High Resolution Observations of Ion-Milling Induced Transformation in Synthetic Hollandses

Author(s):  
T. J. Headley

Oxide phases having the hollandite structure have been identified in multiphase ceramic waste forms being developed for radioactive waste disposal. High resolution studies of phases in the waste forms described in Ref. [2] were initiated to examine them for fine scale structural differences compared to natural mineral analogs. Two hollandites were studied: a (Ba,Cs,K)-titan-ate with minor elements in solution that is produced in the waste forms, and a synthesized BaAl2Ti6O16 phase containing ∼ 4.7 wt% Cs2O. Both materials were consolidated by hot pressing at temperatures above 1100°C. Samples for high resolution microscopy were prepared both by ion-milling (7kV argon ions) and by crushing and dispersing the fragments on holey carbon substrates. The high resolution studies were performed in a JEM 200CX/SEG operating at 200kV.

Author(s):  
M. Hornbostel ◽  
F.J. DiSalvo ◽  
S. Hillyard ◽  
J. Silcox

LiMo3Se3 is a highly anisotropic conductor containing 6Å diameter one dimensional chains of Mo3Se3 triangles. This compound can be dissolved in polar solvents to produce solutions containing micron length Mo3Se3 fibers. Choice of solvent and solution concentrations allows some control of fiber diameters, from a few hundred angstroms down to the molecular limit of a single 6Å diameter chain. These fibers have been deposited from solution on holey carbon substrates by vacuum evaporation of the solvent to produce free-standing, one dimensional wires.High resolution microscopy at 100kV was carried out in a VG HB501A STEM and confirms the presence of many different sized bundles extending all the way down to the single strands. Figure 1a shows an ADF image of a medium sized strand which commonly occured in a sample prepared with the solvent propylene carbonate. The flexibility of the fiber and its seeming attraction to the edges of carbon holes is apparent as it snakes its way along the surface.


Author(s):  
H.A. Cohen ◽  
T.W. Jeng ◽  
W. Chiu

This tutorial will discuss the methodology of low dose electron diffraction and imaging of crystalline biological objects, the problems of data interpretation for two-dimensional projected density maps of glucose embedded protein crystals, the factors to be considered in combining tilt data from three-dimensional crystals, and finally, the prospects of achieving a high resolution three-dimensional density map of a biological crystal. This methodology will be illustrated using two proteins under investigation in our laboratory, the T4 DNA helix destabilizing protein gp32*I and the crotoxin complex crystal.


Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.


Author(s):  
P. A. Marsh ◽  
T. Mullens ◽  
D. Price

It is possible to exceed the guaranteed resolution on most electron microscopes by careful attention to microscope parameters essential for high resolution work. While our experience is related to a Philips EM-200, we hope that some of these comments will apply to all electron microscopes.The first considerations are vibration and magnetic fields. These are usually measured at the pre-installation survey and must be within specifications. It has been our experience, however, that these factors can be greatly influenced by the new facilities and therefore must be rechecked after the installation is completed. The relationship between the resolving power of an EM-200 and the maximum tolerable low frequency interference fields in milli-Oerstedt is 10 Å - 1.9, 8 Å - 1.4, 6 Å - 0.8.


Author(s):  
W. O. Saxton

Recent commercial microscopes with internal microprocessor control of all major functions have already demonstrated some of the benefits anticipated from such systems, such as continuous magnification, rotation-free diffraction and magnification, automatic recording of mutually registered focal series, and fewer control knobs. Complete automation of the focusing, stigmating and alignment of a high resolution microscope, allowing focal series to be recorded at preselected focus values as well, is still imminent rather than accomplished, however; some kind of image pick-up and analysis system, fed with the electron image via a TV camera, is clearly essential for this, but several alternative systems and algorithms are still being explored. This paper reviews the options critically in turn, and stresses the need to consider alignment and focusing at an early stage, and not merely as an optional extension to a basic proposal.


Author(s):  
William Krakow ◽  
David A. Smith

Recent developments in specimen preparation, imaging and image analysis together permit the experimental determination of the atomic structure of certain, simple grain boundaries in metals such as gold. Single crystal, ∼125Å thick, (110) oriented gold films are vapor deposited onto ∼3000Å of epitaxial silver on (110) oriented cut and polished rock salt substrates. Bicrystal gold films are then made by first removing the silver coated substrate and placing in contact two suitably misoriented pieces of the gold film on a gold grid. Controlled heating in a hot stage first produces twist boundaries which then migrate, so reducing the grain boundary area, to give mixed boundaries and finally tilt boundaries perpendicular to the foil. These specimens are well suited to investigation by high resolution transmission electron microscopy.


Author(s):  
Terrence Reilly ◽  
Al Pelillo ◽  
Barbara Miner

The use of transmission electron microscopes (TEM) has proven to be very valuable in the observation of semiconductor devices. The need for high resolution imaging becomes more important as the devices become smaller and more complex. However, the sample preparation for TEM observation of semiconductor devices have generally proven to be complex and time consuming. The use of ion milling machines usually require a certain degree of expertise and allow a very limited viewing area. Recently, the use of an ultra high resolution "immersion lens" cold cathode field emission scanning electron microscope (CFESEM) has proven to be very useful in the observation of semiconductor devices. Particularly at low accelerating voltages where compositional contrast is increased. The Hitachi S-900 has provided comparable resolution to a 300kV TEM on semiconductor cross sections. Using the CFESEM to supplement work currently being done with high voltage TEMs provides many advantages: sample preparation time is greatly reduced and the observation area has also been increased to 7mm. The larger viewing area provides the operator a much greater area to search for a particular feature of interest. More samples can be imaged on the CFESEM, leaving the TEM for analyses requiring diffraction work and/or detecting the nature of the crystallinity.


2010 ◽  
Vol 17 (3) ◽  
pp. 1000-1008 ◽  
Author(s):  
Shareghe Mehraeen ◽  
Apoorva Kulkarni ◽  
Miaofang Chi ◽  
Bryan W. Reed ◽  
Norihiko L. Okamoto ◽  
...  

1981 ◽  
Vol 11 ◽  
Author(s):  
H. C. Burkholder

In response to draft radioactive waste disposal standards, R&D programs have been initiated in the United States which are aimed at developing and ultimately using radionuclide transport-delaying (e.g., long-lived waste containers) and radionuclide transport-controlling (e.g., very low release rate waste forms) engineered components as part of the isolation system. Before these programs proceed significantly, it seems prudent to evaluate the technical justification for development and use of sophisticated engineered components in radioactive waste isolation.


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