Stage cooling rates and specimen-transfer facilities of the Duke University cryomicroscope

Author(s):  
M.K. Lamvik ◽  
R.E. Worsham ◽  
D.A. Kopf ◽  
J.D. Robertson

A liquid helium cold stage offers unique advantages for biological electron microscopy, including a five-fold reduction in radiation damage, higher ultimate specimen resolution and greater stability for frozen hydrated specimens. Ultra-high vacuum and reduced surface diffusion also reduce specimen contamination to negligible levels. To make efficient use of these advantages in biological studies, however, the microscope must be able to handle a variety of specimens while quickly achieving low temperature.The cryomicroscope that is currently in operation at Duke University (Fig. 1) was originally designed and built at Oak Ridge National Laboratory as a high-resolution electron microscope with a superconducting objective lens. The well-shielded cryostat for the objective lens assures a low specimen temperature. There are two thermal shields surrounding the liquid helium vessel, each cooled by the venting cold helium gas. The inner shield is at its nominal value, 20°K, at the end of the helium transfer when gas is actively venting from the system; later during routine operation, the inner shield temperature is about 30°K.

Author(s):  
R. E. Worsham ◽  
J. E. Mann

In the design of the 150 kV High-Coherence Column, it was considered essential that the specimen be in ultra-high vacuum at liquid helium temperature for minimum radiation damage. It followed that the simplest solution was to make the entire region about the specimen at liquid helium temperature and to make the objective lens with a superconducting winding.For mechanical rigidity, two things were considered essential. First, a strong support structure for the liquid helium vessel and the objective lens. Second, the use of no liquid nitrogen but rather the use of helium vapor cooling for the radiation shields, leads and supports. The drawing, fig. 1, shows the helium vessel, 9-1/2-inches diameter by 5-inches tall, surrounded by two concentric radiation shields. The entire assembly is rigidly supported on four posts one of which is shown. These posts consist of cylinders of epoxyglass (G-10) spacing the components between their different temperatures.


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):  
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. E. Worsham ◽  
J. E. Mann ◽  
E. G. Richardson ◽  
G. G. Slaughter ◽  
N. F. Ziegler

The goal of the development program for high resolution microscopy at Oak Ridge National Laboratory is a 100-500 kV instrument with a point-to-point resolution of at least 1Å. As reported previously, this microscope is intended for biological specimens to be observed at liquid helium temperature. This resolution is to be achieved principally by reduction of the primary spherical aberration for the objective lens with a quadrupole-octupole system of lenses.


Author(s):  
Michel Troyonal ◽  
Huei Pei Kuoal ◽  
Benjamin M. Siegelal

A field emission system for our experimental ultra high vacuum electron microscope has been designed, constructed and tested. The electron optical system is based on the prototype whose performance has already been reported. A cross-sectional schematic illustrating the field emission source, preaccelerator lens and accelerator is given in Fig. 1. This field emission system is designed to be used with an electron microscope operated at 100-150kV in the conventional transmission mode. The electron optical system used to control the imaging of the field emission beam on the specimen consists of a weak condenser lens and the pre-field of a strong objective lens. The pre-accelerator lens is an einzel lens and is operated together with the accelerator in the constant angular magnification mode (CAM).


Author(s):  
William Krakow

In recent years electron microscopy has been used to image surfaces in both the transmission and reflection modes by many research groups. Some of this work has been performed under ultra high vacuum conditions (UHV) and apparent surface reconstructions observed. The level of resolution generally has been at least an order of magnitude worse than is necessary to visualize atoms directly and therefore the detailed atomic rearrangements of the surface are not known. The present author has achieved atomic level resolution under normal vacuum conditions of various Au surfaces. Unfortunately these samples were exposed to atmosphere and could not be cleaned in a standard high resolution electron microscope. The result obtained surfaces which were impurity stabilized and reveal the bulk lattice (1x1) type surface structures also encountered by other surface physics techniques under impure or overlayer contaminant conditions. It was therefore decided to study a system where exposure to air was unimportant by using a oxygen saturated structure, Ag2O, and seeking to find surface reconstructions, which will now be described.


1986 ◽  
Vol 67 ◽  
Author(s):  
N. Otsuka ◽  
C. Choi ◽  
Y. Nakamura ◽  
S. Nagakura ◽  
R. Fischer ◽  
...  

ABSTRACTRecent studies have shown that high quality GaAs films can be grown by MBE on Si substrates whose surfaces are slightly tilted from the (100) plane. In order to investigate the effect of the tilting of substrate surfaces on the formation of threading dislocations, the GaAs/Si epitaxial interfaces have been observed with a 1 MB ultra-high vacuum, high voltage electron microscope. Two types of misfit dislocations, one with Burgers vectors parallel to the interface and the other with Burgers vectors inclined from the interface, were found in these epitaxial interfaces. The observation of crosssectional samples perpendicular to each other has shown that the tilting of the substrate surface directly influences the generation of these two types of misfit dislocations. The mechanism of the reduction of threading dislocations by the tilting of the substrate surface is discussed based on these observations.


1999 ◽  
Vol 5 (S2) ◽  
pp. 646-647
Author(s):  
H.W. Mook ◽  
A.H.V. van Veen ◽  
P. Kruit

The energy resolution which can be attained in electron energy loss spectroscopy (EELS) is determined by the energy spread of the electron source. The energy width of a high brightness electron gun (typically 0.4 to 0.8 eV) blurs the energy spectrum. A pre-specimen energy filter or monochromator must be used to reduce the energy width of the beam below 0.1 eV to allow detailed EELS analysis of the electronic band structures in materials. The monochromator can not only improve EELS, but it is also capable of improving the spatial resolution in low voltage SEM, which is limited by the chromatic blur of the objective lens. A new type of monochromator the Fringe Field Monochromator has been designed and experiments in an ultra high vacuum setup show the monochromatisation of a Schottky Field Emission Gun.


2001 ◽  
Vol 7 (S2) ◽  
pp. 906-907
Author(s):  
L. F. Allard ◽  
E. Voelkl ◽  
D. A. Blom ◽  
T. A. Nolan ◽  
F. Kahl ◽  
...  

Field emission electron microscopes operating at 200kV or 300kV and incorporating aberration correctors for either the incident electron probe or for the primary aberrations of the objective lens (OL) are currently under development for several laboratories in the world. OL-corrected instruments require monochromators for the electron beam, built into the electron gun prior to the accelerating stages, in order to optimize the contrast transfer characteristics of the objective lens to push the instrumental resolution limit to well beyond 0.1nm. This will allow the point resolution limit as controlled by the correction of spherical aberration Cs to potentially extend to the instrumental limit of better than 0.1nm. Figure 1 shows the contrast transfer characteristics of a Cs-corrected 200kV TEM, both without and with a beam monochromator.Dedicated STEM instruments such as the 300kV VG-603 and lOOkV VG-501 at Oak Ridge National Laboratory, and other VG instruments at Cornell University and IBM Co. are also being adapted (by Nion Co., Kirkland, WA) to incorporate aberration correctors for the incident probe. The aim is to improve the resolution of the VG-603 instrument in dark-field imaging mode, for example, from 0.13nm to 0.05nm. in another ORNL project, the High Temperature Materials Laboratory has contracted JEOL Ltd. to construct a STEM-TEM instrument with a probe corrector designed and built by CEOS GmbH (Heidelberg, Germany).


Sign in / Sign up

Export Citation Format

Share Document