Specimen Preparation of Thin Crystalline Fibers for Transmission Electron Microscopy

1990 ◽  
Vol 199 ◽  
Author(s):  
Rosemarie Koch ◽  
Ann F. Marshall

ABSTRACTA technique was developed to prepare crystalline fibers of less than 1 mm diameter for transmission electron microscopy. Cross sections were made by casting a short piece of the fiber in an epoxy resin, sectioning the block, and laminating the slices against thin glass discs for stability before dimpling. Longitudinal sections were reinforced in a similar manner. TEM tungsten rings were sometimes used as an alternative method to add stability to the longitudinal sections. The technique was especially developed for Bi-Sr-Ca-Cu-O compounds but is also suitable for other materials.

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):  
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):  
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.


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