Quantitative Convergent Beam Electron Diffraction (CBED) measurements of low-order structure factors in metals

2022 ◽  
pp. 129-132
Author(s):  
M Saunders ◽  
A G Fox
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.


2003 ◽  
Vol 9 (5) ◽  
pp. 379-389 ◽  
Author(s):  
Jesper Friis ◽  
Bin Jiang ◽  
John C.H. Spence ◽  
Randi Holmestad

Accurate low-order structure factors for copper metal have been measured by quantitative convergent beam electron diffraction (QCBED). The standard deviation of the measured structure factors is equal to or smaller than the most accurate measurement by any other method, including X-ray single crystal Pendellösung, Bragg γ-ray diffraction, and high-energy electron diffraction. The electron structure factor for the (440) reflection was used to determine the Debye-Waller (DW) factor. The local heating of the specimen by the electron beam is determined to be 5 K under the current illumination conditions. The low-order structure factors for copper measured by different methods are compared and discussed. The new data set is used to test band theory and to obtain a charge density map. The charge deformation map shows a charge surplus between the atoms and agrees fairly well with the simple model of copper 2+ ions at the atomic sites in a sea of free uniformly distributed electrons.


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):  
B. Aryal ◽  
D. Morikawa ◽  
K. Tsuda ◽  
M. Terauchi

A local structure analysis method based on convergent-beam electron diffraction (CBED) has been used for refining isotropic atomic displacement parameters and five low-order structure factors with sin θ/λ ≤ 0.28 Å−1 of potassium tantalate (KTaO3). Comparison between structure factors determined from CBED patterns taken at the zone-axis (ZA) and Bragg-excited conditions is made in order to discuss their precision and sensitivities. Bragg-excited CBED patterns showed higher precision in the refinement of structure factors than ZA patterns. Consistency between higher precision and sensitivity of the Bragg-excited CBED patterns has been found only for structure factors of the outer zeroth-order Laue-zone reflections with larger reciprocal-lattice vectors. Correlation coefficients among the refined structure factors in the refinement of Bragg-excited patterns are smaller than those of the ZA ones. Such smaller correlation coefficients lead to higher precision in the refinement of structure factors.


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.


2014 ◽  
Vol 70 (a1) ◽  
pp. C1623-C1623
Author(s):  
Yueming Guo ◽  
Philip Nakashima ◽  
Joanne Etheridge

It has been shown mathematically that both the magnitudes and 3-phase invariants of the structure factors of a centrosymmetric crystal can be expressed explicitly in terms of the distances to specific features in the 3-beam convergent beam electron diffraction (CBED) pattern [1].This theoretical inversion can be implemented experimentally, enabling direct observations of 3-phase invariants and the approximate measurement of structure factor magnitudes. This method then enables a different approach to crystal structure determination, which is based on the observation of phases, rather than the measurement of amplitudes. It has been shown that by inspection of just a few phases using 3-beam CBED patterns, centrosymmetric crystal structures can be determined directly to picometre precision without the need to measure magnitudes [2]. Here, we will explore a different approach for measuring structure factor magnitudes from 3-beam CBED patterns. It has been demonstrated that the relative structure factor magnitudes can be determined directly from the ratio of the intensity distributions along specific lines within the CBED discs [3]. We will investigate the potential of using this approach for the relatively fast measurement of approximate structure factor magnitudes from nano-scale volumes of crystals.


Author(s):  
John Mansfield ◽  
Martin Saunders ◽  
George Burgess ◽  
David Bird ◽  
Nestor Zaluzec

There has been considerable recent interest in the determination of structure factors from convergent-beam electron diffraction (CBED) patterns and the ultimate goal is the ability to retrieve the crystal structure of an unknown crystal by inversion of a CBED pattern. There are a number of different methods that have been used to extract structure factor information. The zone-axis pattern fitting technique of Bird and Saunders has recently been used to obtain structure factors for silicon that compare well with those obtained by X-ray methods. This work extends the techniques to f.c.c. metals, specifically copper.CBED patterns were recorded from [110] zone axes of electropolished foils of pure copper (99.999% purity) in the Philips EM420T at Argonne National Laboratory. The patterns were energy-filtered by scanning the whole pattern across the entrance aperture of a Gatan #607 serial energy loss spectrometer and collecting the zero loss intensity only (energy window ∼5eV).


Author(s):  
R. Vincent ◽  
D. J. Exelby

In recent years, significant progress has been made towards a solution for the general problem of crystal structure determination by convergent beam electron diffraction (CBED). Even if we consider only perfectly ordered, periodic crystals defined by one of the conventional space groups, diffraction methods based on a focussed sub-micron beam of electrons are applicable to several related sets of structural problems that are not accessible to conventional X-ray or neutron diffraction techniques. We assume here that the space group either is known or has been determined from CBED patterns and that phases and amplitudes for some subset of the structure factors are required. Two limiting cases have been explored in some detail. For crystals where the atomic parameters and Debye-Waller factors are known accurately from high quality X-ray data, information on the charge redistribution for bonding electrons is available from precise measurements of the low order structure factors. Following the original research of Kambe, some recent work has demonstrated that accurate structure amplitudes and three-beam phase invariants can be extracted from the dynamical intensity distribution in CBED reflections. In principle, this approach is completely general but considerable labour would be required to extract sufficient data to solve the structure of an unknown crystal, whereas a large set of kinematic intensities is acquired from a single X-ray pattern.


2000 ◽  
Vol 33 (4) ◽  
pp. 1119-1121 ◽  
Author(s):  
M.-Y. Wu ◽  
Jing Zhu ◽  
S.-Y. Li ◽  
Z.-H. Du ◽  
S.-L. Li

Using convergent-beam electron diffraction (CBED), the fine structure factors of Co3Ti alloys have been measured and the effects of boron microalloying on the fine structure factors have been studied. The extinction distances of Co3Ti have been obtained by both Kelly's method (making use of the positions of the maximum and minimum intensities in the CBED pattern) and the CBED simulation method.


Sign in / Sign up

Export Citation Format

Share Document