On the Faceting of Polar Ceramic Surfaces: Microscopy and Holography Studies of MGO(111) Surfaces

Author(s):  
M. Gajdardziska-Josifovska ◽  
B. G. Frost ◽  
E. Völkl ◽  
L. F. Allard

Polar surfaces are those crystallographic faces of ionically bonded solids which, when bulk terminated, have excess surface charge and a non-zero dipole moment perpendicular to the surface. In the case of crystals with a rock salt structure, {111} faces are the exemplary polar surfaces. It is commonly believed that such polar surfaces facet into neutral crystallographic planes to minimize their surface energy. This assumption is based on the seminal work of Henrich which has shown faceting of the MgO(111) surface into {100} planes giving rise to three sided pyramids that have been observed by scanning electron microscopy. These surfaces had been prepared by mechanical polishing and phosphoric acid etching, followed by Ar+ sputtering and 1400 K annealing in ultra-high vacuum (UHV). More recent reflection electron microscopy studies of MgO(111) surfaces, annealed in the presence of oxygen at higher temperatures, have revealed relatively flat surfaces stabilized by an oxygen rich reconstruction. In this work we employ a combination of optical microscopy, transmission electron microscopy, and electron holography to further study the issue of surface faceting.

Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.


1998 ◽  
Vol 4 (S2) ◽  
pp. 608-609
Author(s):  
Ruud M. Tromp

To obtain a full and detailed understanding of the spatiotemporal dynamics of surface processes such as epitaxial growth, strain relaxation, phase transformations and phase transitions, chemisorption and etching, in situ real-time observations have proven to be invaluable. The development of two experimental techniques, i.e. Low Energy Electron Microscopy (LEEM) typically operating at electron energies below 10 eV, and Ultra-High-Vacuum Transmission Electron Microscopy (UHV-TEM) at several 100 keV, has made such in situ studies routinely possible. In many cases, the videodata obtained from such experiments are amenable to detailed, quantitative analysis, yielding statistical, kinetic and thermodynamic information that cannot be obtained in any other way.I will discuss recent experimental developments, including the design and construction of a new and improved LEEM instrument. Figure 1 shows a schematic diagram of this new machine. There are several features that distinguishes this design from most other LEEMs. One is the use of a 90 degree deflection magnetic prism array,


2001 ◽  
Vol 7 (6) ◽  
pp. 486-493 ◽  
Author(s):  
Judith C. Yang ◽  
Mridula D. Bharadwaj ◽  
Guangwen Zhou ◽  
Lori Tropia

AbstractWe review our studies of the initial oxidation stages of Cu(001) thin films as investigated by in situ ultra-high vacuum transmission electron microscopy. We present our observations of surface reconstruction and the nucleation to coalescence of copper oxide during in situ oxidation in O2. We have proposed a semi-quantitative model, where oxygen surface diffusion is the dominant mechanism of the initial oxidation stages of Cu. We have also investigated the effect of water vapor on copper oxidation. We have observed that the presence of water vapor in the oxidizing atmosphere retards the rate of Cu oxidation and Cu2O is reduced when exposed directly to steam.


Author(s):  
R. H. Geiss ◽  
K. R. Lawless

Pre-thinned high purity tantalum sheet was oxidized in high purity oxygen at 500°C in an ultra high vacuum reactor vessel at pressures of 10 to 100 microns for 30 to 90 minutes. Transmission electron microscopy revealed changes in the microstructure as the oxidation progressed and electron diffraction showed many different sub-oxide phases and marked ordering effects.For the lowest oxygen exposure, 10 microns for 30 minutes, a microstructure showing both large and small domains was found, Figure 1. As can be seen the size and shape of the domains varied considerably. The long narrow domains are near the edge of the foil and all have boundaries along ﹛100﹜ In intermediate regions, about one micron in from the edge, the domains have a peculiar “air plane” shape with boundaries along both ﹛100﹜ and ﹛110﹜ and “wings” adjacent to the ﹛100﹜ boundary. Interspaced among the airplane shaped domains and in regions up to 3 microns from the edge are very small, interconnected nuclei.


Author(s):  
F. A. Ponce ◽  
S. Suzuki ◽  
H. Kobayashi ◽  
Y. Ishibashi ◽  
Y. Ishida ◽  
...  

Electron microscopy in an ultra high vacuum (UHV) environment is a very desirable capability for the study of surfaces and for near-atomic-resolution imaging. The existence of amorphous layers on the surface of the sample generally prevents the direct observation of the free surface structure and limits the degree of resolution in the transmission electron microscope (TEM). In conventional TEM, these amorphous layers are often of organic nature originating from the electron bombardment of hydrocarbons in the vicinity of the sample. They can in part also be contaminants which develop during the specimen preparation and transport stages. In the specimen preparation stage, contamination can occur due to backsputtering during the ion milling process. In addition, oxide layers develop from contact to air during transport to the TEM. In order to avoid these amorphous overlayers it is necessary: i) to improve the vacuum of the instrument, thus the need for ultra high vacuum; and ii) to be able to clean the sample and transfer it to the column of the instrument without breaking the vacuum around the sample.


2005 ◽  
Vol 20 (7) ◽  
pp. 1684-1694 ◽  
Author(s):  
Guangwen Zhou ◽  
Judith C. Yang

The initial oxidation stages of Cu(100), (110), and (111) surfaces have been investigated by using in situ ultra-high-vacuum transmission electron microscopy (TEM) techniques to visualize the nucleation and growth of oxide islands. The kinetic data on the nucleation and growth of oxide islands shows a highly enhanced initial oxidation rate on the Cu(110) surface as compared with Cu(100), and it is found that the dominant mechanism for the nucleation and growth is oxygen surface diffusion in the oxidation of Cu(100) and (110). The oxidation of Cu(111) shows a dramatically different behavior from that of the other two orientations, and the in situ TEM observation reveals that the initial stages of Cu(111) oxidation are dominated by the nucleation of oxide islands at temperatures lower than 550 °C, and are dominated by two-dimensional oxide growth at temperatures higher than 550 °C. This dependence of the oxidation behavior on the crystal orientation and temperature is attributed to the structures of the oxygen-chemisorbed layer, oxygen surface diffusion, surface energy, and the interfacial strain energy.


1994 ◽  
Vol 357 ◽  
Author(s):  
T. Wagner ◽  
M. Ruhle

AbstractThe A1/MgO system has been used as a model system to study growth processes and structure at metal/ceramic interfaces. Aluminum films were grown on air-cleaved MgO (100) substrates in ultra high vacuum (UHV) by molecular beam epitaxy (MBE). The substrates and films were characterized by reflection high energy electron diffraction (RHEED), x-ray diffraction (XRD), conventional transmission electron microscopy (CTEM), and high resolution transmission electron microscopy (HREM). XRD measurements exhibited a pronounced {100} texture. Employing electron diffraction in the TEM on cross sectional samples, we observed the following orientation relationship between Al and MgO: (100)A1 II (100)MgO; [010]A1 II [010]MgO. The atomistic structure of the interface was investigated by HREM. Regions of structural defects can be identified clearly at the interface.


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