural information at a comparable resolution with significantly lower radiation on the sample.