Specimen Devices for in Situ Experiments

Author(s):  
P.R. Swann

The space available in the specimen region of the electron microscope has been the major limitation controlling the development of specimen devices. There has always been a tendency for microscope designers to minimize this available space in order to achieve the best electron optical resolution and this has made it very difficult to construct workable specimen devices for double tilting, heating, cooling, straining, etc. This problem has been recognized, however, and some microscopes have been equipped with a second interchangeable objective pole piece which although having a lower resolution has a large upper bore capable of accepting relatively complex top entry cartridges. This design feature has contributed greatly to the development of specimen devices capable of performing in situ experiments. Further impetus to the development of specimen devices has come from the availability of higher voltage microscopes which for equivalent resolutions have a larger working volume in the specimen region than conventional 100KV instruments. A particularly versatile pole piece design used in the AEI EM7 high voltage microscope is shown in figure 1. This design permits rapid exchange between a high resolution top entry pole piece, a wide gap (20mm) pole piece for side entry specimen rods and a wide bore (30mm) pole piece for large top entry specimen cartridges.

Author(s):  
P. R. Swann

The recent availability of high voltage microscopes with their increased specimen penetration and their large working volume in the specimen region has stimulated new attempts to carry out in situ experiments. The thicker specimens which can now be used behave more like bulk material and the large working volume simplifies the design and construction of the special specimen stages required. In most high voltage microscopes several objective pole piece configurations are available but for in situ work the wide gap side entry is preferred because one of the tilt requirements is satisfied in a simple manner by rotating the specimen rod about its axis. Furthermore, tilting about the transverse axis can be achieved by operating a micrometer drive through the nose of the specimen rod thereby leaving the rest of specimen rod free for transmitting services such as cooling and heating to the specimen.


2006 ◽  
Vol 88 (12) ◽  
pp. 123101 ◽  
Author(s):  
D. Golberg ◽  
M. Mitome ◽  
K. Kurashima ◽  
C. Y. Zhi ◽  
C. C. Tang ◽  
...  

2008 ◽  
Vol 8 (11) ◽  
pp. 5878-5886 ◽  
Author(s):  
Jun Wang ◽  
Stephen J. Sollenberger ◽  
Ying Yuan ◽  
Timothy J. Yosenick ◽  
James H. Adair

Silica coated CdS tabular nanocomposites were synthesized through precipitation of CdS nanoparticles in octylamine/water bilayer system followed by in situ hydrolysis of tetraethoxylsilicate (TEOS) precursor. Face diameter of the nanoplatelets was in the range of 50∼250 nm with a variable thickness (3 to 25 nm) dictated by octylamine content or R ratio ([water]/[octylamine]). A uniform SiO2 outer shell of about 15 nm was observed regardless of the size of the high aspect ratio CdS nanoplatelets, which appeared to be agglomerated primarily owing to the confined bilayer template. Morphology and microstructure of the CdS/SiO2 tabular nanocomposites were characterized using atomic force microscope (AFM) and high resolution transmission electron microscope (HRTEM). A noticeable enhancement in absorbance for the UV-vis spectra was observed due to the SiO2 coating layer. Growth mechanism of nanocomposite platelets and potential applications associated with this anisotropic nanocomposite are discussed.


1996 ◽  
Vol 439 ◽  
Author(s):  
Charles W. Allen ◽  
Edward A. Ryan

AbstractSince Fall 1995, a state-of-the-art intermediate voltage electron microscope (IVEM) has been operational in the HVEM-Tandem Facility with in situ ion irradiation capabilities similar to those of the HVEM of the Facility. A 300 kV Hitachi H-9000NAR is interfaced to the two ion accelerators of the Facility, with a demonstrated point-topoint spatial resolution for imaging of 0.25 nm with the ion beamline attached to the microscope. The IVEM incorporates a Faraday cup system for ion dosimetry with measurement aperture 6.5 cm from the TEM specimen, which was described in Symposium A of the 1995 MRS Fall Meeting. The IVEM is now employed for a variety of in situ ion beam studies ranging from low dose ion damage experiments with GaAs, in which damage zones individual displacement cascades are observed, to implantation studies in metals, in which irradiation-induced noble gas precipitate mobility is studied in real time. In this presentation, the new instrumentation and its specifications will be described briefly, several basic concepts relating to in situ experiments in transmission electron microscopes will be summarized and examples of in situ experiments will be presented which exploit the experimental capabilities of this new user facility instrumentation.


1999 ◽  
Vol 5 (S2) ◽  
pp. 476-477
Author(s):  
T. Takizawa ◽  
J. M. Robinson

[Introduction] Immunocytochemical labeling of cryosections, especially immunofluorescence microscopy using semi-thin (0.5-μm) cryosections, has been a powerful technique for detection of cellular antigens in situ and has been widely employed in cell and molecular biology studies. In many cases, immunofluorescence provides sufficient resolution and sensitivity to answer the question being addressed. However, in certain cases the increased resolution of the electron microscope using ultrathin (90-nm) cryosections may be required to define more precisely the localization of specific molecules. Recently, a unique fluorescent ultrasmall immunogold probe, FluoroNanogold (FNG), has been developed for use as a secondary antibody in immunocytochemical applications. It consists of a Fab' fragment of an antibody to which a 1.4-nm gold particle and fluorochromes are conjugated. FNG permits correlative microscopic observation of a sample stained in a single labeling procedure by multiple optical imaging. Recently, we have shown FNG immunocytochemistry on ultrathin cryosections to be valuable for high-resolution correlation of immunofluorescence and immunoelectron microscopy. In the present study, we have examined the utility of FNG as a secondary antibody for immunolabeling of myeloperoxidase (a marker protein for the azurophillic granules) in ultrathin cryosectioned human neutrophils.[Materials and Methods] Purified human neutrophils were fixed with paraformaldehyde, embedded in gelatin, infiltrated with sucrose, cut as ultrathin cryosections, and then collected on formvar film-coated nickel EM grids as described previously. Grids containing ultrathin cryosections were incubated with antimyeloperoxidase and then incubated with FNG.


Author(s):  
M.L. McDonald ◽  
J.M. Gibson

Interest in ultrahigh vacuum (UHV) specimen environments in the transmission electron microscope (TEM) has grown considerably in recent years. The possibility of in-situ studies of atomically clean surfaces has been demonstrated by Yagi et.al., Wilson & Petroff & others. Most designs have involved a side entry specimen holder with cryopumping in the pole piece and are not easily compatible with ultrahigh resolution(UHR) due to size and stability requirements. We have designed a differentially pumped UHV specimen chamber for the JEOL 200CX (UHRTEM). It is intended to allow examination of clean thin specimens at pressures below 10-9 torr with a point to point resolution of 2.5 Å. Provisions for in-situ heating, cooling & deposition have been made. A unique part of this design is the relatively large volume sample chamber held at UHV (figsl&2). This design allows characterization of the atmosphere to which the sample is exposed & cleaning & preparation of samples out of the pole piece which is believed to be necessary for UHRTEM. Another possibility with this design is the transfer of a sample into the TEM from other chambers by use of a transfer case without exposing the sample to an atmosphere above 10-9 torr. Extra ports have been provided to accommodate future experiments.


Author(s):  
K. Furuya ◽  
M. Osaki ◽  
S. Hagiwara ◽  
T. Saito

The ultra high voltage transmission electron microscope (UHV-TEM) having an acceleration voltage of 1000 kV or more has been used for the observation of atomic structure of materials because of its high resolution approaching to 0.1 nm. Few effort has been done to develop an analytical UHV-TEM with energy dispersive x-ray spectroscope (EDS) for in-situ experiments such as ion irradiation, because high density of hard x-ray accompanied with primary electrons is supposed to prevent to measure the characteristic x-ray from the specimen. However, the observation of the heterostructures and interfaces requires analytical capability of determining the local chemical composition compatible with high resolution electron microscopy. This paper describes about a new analytical UHV-TEM (AHV-TEM) equipped with EDS and energy filtered imaging system and its application to Ni silicide thin film.The AHV-TEM in this study is based on JEM-ARM1000 with a side entry goniometer. Figure 1 shows the comparison of calculated CTF and optical diffractogram of amorphous Ge taken near Scherzer defocus with E=1000 keV, Cs=2.6 mm, Cc=3.4 mm and Qi=0.3 mrad.


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