Electron diffraction selected area

Figure C2.17.7. Selected area electron diffraction pattern from TiC nanocrystals. Electron diffraction from fields of nanocrystals is used to detennine tire crystal stmcture of an ensemble of nanocrystals [119]. In tliis case, tliis infonnation was used to evaluate the phase of titanium carbide nanocrystals [217].

Asbestos fiber identification can also be achieved through transmission or scanning electron microscopy (tern, sem) techniques which are especially usefiil with very short fibers, or with extremely small samples (see Microscopy). With appropriate peripheral instmmentation, these techniques can yield the elemental composition of the fibers using energy dispersive x-ray fluorescence, or the crystal stmcture from electron diffraction, selected area electron diffraction (saed). 

The spacings between the layers (rfooz) measured by selected area electron diffraction were in a range of 0.34 to 0.35 nm[3]. X-ray diffraction (XRD) of the cathode deposit, including nanoparticles and nano-... 

The powder patterns obtained by X-ray diffraction and selected area electron diffraction do represent averages over very large numbers of particles but the averaging over size, orientation and imperfection of crystals removes much of the important information, especially that on the correlations of properties,e.g, the orientational relationship of adjacent crystal regions or the dependence of twinning on size. 

Figure 5a. Mineral aurichalcite calcined at 350°C for 4 hours. Selected area electron diffraction pattern showing ZnO orientations with zone axes of [lOTo] and [3031]. See text for other ZnO orientations. An aurichalcite pattern close to a [101] zone axis is also present.

The most important information about the nanoparticles is the size, shape, and their distributions which crucially influence physical and chemical properties of nanoparticles. TEM is a powerful tool for the characterization of nanoparticles. TEM specimen is easily prepared by placing a drop of the solution of nanoparticles onto a carbon-coated copper microgrid, followed by natural evaporation of the solvent. Even with low magnification TEM one can distinguish the difference in contrast derived from the atomic weight and the lattice direction. Furthermore, selective area electron diffraction can provide information on the crystal structure of nanoparticles. 

Linear absorption measurements can therefore give the first indication of possible alloy formation. Nevertheless, in systems containing transition metals (Pd-Ag, Co-Ni,. ..) such a simple technique is no longer effective as interband transitions completely mask the SPR peak, resulting in a structurless absorption, which hinders any unambiguous identification of the alloy. In such cases, one has to rely on structural techniques like TEM (selected-area electron diffraction, SAED and energy-dispersive X-ray spectroscopy, EDS) or EXAFS (extended X-ray absorption fine structure) to establish alloy formation. 

Figure 57.12. The HRTEM selected area electron diffraction (SAED) of the CA53 leached for 45 min at rt showing the presence of the Ni/Al bee phase (A) and the coexistence of both the Ni-Al bee phase with the original Ni2Al3 alloy (B).

Figure 2. On the left hand side is the HRTEM image of Ti-Beta nanoparticles obtained from the colloidal solution that was thermally treated for 28 hours. In the inset a selected area electron diffraction ofTi-Beta nanpoarticles shows their crystalline structure. On the right hand side are the 29Si MAS and H - 29Si CPMAS spectra of the sample g).

Bismuth Molybdates. Bismuth molybdates are used as selective oxidation catalysts. Several phases containing Bi and/or Mo may be mixed together to obtain desired catalytic properties. While selected area electron diffraction patterns can identify individual crystalline particles, diffraction techniques usually require considerable time for developing film and analyzing patterns. X-ray emission spectroscopy in the AEM can identify individual phases containing two detectable elements within a few minutes while the operator is at the microscope. 

The transmission electron microscopy (TEM) and correlated electron diffraction patterns of quenched QAB2-4 alloy is shown in Figure 2. When annealed at 773K, by selected-area electron diffraction (SAED) patterns at transmission electron microscopy appears as a bright continuous ring, indicating an amorphous phase. 

In the case of a synthetic Mg2 A1 - CO3 LDH, selected area electron diffraction (SARD) [264] patterns of a few crystals with zone axis (00() showed evidence of a superlattice with a = floV3 = 0.532 nm [71], although this was... 

Stmcture determination of unknown crystals by electron diffraction was performed by several research groups, on Al-Fe alloys by Gjonnes et al. (1998), on metal-cluster compounds by Weirich et al. (2000) and on zeolites by Wagner et al. (1999). Selected area electron diffraction or electron diffraction collected by a precession technique were used and the structure factor phases were deduced by direct methods, Patterson method or from convergent beam electron diffraction. 

Structure refinement based on kinematical scattering was already applied by the Russian scientist 60 years ago. Weirich et al. (1996) first solved the structure of an unknown TinSe4by HREM combined with crystallographic image processing. Then they used intensities extracted from selected area electron diffraction patterns of a very thin crystal and refined the structure to a precision of 0.02 A for all the atoms. Wagner and Terasaki et al. (1999) determined the 3D structure of a new zeolite from selected area electron diffraction, based on kinematical approach. 

For a long time, Selected-Area Electron Diffraction (SAED) performed with a parallel incident beam and a selected-area aperture was the only experimental method available. During the three last decades, new diffraction techniques based on a convergent electron incident beam (CBED Convergent-Beam Electron Diffraction, LACBED Large-Angle... 

Electron diffraction performed with a parallel incident beam, i.e. Selected-Area Electron Diffraction is used to obtain good electron micrographs. The two-beam condition allows the observation of defects. SAED is also used in High-Resolution Electron Microscopy (HREM) to set a crystal to a zone axis so that the atomic columns are vertical in the microscope. SAED is very useful for the identification of phases and the... 

Various electron diffraction techniques are available on modem transmission electron microscopes. Selected-Area Electron Diffraction (SAED) and Microdiffraction are performed with a parallel or nearly parallel incident beam and give spot patterns. Convergent-Beam Electron Diffraction (CBED) and Large-Angle Convergent-Beam Electron Diffraction (LACBED) are performed with a focused and defocused convergent beam... 

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