Extended electron energy-loss fine structure and selected-area electron diffraction studies of small palladium clusters

Extended electron energy-loss fine structure (EXELFS) and selected-area electron diffraction (SAED) techniques have both been applied to the study of the crystalline structure of Pd clusters of average diameters ranging from bulk to 24 Å. The combined use of these techniques gives complementary information about the crystalline structure of Pd clusters. Both techniques show the same lattice parameter expansion, about 4% for the smallest Pd cluster, with respect to the bulk. The EXELFS analysis performed on the Pd-M_4,5 edge shows a sizeable increase of structural disorder in the smallest cluster. SAED gives additional information about the Pd bulk sample, showing the occurrence of crystalline regions about 50 Å in diameter.     

Ab initio determination of the framework structure of the heavy-metal oxide Cs(x)Nb2.54W2.46O14 from 100 kV precession electron diffraction data

The present work deals with the ab initio determination of the heavy metal framework in Cs(x)(Nb, W)(5)O(14) from precession electron diffraction intensities. The target structure was first discovered by Lundberg and Sundberg [Ultramicroscopy 52 (1993) 429-435], who succeeded in deriving a tentative structural model from high-resolution electron microsopy (HREM) images. The metal framework of the compound was solved in this investigation via direct methods from hk0 precession electron diffraction intensities recorded with a Philips EM400 at 100 kV. A subsequent (kinematical) least-squares refinement with electron intensities yielded slightly improved co-ordinates for the 11 heavy atoms in the structure. Chemical analysis of several crystallites by EDX is in agreement with the formula Cs(0.44)Nb(2.54)W(2.46)O(14). Moreover, the structure was independently determined by Rietveld refinement from X-ray powder data obtained from a multi-phasic sample. The compound crystallises in the orthorhombic space group Pbam with refined lattice parameters a=27.145(2), b=21.603(2), and c=3.9463(3)A. Comparison of the framework structure from electron diffraction with the result from Rietveld refinement shows an average agreement for the heavy atoms within 0.09 A.     

Nanosecond time-resolved investigations using the in situ of dynamic transmission electron microscope (DTEM)

Most biological processes, chemical reactions and materials dynamics occur at rates much faster than can be captured with standard video rate acquisition methods in transmission electron microscopes (TEM). Thus, there is a need to increase the temporal resolution in order to capture and understand salient features of these rapid materials processes. This paper details the development of a high-time resolution dynamic transmission electron microscope (DTEM) that captures dynamics in materials with nanosecond time resolution. The current DTEM performance, having a spatial resolution <10nm for single-shot imaging using 15ns electron pulses, will be discussed in the context of experimental investigations in solid state reactions of NiAl reactive multilayer films, the study of martensitic transformations in nanocrystalline Ti and the catalytic growth of Si nanowires. In addition, this paper will address the technical issues involved with high current, electron pulse operation and the near-term improvements to the electron optics, which will greatly improve the signal and spatial resolutions, and to the laser system, which will allow tailored specimen and photocathode drive conditions.     

Structural and electron diffraction data for sapphire (α-al2o3)

Crystallographic and electron diffraction data for sapphire (α-Al₂O₃) are presented which enable ready and unique identification of TEM diffraction patterns and facilitate image analysis. Crystallographic data is presented in the form of stereographic projections and in figures listing angles between planes and angles between zones. Electron diffraction data consist of computer-simulated diffraction patterns and tables of extinction distances calculated using atomic and ionic electron scattering factors.