Towards automatic alignment of a crystalline sample in an electron microscope along a zone axis.

A method is presented to use an electron microscope in transmission mode to determine the mis-tilt from a zone axis of a crystalline material. The method involves recording a number of additional diffraction patterns with incident beams tilted over 2 to 3 degrees. It is shown that an accuracy of 0.02 degree can be achieved, which is far better than that of the specimen-stage tilt axes, which is about 0.1 degree for the ß-tilt.

Towards automated diffraction tomography. Part II--Cell parameter determination.

Automated diffraction tomography (ADT) allows the collection of three-dimensional (3d) diffraction data sets from crystals down to a size of only few nanometres. Imaging is done in STEM mode, and diffraction data are collected with quasi-parallel beam nanoelectron diffraction (NED). Here, we present a set of developed processing steps necessary for automatic unit-cell parameter determination from the collected 3d diffraction data. Cell parameter determination is done via extraction of peak positions from a recorded data set (called the data reduction path) followed by subsequent cluster analysis of difference vectors. The procedure of lattice parameter determination is presented in detail for a beam-sensitive organic material. Independently, we demonstrate a potential (called the full integration path) based on 3d reconstruction of the reciprocal space visualising special structural features of materials such as partial disorder. Furthermore, we describe new features implemented into the acquisition part.

Towards automated diffraction tomography: part I--data acquisition.

The ultimate aim of electron diffraction data collection for structure analysis is to sample the reciprocal space as accurately as possible to obtain a high-quality data set for crystal structure determination. Besides a more precise lattice parameter determination, fine sampling is expected to deliver superior data on reflection intensities, which is crucial for subsequent structure analysis. Traditionally, three-dimensional (3D) diffraction data are collected by manually tilting a crystal around a selected crystallographic axis and recording a set of diffraction patterns (a tilt series) at various crystallographic zones. In a second step, diffraction data from these zones are combined into a 3D data set and analyzed to yield the desired structure information. Data collection can also be performed automatically, with the recent advances in tomography acquisition providing a suitable basis. An experimental software module has been developed for the Tecnai microscope for such an automated diffraction pattern collection while tilting around the goniometer axis. The module combines STEM imaging with diffraction pattern acquisition in nanodiffraction mode. It allows automated recording of diffraction tilt series from nanoparticles with a size down to 5nm.

The effect of inelastic scattering on crystal structure refinement from electron diffraction patterns recorded under almost parallel illumination.

Recently a number of crystal structures were determined using electron diffraction data with an almost parallel electron beam. In many cases no energy filtering was applied. On the other hand, the contrast in convergent beam electron diffraction patterns is greatly improved by energy filtering of the electrons. To investigate whether energy filtering will improve the accuracy of the structure analysis from diffraction data recorded under an almost parallel beam condition, we recorded diffraction patterns of the [100] zone of YBa(2)Cu(3)O(7) using unfiltered electrons, zero-loss electrons and plasmon-loss electrons, respectively. Subsequently, the structure is refined based on these different electron diffraction datasets, using the program MSLS (Acta Crystallogr. A 54 (1998) 91). The results show that the obtained atomic positions are not significantly different for the chosen filter conditions. Even with amorphous carbon deposited on the specimen, which will cause a significant increase (>40 times) of energy-loss electrons, the structure refinement led to the same atomic positions.

High-angle annular dark-field imaging on a TEM/STEM system.

The technique of high-angle annular dark-field (HAADF) imaging, which is highly sensitive to atomic-number contrast, can be performed on TEM/STEM systems using the standard annular dark-field detector. For optimum HAADF imaging, the TEM/STEM must have a high maximum diffraction angle, small minimum camera length, and a descanning facility. The sensitivity of the technique is demonstrated to be about 10(5) to 10(6) times higher than energy-dispersive X-ray spectroscopy. Examples are shown from semiconductor, catalysis, ceramics, and particle analysis applications.