Thin sectioning for cryo transmission electron microscopy (cryo TEM)

Author(s):  
A.W. McDowall ◽  
J.M. Smith ◽  
J. Dubochet

Processing whole cells and tissues for conventional TEM is known to cause structural alterations. Much effort has been devoted, therefore, to developing techniques which avoid specimen preparation artefacts. Recently, research using a cryo-electron microscope has shown that biological suspensions embedded in vitreous ice retain their structural integrity, and when compared with conventionally prepared TEM specimens, are free from many of the classical artefacts. In order to extend the advantage of cryo TEM to whole cells and tissues, we have developed a method of thin sectioning vitrified material.

Author(s):  
R. W. Anderson ◽  
D. L. Senecal

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.


Author(s):  
E. U. Lee ◽  
P. A. Garner ◽  
J. S. Owens

Evidence for ordering (1-6) of interstitial impurities (O and C) has been obtained in b.c.c. metals, such as niobium and tantalum. In this paper we report the atomic and microstructural changes in an oxygenated c.p.h. metal (alpha titanium) as observed by transmission electron microscopy and diffraction.Oxygen was introduced into zone-refined iodide titanium sheets of 0.005 in. thickness in an atmosphere of oxygen and argon at 650°C, homogenized at 800°C and furnace-cooled in argon. Subsequently, thin foils were prepared by electrolytic polishing and examined in a JEM-7 electron microscope, operated at 100 KV.


Author(s):  
Mircea Fotino

A new 1-MeV transmission electron microscope (Model JEM-1000) was installed at the Department of Molecular, Cellular and Developmental Biology of the University of Colorado in Boulder during the summer and fall of 1972 under the sponsorship of the Division of Research Resources of the National Institutes of Health. The installation was completed in October, 1972. It is installed primarily for the study of biological materials without many of the limitations hitherto unavoidable in standard transmission electron microscopy. Only the technical characteristics of the installation are briefly reviewed here. A more detailed discussion of the experimental program under way is being published elsewhere.


Author(s):  
M. J. Carr ◽  
J. F. Shewbridge ◽  
T. O. Wilford

Strong solid state bonds are routinely produced between physical vapor deposited (PVD) silver coatings deposited on sputter cleaned surfaces of two dissimilar metal parts. The low temperature (200°C) and short time (10 min) used in the bonding cycle are advantageous from the standpoint of productivity and dimensional control. These conditions unfortunately produce no microstructural changes at or near the interface that are detectable by optical, SEM, or microprobe examination. Microstructural problems arising at these interfaces could therefore easily go undetected by these techniques. TEM analysis has not been previously applied to this problem because of the difficulty in specimen preparation. The purpose of this paper is to describe our technique for preparing specimens from solid state bonds and to present our initial observations of the microstructural details of such bonds.


Author(s):  
George Guthrie ◽  
David Veblen

The nature of a geologic fluid can often be inferred from fluid-filled cavities (generally <100 μm in size) that are trapped during the growth of a mineral. A variety of techniques enables the fluids and daughter crystals (any solid precipitated from the trapped fluid) to be identified from cavities greater than a few micrometers. Many minerals, however, contain fluid inclusions smaller than a micrometer. Though inclusions this small are difficult or impossible to study by conventional techniques, they are ideally suited for study by analytical/ transmission electron microscopy (A/TEM) and electron diffraction. We have used this technique to study fluid inclusions and daughter crystals in diamond and feldspar.Inclusion-rich samples of diamond and feldspar were ion-thinned to electron transparency and examined with a Philips 420T electron microscope (120 keV) equipped with an EDAX beryllium-windowed energy dispersive spectrometer. Thin edges of the sample were perforated in areas that appeared in light microscopy to be populated densely with inclusions. In a few cases, the perforations were bound polygonal sides to which crystals (structurally and compositionally different from the host mineral) were attached (Figure 1).


Author(s):  
Alfred Baltz

As part of a program to develop iron particles for next generation recording disk medium, their structural properties were investigated using transmission electron microscopy and electron diffraction. Iron particles are a more desirable recording medium than iron oxide, the most widely used material in disk manufacturing, because they offer a higher magnetic output and a higher coercive force. The particles were prepared by a method described elsewhere. Because of their strong magnetic interaction, a method had to be developed to separate the particles on the electron microscope grids.


Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.


Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.


1999 ◽  
Vol 14 (7) ◽  
pp. 3169-3174 ◽  
Author(s):  
Reiko Murao ◽  
Masae Kikuchi ◽  
Kiyoto Fukuoka ◽  
Eiji Aoyagi ◽  
Toshiyuki Atou ◽  
...  

Shock compression experiments on powder mixtures of niobium metal and quartz were conducted for the pressure range of 30–40 GPa by a 25-mm single-stage propellant gun. Chemical reaction occurred above 35 GPa, and products were found to be mainly so-called “Cu3Au-type” Nb3Si, which contained a small amount of oxygen. Microtextures of the specimen were examined by scanning and transmission electron microscopy. A field-emission transmission electron microscope was used for energy-dispersive x-ray analysis of microtextures in small particles found in the SiO2 matrix, and various species with different Nb/Si ratio and oxygen content were shown to be produced through the nonequilibrium process of shock compression.


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