Reflection electron microscopy (REM) of NaCl crystals

Author(s):  
Tung Hsu

NaCl and other alkaline halide crystals are unstable under the electron beam and therefore have seldom been examined with the various electron beam techniques. Surfaces of these crystals, however, are of fundamental and application interests. There has been a considerable effort in studying these surfaces using the replica methods.Reflection high energy electron diffraction (RHEED) and reflection electron microscopy (REM) have been successfully applied to the study of stable insulators. Since direct observation on an uncoated surface is always desirable, we tried RHEED and REM on cleaved NaCl(100) surfaces.The experiment was carried out on a JEOL JEM-200CX electron microscope with a high tilt side-entrystage. The accelerating voltage of lOOkV was used throughout the experiment. There is no special protection to the specimen except the standard anti-contamination cold finger. The initial effort of doing ordinary REM on NaCl was a failure: When the electron beam and the specimen were properly tilted toget a good RHEED pattern, the bright pattern remained for only a couple of seconds and then turned into a pattern of weak spots and high diffuse background. The bright REM image also lost its contrast in a few seconds.

Author(s):  
Yootaek Kim ◽  
Tung Hsu

When applying the reflection high energy electron diffraction (RHEED) and reflection electron microscopy (REM) methods[1] on the study of crystal surfaces it is necessary to index the RHEED spots and recognize the azimuth of the electron beam direction. This can be difficult because the RHEED pattern, unlike the transmission electron diffraction (TED) pattern, is distorted by the inner potential of the specimen and only one half of the pattern is shown. We found that it is useful, at the beginning of working on a certain surface of a certain crystal, to record a panoramic RHEED pattern by rotating the crystal through a large azimuth angle. This produces a map which is similar to the Kikuchi maps[2] used in transmission electron microscopy (TEM).Two examples of these panoramic RHEED patterns, one from the Pt(111) [3] and the other from α-Al203 (0001) [4,5,6), are shown in Figs. 1 and 2.The transmission Kikuchi maps are recorded using a specimen of suitable thickness such that the Kikuchi lines are strong and the diffraction spots are practically invisible. On the contrary, in making the panoramic RHEED patterns (or RHEED maps) we have no control over the thickness of the specimen. The electron beam enters and exits the same surface of the crystal; therefore, the relative intensities of the Bragg diffracted spots and the Kikuchi lines are not adjustable. The only adjustment lies in choosing the accelerating voltage and the incidence angle of the electrons such that the RHEED pattern has relatively low diffuse scattering.


Author(s):  
Nan Yao ◽  
J. M. Cowley

The RHEED (Reflection High Energy Electron Diffraction) patterns as essential indications of the diffraction conditions in relation to REM (Reflection Electron Microscopy) imaging provide a wealth of information about the surfaces. They contain extensive patterns of Kikuchi lines, bands and envelopes resulting from diffuse inelastic scattering processes. They also contain arrays of diffuse spots forbidden by the boundary conditions for elastic scattering but generated by multiple diffuse scattering processes.However, a word of caution has to be sounded. Strictly speaking, the normal RHEED pattern does not exactly present the diffraction condition for REM imaging in a commercial transmission electron microscope. Practical and theoretical studies of the electron optics of the illuminating system on a Philip-400T transmission electron microscope, in which the specimen is immersed in the magnetic field of the twin objective lens, indicate that the convergent angle of the incident electron beam can be adjusted precisely, in a range from about 0.1 mrad to 5 mrad, with a selection of the second condenser aperture size, by adjusting the excitation current in the second condenser lens. For the best contrast and illumination, the RHEED pattern is generally obtained by focusing the electron beam on the surface with the maximum convergence angle, and the REM image is obtained with an almost parallel illumination with the minimum convergence angle. A typical example obtained from a fresh cleavage (110) surface of InP single crystal is demonstrated in figure 1, in which (a) and (b) are RHEED patterns with the (10,10,0) specular Bragg-reflection condition fulfilled and correspond to the incident electron beam with 2 mrad and 0.2 mrad convergence angles, respectively; (c) is a REM image obtained under exactly the same operation condition as (b) except for changing from diffraction mode to image mode, which indeed has nothing to do with the illumination condition above the specimen position; and (c) is taken from an area consisting of many steps of atomic height. Comparison of (a) and (b) shows that, for the parallel electron illumination, only those diffraction spots are dominant which represent the possible diffracted directions and mark the intersections of Ewald sphere with reciprocal lattice rods of the crystal surface. The extensive Kikuchi lines, bands and envelopes, and even the parabolas appearing in (a), are scarcely visible in (b). This suggests that the channeling effects characterized as the appearance of surface diffraction parabolas showing in RHEED pattern are mainly caused by the portion of electrons with incident direction slightly deviated from the rows of atoms; that is, the inelastically scattered electrons propagating in the directions of rows of atoms only occur when the initial incident electrons interact with the lattice in a direction slightly different from that of the rows of atoms. Following this argument, we may propose that the contrasts observed in REM image are mostly contributed from the diffraction and phase contrasts.


Author(s):  
Joseph J. Comer ◽  
Charles Bergeron ◽  
Lester F. Lowe

Using a Van De Graaff Accelerator thinned specimens were subjected to bombardment by 3 MeV N+ ions to fluences ranging from 4x1013 to 2x1016 ions/cm2. They were then examined by transmission electron microscopy and reflection electron diffraction using a 100 KV electron beam.At the lowest fluence of 4x1013 ions/cm2 diffraction patterns of the specimens contained Kikuchi lines which appeared somewhat broader and more diffuse than those obtained on unirradiated material. No damage could be detected by transmission electron microscopy in unannealed specimens. However, Dauphiné twinning was particularly pronounced after heating to 665°C for one hour and cooling to room temperature. The twins, seen in Fig. 1, were often less than .25 μm in size, smaller than those formed in unirradiated material and present in greater number. The results are in agreement with earlier observations on the effect of electron beam damage on Dauphiné twinning.


Author(s):  
M. Gajdardziska-Josifovska

Parabolas have been observed in the reflection high-energy electron diffraction (RHEED) patterns from surfaces of single crystals since the early thirties. In the last decade there has been a revival of attempts to elucidate the origin of these surface parabolas. The renewed interest stems from the need to understand the connection between the parabolas and the surface resonance (channeling) condition, the latter being routinely used to obtain higher intensity in reflection electron microscopy (REM) images of surfaces. Several rather diverging descriptions have been proposed to explain the parabolas in the reflection and transmission Kikuchi patterns. Recently we have developed an unifying general treatment in which the parabolas are shown to be K-lines of two-dimensional lattices. Here we want to review the main features of this description and present an experimental diffraction pattern from a 30° MgO (111) surface which displays parabolas that can be attributed to the surface reconstruction.


Author(s):  
Z.L. Wang ◽  
J. Bentley ◽  
R.E. Clausing ◽  
L. Heatherly ◽  
L.L. Horton

It has been found that the abrasion of diamond-on-diamond depends on the crystal orientation. For a {100} face, the friction coefficient for sliding along <011> is much higher than that along <001>. For a {111} face, the abrasion along <11> is different from that in the reverse direction <>. To interpret these effects, a microcleavage mechanism was proposed in which the {100} and {111} surfaces were assumed to be composed of square-based pyramids and trigonal protrusions, respectively. Reflection electron microscopy (REM) has been applied to image the microstructures of these diamond surfaces.{111} surfaces of synthetic diamond:The synthetic diamonds used in this study were obtained from the De Beers Company. They are in the as-grown condition with grain sizes of 0.5-1 mm without chemical treatment or mechanical polishing. By selecting a strong reflected beam in the reflection high-energy electron diffraction (RHEED) pattern, the dark-field REM image of the surface is formed (Fig. 1).


Author(s):  
H. Banzhof ◽  
I. Daberkow

A Philips EM 420 electron microscope equipped with a field emission gun and an external STEM unit was used to compare images of single crystal surfaces taken by conventional reflection electron microscopy (REM) and scanning reflection electron microscopy (SREM). In addition an angle-resolving detector system developed by Daberkow and Herrmann was used to record SREM images with the detector shape adjusted to different details of the convergent beam reflection high energy electron diffraction (CBRHEED) pattern.Platinum single crystal spheres with smooth facets, prepared by melting a thin Pt wire in an oxyhydrogen flame, served as objects. Fig. 1 gives a conventional REM image of a (111)Pt single crystal surface, while Fig. 2 shows a SREM record of the same area. Both images were taken with the (555) reflection near the azimuth. A comparison shows that the contrast effects of atomic steps are similar for both techniques, although the depth of focus of the SREM image is reduced as a result of the large illuminating aperture. But differences are observed at the lengthened images of small depressions and protrusions formed by atomic steps, which give a symmetrical contrast profile in the REM image, while an asymmetric black-white contrast is observed in the SREM micrograph. Furthermore the irregular structures which may be seen in the middle of Fig. 2 are not visible in the REM image, although it was taken after the SREM record.


Author(s):  
JINGYUE LIU

In reflection electron microscopy (REM) and reflection high energy electron diffraction (RHEED) the average path length of the elastically scattered electrons in the crystal ranges from 10 -100 nm and a significant portion of the electrons in the RHEED pattern spots used for imaging is inelastically scattered. The excitations of surface plasmons, bulk plasmons and valence electrons involves energy losses of 10 ∽30 eV. Thus the image contrast and resolution in REM are degraded due to chromatic aberration of the objective lens. The use of energy filters in a TEM should offer significant improvement in resolution and contrast of REM images. We present here some new results on the investigation of resolution limit and contrast mechanisms in energy filtered REM images.The experiments were performed on a Zeiss 912 TEM fitted with an Omega magnetic imaging energy filter. Digital RHEED patterns and REM images were acquired into 1024 pixels by 1024 pixels via a Gatan 679 CCD camera fitted to the microscope.


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