Studies of Oxide Formation on Copper Thin Films by Electron Microscopy

Author(s):  
G. G. Hembree ◽  
M. A. Otooni ◽  
J. M. Cowley

The formation of oxide structures on single crystal films of metals has been investigated using the REMEDIE system (for Reflection Electron Microscopy and Electron Diffraction at Intermediate Energies) (1). Using this instrument scanning images can be obtained with a 5 to 15keV incident electron beam by collecting either secondary or diffracted electrons from the crystal surface (2). It is particularly suited to studies of the present sort where the surface reactions are strongly related to surface morphology and crystal defects and the growth of reaction products is inhomogeneous and not adequately described in terms of a single parameter. Observation of the samples has also been made by reflection electron diffraction, reflection electron microscopy and replication techniques in a JEM-100B electron microscope.A thin single crystal film of copper, epitaxially grown on NaCl of (100) orientation, was repositioned on a large copper single crystal of (111) orientation.

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.


1975 ◽  
Vol 46 (7) ◽  
pp. 826 ◽  
Author(s):  
J. M. Cowley ◽  
J. L. Albain ◽  
G. G. Hembree ◽  
P. E. Ho̸jlund-Nielsen ◽  
F. A. Koch ◽  
...  

Author(s):  
Frank E. Wawner ◽  
Kenneth R. Lawless

Thin single crystal films of high purity titanium were needed in our laboratory for investigations of the early stages of the oxidation of titanium. Experiments were carried out to determine the feasibility of preparing single crystal titanium films of different orientations by evaporation onto the (100), (110) and (111) surfaces of rocksalt. The structures of these films were investigated by transmission electron microscopy and electron diffraction.


Author(s):  
H.-J. Ou

Studies of the surface structure of silicon with good spatial resolution made recently by reflection electron microscopy, (REM) have complemented and greatly extended the earlier studies, made by LEED and other methods, of the formation of surface reconstruction superstructures such a the Si(111) 7x7. These studies have not included the 2x1 superstructure on (111) surfaces formed by cleaving Si crystals in ultra-high vacuum. We have now investigated the form of the domains of this 2x1 structure by use of a reconstructed REMEDIE system 2.3 (for Reflection Electron Microscopy and Electron Diffraction at Intermediate Energies, 1-20keV). This system has shown a spatial resolution of better than 100Å although resolutions of about 300Å may be more common in practise because of the limitations due to probe size, vibration and signal noise.


Author(s):  
Akira Tanaka ◽  
David F. Harling

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.


2020 ◽  
Vol 6 (1) ◽  
pp. 1-7
Author(s):  
Tatyana V. Kritskaya ◽  
Vladimir N. Zhuravlev ◽  
Vladimir S. Berdnikov

We have improved the well-known Czochralski single crystal silicon growth method by using two argon gas flows. One flow is the main one (15–20 nl/min) and is directed from top to bottom along the growing single crystal. This flow entrains reaction products of melt and quartz crucible (mainly SiO), removes them from the growth chamber through a port in the bottom of the chamber and provides for the growth of dislocation-free single crystals from large weight charge. Similar processes are well known and have been generally used since the 1970s world over. The second additional gas flow (1.5–2 nl/min) is directed at a 45 arc deg angle to the melt surface in the form of jets emitted from circularly arranged nozzles. This second gas flow initiates the formation of a turbulent melt flow region which separates the crystallization front from oxygen-rich convective flows and accelerates carbon evaporation from the melt. It has been confirmed that oxygen evaporated from the melt (in the form of SiO) acts as transport agent for nonvolatile carbon. Commercial process implementation has shown that carbon content in as-grown single crystals can be reduced to below the carbon content in the charge. Single crystals grown with two argon gas flows have also proven to have highly macro- and micro-homogeneous oxygen distributions, with much greater lengths of single crystal portions in which the oxygen concentration is constant and below the preset limit. Carbon contents of 5–10 times lower than carbon content in the charge can be achieved with low argon gas consumption per one growth process (15–20 nl/min vs 50–80 nl/min for conventional processes). The use of an additional argon gas flow with a 10 times lower flowrate than that of the main flow does not distort the pattern of main (axial) flow circumvention around single crystal surface, does not hamper the “dislocation-free growth” of crystals and does not increase the density of microdefects. This suggests that the new method does not change temperature gradients and does not produce thermal shocks that may generate thermal stresses in single crystals.


1997 ◽  
Vol 3 (S2) ◽  
pp. 1039-1040
Author(s):  
R. Plass ◽  
K. Egan ◽  
C. Collazo-Davila ◽  
D. Grozea ◽  
E. Landree ◽  
...  

It has long been thought that (111) surfaces of rock salt oxides microfacet to neutral surfaces upon annealing because of the very large energies involved in bulk terminating a layer of like ions. However in a recent reflection electron microscopy (REM) study Gajdardziska-Josifovska et al. found that MgO(lll) surfaces annealed in flowing oxygen furnaces at 1500°C not only did not microfacet, but displayed a √3×√3R30° surface periodicity that was stable in air. To determine the structure of this unusually stable surface MgO (111) transmission electron microscopy (TEM) samples were annealed in a vacuum furnace in the present study and their transmission electron diffraction (TED) patterns were analyzed with direct phasing methods.The TEM samples were prepared by orienting a MgO single crystal and sawing lmm wafers along a (111) plane. Disk samples were then ultrasonically drilled, dimpled, mechanically polished and/or hot nitric acid etched, and milled with 5 KeV Ar+ ions.


Sign in / Sign up

Export Citation Format

Share Document