Determination of crystal polarity in the Electron Microscope

Author(s):  
W. Mader ◽  
A. Recnik

A few methods were proposed for the determination of crystal polarity using electron diffraction. The method by Taftø and Spence is based on the coupling between ZOLZ and FOLZ reflections, requiring exact tilting to excite weak high- and odd-indexed reflections. The method by Spellward and James relies on the comparison of experimentally observed and calculated CBED patterns of fairly thick crystals, where the features in the CBED discs are compared. In this paper we present a method for polarity determination readily evident from ZOLZ reflections in zone-axis microdiffraction patterns. The method is based on zero-layer interactions from thin crystals with thickness t smaller than the extinction length of the primary beam. Then the diffraction discs appear homogeneous, and the breakdown of Friedel's law is noticable in a difference of the intensities of the reflections g and -g which are not related to a mirror plane (Bijvoet-related reflections).The method can be applied using any transmission electron microscope which is designed for obtaining convergent-beam microdiffraction patterns and in principle, specimen-cooling is not necessary. The crystals have to be oriented to a low-indexed zone axis, where the diffraction plane contains a polar crystal axis.

2015 ◽  
Vol 48 (3) ◽  
pp. 736-746 ◽  
Author(s):  
Katsushi Tanaka ◽  
Norihiko L. Okamoto ◽  
Satoshi Fujio ◽  
Hiroki Sakamoto ◽  
Haruyuki Inui

A convergent-beam electron diffraction (CBED) method is proposed for polarity determination, in which polarity is determined from the intensity asymmetry of any of thehkl–\overline h\overline k\overline l Friedel pairs appearing in a zone-axis CBED pattern with a symmetric arrangement of Bijvoet pairs of reflections. The intensity asymmetry occurs as a result of multiple scattering among Bijvoet pairs of reflections in the CBED pattern. The appropriate zone-axis orientations for polarity determination are deduced for 19 of the 25 polar point groups from symmetry considerations so as to observe Bijvoet pairs of reflections symmetrically in a single CBED pattern. These appropriate zone-axis orientations deduced for the 19 polar point groups coincide with nonpolar directions. This is because the nonpolar directions for these point groups are perpendicular to an even-fold rotation axis, which guarantees the symmetric arrangement of Bijvoet pairs of reflections with respect to the symmetry (m–m′) line in a CBED pattern taken along any of the appropriate zone-axis orientations. Them–m′ line in the CBED pattern is proved to be perpendicular to the trace of the even-fold rotation axis. On the other hand, if the nonpolar direction is either perpendicular to a mirror plane or parallel to a roto-inversion axis as in the four point groupsm, 3m1, 31m, \overline 6, the nonpolar direction cannot be used as the appropriate zone-axis orientation for polarity determination because the Bijvoet pairs of reflections are not arranged symmetrically in the CBED pattern. The validity of the CBED method is confirmed both by experiment and by calculation of CBED patterns.


1985 ◽  
Vol 62 ◽  
Author(s):  
J. A. Eades ◽  
M. J. Kaufman ◽  
H. L. Fraser

ABSTRACTConvergent-beam diffraction in the transmission electron microscope is a powerful technique for the characterization of crystalline materials. Examples are presented to show the way in which convergent-beam zone-axis patterns can be used to determine: the unit cell; the symmetry; the strain of a crystal. The patterns are also recognizable and so can be used, like fingerprints, to identify phases.


Author(s):  
J W Steeds ◽  
R Vincent

We review the analytical powers which will become more widely available as medium voltage (200-300kV) TEMs with facilities for CBED on a nanometre scale come onto the market. Of course, high performance cold field emission STEMs have now been in operation for about twenty years, but it is only in relatively few laboratories that special modification has permitted the performance of CBED experiments. Most notable amongst these pioneering projects is the work in Arizona by Cowley and Spence and, more recently, that in Cambridge by Rodenburg and McMullan.There are a large number of potential advantages of a high intensity, small diameter, focussed probe. We discuss first the advantages for probes larger than the projected unit cell of the crystal under investigation. In this situation we are able to perform CBED on local regions of good crystallinity. Zone axis patterns often contain information which is very sensitive to thickness changes as small as 5nm. In conventional CBED, with a lOnm source, it is very likely that the information will be degraded by thickness averaging within the illuminated area.


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.


Author(s):  
W. T. Pike

With the advent of crystal growth techniques which enable device structure control at the atomic level has arrived a need to determine the crystal structure at a commensurate scale. In particular, in epitaxial lattice mismatched multilayers, it is of prime importance to know the lattice parameter, and hence strain, in individual layers in order to explain the novel electronic behavior of such structures. In this work higher order Laue zone (holz) lines in the convergent beam microdiffraction patterns from a thermal emission transmission electron microscope (TEM) have been used to measure lattice parameters to an accuracy of a few parts in a thousand from nanometer areas of material.Although the use of CBM to measure strain using a dedicated field emission scanning transmission electron microscope has already been demonstrated, the recording of the diffraction pattern at the required resolution involves specialized instrumentation. In this work, a Topcon 002B TEM with a thermal emission source with condenser-objective (CO) electron optics is used.


2013 ◽  
Vol 19 (S5) ◽  
pp. 58-61 ◽  
Author(s):  
Mino Yang ◽  
Jun-Ho Lee ◽  
Hee-Goo Kim ◽  
Euna Kim ◽  
Young-Nam Kwon ◽  
...  

AbstractDistribution of wax in laser printer toner was observed using an ultra-high-voltage (UHV) and a medium-voltage transmission electron microscope (TEM). As the radius of the wax spans a hundred to greater than a thousand nanometers, its three-dimensional recognition via TEM requires large depth of focus (DOF) for a volumetric specimen. A tomogram with a series of the captured images would allow the determination of their spatial distribution. In this study, bright-field (BF) images acquired with UHV-TEM at a high tilt angle prevented the construction of the tomogram. Conversely, the Z-contrast images acquired by the medium-voltage TEM produced a successful tomogram. The spatial resolution for both is discussed, illustrating that the image degradation was primarily caused by beam divergence of the Z-contrast image and the combination of DOF and chromatic aberration of the BF image from the UHV-TEM.


2013 ◽  
Vol 21 (2) ◽  
pp. 40-40
Author(s):  
Lydia Rivaud

Central to the operation of the transmission electron microscope (TEM) (when used with crystalline samples) is the ability to go back and forth between an image and a diffraction pattern. Although it is quite simple to go from the image to a convergent-beam diffraction pattern or from an image to a selected-area diffraction pattern (and back), I have found it useful to be able to go between image and diffraction pattern even more quickly. In the method described, once the microscope is set up, it is possible to go from image to diffraction pattern and back by turning just one knob. This makes many operations on the microscope much more convenient. It should be made clear that, in this method, neither the image nor the diffraction pattern is “ideal” (details below), but both are good enough for many necessary procedures.


2000 ◽  
Vol 6 (S2) ◽  
pp. 946-947 ◽  
Author(s):  
J. R. Michael ◽  
R. P. Goehner

Electron backscatter diffraction (EBSD) is a technique that can provide identification of unknown crystalline phases while exploiting the excellent imaging capabilities of the scanning electron microscope (SEM). Phase identification using EBSD has now progressed to the point that it is commercially available. Phase identification in the SEM requires high quality EBSD patterns that can only be collected using either film or charge coupled device (CCD)-based cameras. High quality EBSD patterns obtained in this manner show many diffraction features that are useful in the determination of the unit cell of the sample.’ This paper will discuss the features in the EBSD patterns and the procedure used to determine the reduced unit cell of the sample.One of the major advantages of EBSD over electron diffraction in the transmission electron microscope is the remarkable field of view that is routinely attained. The large angular view of the diffraction pattern permits many zone axes and their associated symmetries to be viewed in a single pattern or at most a few patterns.


2001 ◽  
Vol 7 (S2) ◽  
pp. 334-335
Author(s):  
J. Tafto

Multilayers, heterostructures, nanostructures and composites are of great interest to the materials scientists, and frequently we encounter crystals lacking centrosymmetry. Thus crystal polarity determination on a microscopic scale is becoming increasingly important in describing interface structures and the internal defects in small crystals. in many cases the polarity of a crystallite can be determined by convergent beam electron diffraction, CBED. Powerful alternatives are to monitor the electron induced x-ray emission, EDS, or electron energy losses, EELS, under channeling conditions. While the determination of the phase of the structure factors, and thus the determination of the crystal polarity, relies on many beam diffraction effects when the CBED technique is used, two-beam experiments provide information about the phase of the structure factor when localized EDS or EELS signals are detected under channeling conditions.The experimental conditions used to determine the polarity and absolute orientation from electron channeling are similar to those used in ALCHEMI experiments to locate small amounts of atoms by electron channeling.


Sign in / Sign up

Export Citation Format

Share Document