Quantitative Zone-Axis Convergent Beam Electron Diffraction: Current Status and Future Prospects

2003 ◽  
Vol 9 (5) ◽  
pp. 411-418 ◽  
Author(s):  
Martin Saunders

Quantitative zone-axis convergent beam electron diffraction (CBED) is now an established technique. Over the past decade it has been developed into a tested method for the accurate refinement of structure factors, allowing the details of the charge density and bonding effects to be studied in crystalline materials. Strategies for obtaining the most accurate results have evolved, and the most important influences on the accuracy have been determined. Initial applications of the technique to bond charge density determination have led to the extension of the method to the refinement of other important parameters influencing the experimental data, such as Debye–Waller factors and the absorption potential. The development and current status of quantitative zone-axis CBED are discussed. Prospects for the future development and application of the technique are also considered.

2011 ◽  
Vol 1295 ◽  
Author(s):  
X. H. Sang ◽  
A. Kulovits ◽  
J. Wiezorek

ABSTRACTAccurate Debye-Waller (DW) factors of chemically ordered β-NiAl (B2, cP2, ${\rm{Pm}}\bar 3 {\rm{m}}$) have been measured at different temperatures using an off-zone axis multi-beam convergent beam electron diffraction (CBED) method. We determined a cross over temperature below which the DW factor of Ni becomes smaller than that of Al of ~90K. Additionally, we measured for the first time DW factors and structure factors of chemically ordered γ1-FePd (L10, tP2, P4/mmm) at 120K. We were able to simultaneously determine all four anisotropic DW factors and several low order structure factors using different special off-zone axis multi-beam convergent beam electron diffraction patterns with high precision and accuracy. An electron charge density deformation map was constructed from measured X-ray diffraction structure factors for γ1-FePd.


Author(s):  
S. Swaminathan ◽  
I. P. Jones ◽  
N. J. Zaluzec ◽  
D. M. Maher ◽  
H. L. Fraser

It has been claimed that the effective Peierls stresses and mobilities of certain dislocations in TiAl are influenced by the anisotropy of bonding charge densities. This claim is based on the angular variation of electron charge density calculated by theory. It is important to verify the results of these calculations experimentally, and the present paper describes a series of such experiments. A description of the bonding charge density distribution in materials can be obtained by utilizing the charge deformation density (Δρ (r)) defined by(1) where V is the volume of the unit cell, Fobs is the experimentally determined low order structure factor and Fcalc is the structure factor calculated using the Hartree-Fock neutral atom model. To determine the experimental low order structure factors, a technique involving a combination of convergent beam electron diffraction (CBED) and electron energy loss spectroscopy (EELS) has been used.


2017 ◽  
Vol 50 (2) ◽  
pp. 602-611 ◽  
Author(s):  
Ding Peng ◽  
Philip N. H. Nakashima

The effectiveness of tripod polishing and crushing as methods of mechanically preparing transmission electron microscopy specimens of hard brittle inorganic crystalline materials is investigated via the example of cerium hexaboride (CeB6). It is shown that tripod polishing produces very large electron-transparent regions of very high crystal perfection compared to the more rapid technique of crushing, which produces crystallites with a high density of imperfections and significant mosaicity in the case studied here where the main crystallite facets are not along the natural {001} cleavage planes of CeB6. The role of specimen quality in limiting the accuracy of structure factor measurements by quantitative convergent-beam electron diffraction (QCBED) is investigated. It is found that the bonding component of structure factors refined from CBED patterns obtained from crushed and tripod-polished specimens varies very significantly. It is shown that tripod-polished specimens yield CBED patterns of much greater integrity than crushed specimens and that the mismatch error that remains in QCBED pattern matching of data from tripod-polished specimens is essentially nonsystematic in nature. This stands in contrast to QCBED using crushed specimens and lends much greater confidence to the accuracy and precision of bonding measurements by QCBED from tripod-polished specimens.


Author(s):  
E. Silva ◽  
R. Scozia

The purpose in obtaining zone axis pattern map (zap map) from a given material is to provide a quick and reliable tool to identify cristaline phases, and crystallographic directions, even in small particles. Bend contours patterns and Kossel lines patterns maps from Zr single crystal in the [0001] direction have been presented previously. In the present communication convergent beam electron diffraction (CBED) zap map of Zr will be shown. CBED patterns were obtained using a Philips microscope model EM300, which was set up to carry out this technique. Convergent objective upper pole piece for STEM and some electronic modifications in the lens circuits were required, furthermore the microscope was carefully cleaned and it was operated at a vacuum eminently good.CBED patterns in the Zr zap map consist of zero layer disks, showing fine details within them which correspond to intersecting set of higher order Laue zone (HOLZ) deficiency lines.


1999 ◽  
Vol 55 (2) ◽  
pp. 188-196 ◽  
Author(s):  
R. Høier ◽  
C. R. Birkeland ◽  
R. Holmestad ◽  
K Marthinsen

Quantitative convergent-beam electron diffraction is used to determine structure factors and three-phase structure invariants. The refinements are based on centre-disc intensities only. An algorithm for parameter-sensitive pixel sampling of experimental intensities is implemented in the refinement procedure to increase sensitivity and computer speed. Typical three-beam effects are illustrated for the centrosymmetric case. The modified refinement method is applied to determine amplitudes and three-phase structure invariants in noncentrosymmetric InP. The accuracy of the results is shown to depend on the choice of the initial parameters in the refinement. Even unrealistic starting assumptions and incorrect temperature factor lead to stable results for the structure invariant. The examples show that the accuracy varies from 1 to 10° in the electron three-phase invariants determined and from 0.5 to 5% for the amplitudes. Individual phases could not be determined in the present case owing to spatial intensity correlations between phase-sensitive pixels. However, for the three-phase structure invariant, stable solutions were found.


2007 ◽  
Vol 40 (2) ◽  
pp. 241-249 ◽  
Author(s):  
Haruyuki Inui ◽  
Akihiro Fujii ◽  
Hiroki Sakamoto ◽  
Satoshi Fujio ◽  
Katsushi Tanaka

The recently proposed CBED (convergent-beam electron diffraction) method for enantiomorph identification has been successfully applied to crystals belonging to the point groups 321 and 312. The intensity asymmetry of zeroth-order Laue zone and/or first-order Laue zone reflections of Bijvoet pairs is easily recognized in CBED patterns with the incidence along appropriate zone-axis orientations for each member of the enantiomorphic pair. The intensity asymmetry with respect to the symmetry line is reversed upon changing the space group (handedness) from one to the other. Thus, enantiomorph identification can be easily performed in principle for all crystals belonging to the point groups 321 and 312.


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