Surface Structures and Rearrangements in Oxides

1990 ◽  
Vol 183 ◽  
Author(s):  
M. R. Mccartney ◽  
David J. Smith

AbstractElectron-beam-induced surface reactions and rearrangements have been observed for a number of oxides including MgO, TiO2, SrTiO3 and SnO2 using conventional and ultra-high-vacuum high-resolution electron microscopes. Electron irradiation of TiO2 resulted in a variety of effects including reduction, re-oxidation and amorphization. SnO2 was observed to form facets readily during high-resolution imaging but it was stable against reduction except when exposed to extreme current densities which caused the formation of metallic tin crystals. Electron irradiation of MgO under UHV conditions resulted in the formation of facetted pits. The surfaces of SrTiO3 were stable for moderate electron dose rates but rapidly amorphized when irradiated at extreme current densities.

Author(s):  
M. R. McCartney ◽  
David J. Smith

The examination of surfaces requires not only that they be free of adsorbed layers but the environment of the sample must also be maintained at high vacuum so that the surfaces remain clean. The possibility of resolving surface structures with atomic resolution has provided the motivation for optimizing intermediate and high voltage electron microscopes for this particular application. Electron microscopy offers a variety of techniques which have the capability of achieving atomic level detail of surfaces including plan-view imaging, REM and profile imaging. Operation at higher voltages permits reasonable pole piece dimensions thereby providing space for in situ studies yet still compatible with high resolution. Moreover, video systems can be attached which permit observation and recording of dynamic phenomena without compromising microscope performance.


Author(s):  
William Goldfarb ◽  
Benjamin M. Siegel

The image collecting system of the experimental high resolution electron microscope being developed in this laboratory must be compatible with the ultra-high vacuum (10−10Torr) maintained in the total column. The characteristics of an SEC porous KCl target used to record directly the primary high energy beam has been previously reported. It was also noted that a phosphor transducer could be used with an external recording medium without loss of information if adequate electron optical magnification and sufficient light coupling are utilized.


Author(s):  
D. L. Musinski ◽  
S. T. Wang ◽  
B. M. Siegel

The specimen environment for high resolution microscopy of biomolecular materials is critical. To obtain the optimum conditions we maintain the specimen in an ultra high vacuum (10-10 Torr) and at liquid helium temperatures to minimize contamination and hopefully radiation damage. To meet these specifications, the imaging system composed of the cryostat shown in the schematic drawing was developed and constructed. Besides assuring that the basic design does not limit the desired resolution, our cryostat offers the maximum in engineering flexibility so alternate lens configurations or even extensive design modifications are relatively easy to accomplish.


Author(s):  
M. Shamzuzzoha ◽  
P.A. Deymier ◽  
David J. Smith

The determination of the core structure of grain boundaries is central to a better understanding of the properties of polycrystalline materials. With the recent advent of intermediate-voltage electron microscopes (300-400kV), it is possible to obtain atomic-resolution images of grain boundaries in many metals - for example, the atomic structure of periodic grain boundaries in selected metals has been studied. Our knowledge of materials properties can be further enhanced by investigating more complex, arbitrarily misoriented grain boundaries. In this paper, we will report HREM imaging of a symmetric tilt low-angle grain boundary and a twist-and-tilt (mixed character) grain boundary in Al.The Al bicrystals used in this study were produced by cross-rolling and annealing methods described in detail elsewhere. Thin foil specimens of 3mm diameter containing specific boundaries were obtained by spark-cutting and subsequent electropolishing in 73% methanol, 25% nitric acid and 2% hydrochloric acid. HREM was performed with a JEM-4000EX operated at 400kV, using axial illumination and without an objective aperture. High-resolution electron micrographs were recorded near the optimum defocus, typically at a magnification of 500,000 times.


Author(s):  
Ping Lu ◽  
David J. Smith

Surface profile imaging at resolutions of better than 2Å is highly suitable for studies of surface structures and reactions. In the case of semiconductor materials, the main challenge is to prepare surfaces free of any contamination. The technique has previously been used to study surface reconstructions of Si and CdTe. In our previous observations, clean surfaces of CdTe were obtained by careful control of the incident electron beam within a JEM-4000EX high resolution electron microscope with a pressure of 10-7 torr. In the present study, observations of reconstructions and dynamic phenomena on CdTe surfaces were carried out with a Phillips-430ST, modified for Ultra-High Vacuum in the vicinity of the specimen and equipped with an in situ heating facility. The base vacuum in the region of the sample could usually reach ∼3×l0-9 torr after baking the microscope column at ∼120°C for 36 hours. The CdTe specimen was prepared by cutting a large single crystal into 3mm discs in a [110] direction, then mechanically polishing to a thickness of ∼20 microns, and finally ion milling to perforation.When viewed along a [110] projection, the CdTe sample was found to be dominated by clean or nearly clean (111) and (110) surfaces(with amorphous materials less than 5Å) whilst the (001) surface was usually very short and rough. A completely clean surface was obtained by in situ annealing of the crystal to about 200°. The (110) surface was then found to be reconstructed with a very characteristic chevron appearance in the manner described previously. Long and flat CdTe(OOl) surfaces were obtained by insitu annealing of the crystal at ∼510°C at which temperature edges of the crystal started to gradually sublime. Characterization of the surface structure was then possible when the crystal was cooled back down to temperatures below about 300°C. It was found that the (001) surface had a (2×1) reconstruction at temperatures below about 200°C which transformed reversibly into a (3×1) reconstruction over the approximate temperature range of 200°C<T<300°C. Figures la and lb show the (2×1) and (3×1) reconstructed (001) surfaces, viewed along the [110] projection, which were recorded at temperatures of 140°C and 240°C respectively. Structural models for the (2×1) and (3×1) reconstructions, obtained directly on the basis of the experimental images, are shown in Figs.2a and 2b respectively. The (2×1) reconstruction involves a 1/2 monolayer of Cd vacancies and a very large inward contraction of the remaining Cd surface atoms, which then displace the second layer of Te atoms as indicated. This model is similar to that proposed by Chadi for the Ga-rich (2×1) reconstructed GaAs(100) surface. The (3×1) reconstruction involves both the formation of surface dimers and the presence of vacancies at the surface. Every third atomic-pair is missing along the [1,-1,0] direction, and the remaining two atom pairs at the surface form the surface dimer. Although the (3×1) reconstruction has a larger number of electrons in dangling bonds, a surface with vacancies can be relaxed to reduce the strain energy due to the surface dimers. The directions of the atomic displacements away from the ideal dimer positions are indicated in the figure. Relatively large atomic displacements for several layers into the bulk are clearly visible in experimental images, as seen in Fig.lb. Further details of the surface reconstructions can be found elsewhere.


2001 ◽  
Vol 7 (S2) ◽  
pp. 880-881 ◽  
Author(s):  
Peter Gnauck ◽  
Volker Drexel ◽  
J. Greiser

To examine non conductive samples in their natural state (i.e. without significant sample preparation) at high resolution in the SEM the technique of low voltage field emission scanning electron microscopy (LVFESEM) is used. Due to the limitation in accelerating voltage (U<1kV) this technique is limited in respect of chemical analysis. Furthermore it is not possible to examine humid and outgassing samples in high vacuum. in recent years the application of variable pressure scanning electron microscopes (VPSEM) became an important technique in materials science as well as in life science. Due to the capability of maintaining a high chamber pressure humid, outgassing and non-conductive samples, can be examined in their natural state without significant sample modification or preparation. Especially compound materials with different electron yields can be imaged without any charging effects (Fig. 2), [2]. This paper describes a high resolution field emission electron microscope, that combines low voltage and variable pressure capabilities.The high pressure capabilities of the instrument are realized by eliminating the high vacuum requirements of SEM in the microscope chamber. This is done by separating the vacuum environment in the chamber from the ultra high vacuum environment in the gun area.


Author(s):  
Nestor J. Zaluzec ◽  
John F. Mansfield

The advent of medium and high voltage electron microscopes having high brightness electron sources and ultra-high vacuum environments has been awaited with great anticipation for the last few years. There has been a particuliarly keen interest with respect to their potentials for enhanced performance in analytical and high resolution modes. Along with these positive aspects there are also the inevitable detrimental effects, the foremost of these relative to microcharacterization are electron sputtering, displacement damage and concomittent radiation induced segregation (RIS) of the various atomic species within the specimen. Previous work on this problem has concentrated upon the RIS aspects, in this study we have expanded calculations to include a comparision of electron induced sputtering.


Author(s):  
Peter R. Swann ◽  
Joseph S. Jones ◽  
Ondrei L. Krivanek ◽  
David J. Smith ◽  
John A. Venables ◽  
...  

Ultra-high-vacuum high-resolution electron microscopy (UHV-HREM) is a powerful technique for studying the structure of surfaces, and for characterizing the mechanisms and kinetics of surface and interface reactions. It requires an electron microscope capable of atomic resolution, a vacuum of about 10-10 torr around the sample, and a range of specimen treatment capabilities. We have replaced the standard specimen chamber of a Philips 430ST high resolution microscope by a special UHV chamber which allows for limited specimen treatment in-situ, and a full range of specimen treatments in a preparation chamber mounted on the side of the microscope column. At 300 kV, the objective lens (Cs= Cc = 1.1mm) of the 430ST has demonstrated a point-to-point resolution of 2.0 Å, and a spatial frequency transfer limit with axial illumination of better than 1.5 Å. A critical specification for the microscope conversion was that this performance should not be compromised even under full UHV operation.


Author(s):  
R. Ai ◽  
D.N. Dunn ◽  
T.S. Savage ◽  
J.P. Zhang ◽  
L.D. Marks

The recent development of ultra high vacuum high resolution electron microscopes has made it possible to use an electron microscope to study surface structures with atomic resolution. Although surface images of Au(110) 2x11 and Si(111) 7x72 reconstructions have been obtained, no standard TEM sample preparation technique for surface imaging has been developed for routine uses. In conventional surface science, the common method of producing an UHV clean sample is a combination of ion sputtering and annealing; can this process be used to produce TEM samples for surface imaging. Our studies show that clean, well order TEM samples can be achieved by this approach.


Author(s):  
R. Ai

With the recent development of ultra-high vacuum high resolution electron microscopes (UHV-HREM), electron microscopes have become valuable tools for surface studies. Techniques such as surface profile image, surface sensitive plane view, and reflection electron microscopy have been developed to take full advantage of the atomic resolution of HREM to study surface structures. However a complete surface study requires information on both the surface structure and surface chemistry. Therefore in order to turn an electron microscope into a real surface analytical tool, the challenge is to develop a microscopecompatible, surface sensitive tool for in-situ surface chemical analysis.


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