EELS characterization of bulk crystal surfaces in Rem: Surface micro analysis and surface channelling effect

Author(s):  
Z.L. Wang ◽  
J.M. Cowley

Electron energy-loss spectroscopy (EELS) is used in parallel with reflection electron microscopy (REM) for studying surface chemical characterization. The successful observation of Pt and Au M4,5 edge modifications in the REM case has shown that it is possible to do surface chemical analysis for those heavy elements [1]. The reflection of electrons from the surface is critically affected by the surface resonance condition; it has been shown that the electrons will propagate parallel to the surface for some distance if the incident angle satisfies the surface resonance (SR) condition[2-3], then surface channeling is likely to be observed in this SR case. There is less propagation along the surface under the surface non-resonance (SNR) condition.The GaAs bulk crystal (011) surface was chosen for observing the surface channeling effect in REM case, using a Philips 400T TEM. The surface absorbed oxygen is identified with the O-K edge (fig.l(A)).

Author(s):  
L. Wang ◽  
J. Liu ◽  
J. M. Cowley

Single crystal TiO2 (rutile) (110) surface has been characterized by several experimental techniques. In this paper, we report the investigations of “optically polished” as well as high temperature oxygen annealed rutile (110) surfaces by using reflection electron microscopy (REM) and reflection high energy electron diffraction (RHEED) techniques.The crystal was purchased, “optically polished” as-received, from Commercial Crystal Laboratories, Inc.. The details in specimen cutting and surface cleaning procedures have been reported previously. The samples were annealed in pure oxygen at 1425°C for 36 h. The experimental observations were carried out in a Philips 400T microscope operated at 120 kV. The REM images were obtained by selecting the specular reflection spots satisfying surface resonance conditions.Figure 1 is a REM image of as-received rutile (110) surface. The corresponding RHEED pattern is shown in the inset. The azimuthal angle of the incident beam was at 3.9° away from [001] zone axis and the image was formed by choosing (440) specular reflection spot under surface resonance condition.


Author(s):  
Nan Yao ◽  
John M. Cowley

In order to increase intensity and contrast in the image of a surface, the surface resonance conditions have been widely used to enhance the Bragg reflection for image formation in REM (Reflection Electron Microscopy). However, detailed studies of how the resonance conditions relate to the imaging contrast have not been reported. This paper will concentrate on the general properties of the different resonance conditions, as well as the resulting image contrast.Figure 1 shows a series of RHEED (Reflection High Energy Electron Diffraction) patterns and REM images from the same region of a Pt(l11) surface with the incident electron beam in a direction close to the [112] zone axis at 200 KeV, with a glancing incident angle of about 24 mrad which corresponds to the (555) Bragg reflection condition inside the crystal. For the purpose of convenience in discussion, the four different diffraction conditions shown in figures l(al)-(dl) have been named as D1-D4. With Dl, the specular reflected spot falls in an intersection of a parallel Kikuchi line with a parabola; with D2, the specular reflected spot coincides with an intersection of the Kikuchi lines running parallel to and inclined to the crystal surface; with D3, the specular reflected spot crosses only the parallel Kikuchi line; and with D4, the specular reflected spot intersects only with a parabola. It was found that the diffraction conditions Dl and D2 can not be considered as identical, although the specular reflected spots for both cases are commonly regarded as (555) Bragg reflection in the RHEED pattern. Detailed inspection indicates that for Dl, both the Bragg reflection and the electron surface channelling wave are excited, and for D2, the excitement of simultaneous Bragg reflection occurs closely associated with the properties of three-dimensional dynamical diffraction for a bulk crystal.


Author(s):  
Z. L. Wang ◽  
J. Bentley

Studying the behavior of surfaces at high temperatures is of great importance for understanding the properties of ceramics and associated surface-gas reactions. Atomic processes occurring on bulk crystal surfaces at high temperatures can be recorded by reflection electron microscopy (REM) in a conventional transmission electron microscope (TEM) with relatively high resolution, because REM is especially sensitive to atomic-height steps.Improved REM image resolution with a FEG: Cleaved surfaces of a-alumina (012) exhibit atomic flatness with steps of height about 5 Å, determined by reference to a screw (or near screw) dislocation with a presumed Burgers vector of b = (1/3)<012> (see Fig. 1). Steps of heights less than about 0.8 Å can be clearly resolved only with a field emission gun (FEG) (Fig. 2). The small steps are formed by the surface oscillating between the closely packed O and Al stacking layers. The bands of dark contrast (Fig. 2b) are the result of beam radiation damage to surface areas initially terminated with O ions.


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):  
Feng Tsai ◽  
J. M. Cowley

Reflection electron microscopy (REM) has been used to study surface defects such as surface steps, dislocations emerging on crystal surfaces, and surface reconstructions. However, only a few REM studies have been reported about the planar defects emerging on surfaces. The interaction of planar defects with surfaces may be of considerable practical importance but so far there seems to be only one relatively simple theoretical treatment of the REM contrast and very little experimental evidence to support its predications. Recently, intersections of both 90° and 180° ferroelectric domain boundaries with BaTiO3 crystal surfaces have been investigated by Tsai and Cowley with REM.The REM observations of several planar defects, such as stacking faults and domain boundaries have been continued by the present authors. All REM observations are performed on a JEM-2000FX transmission electron microscope. The sample preparations may be seen somewhere else. In REM, the incident electron beam strikes the surface of a crystal with a small glancing angle.


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