Comparative study of ion milling techniques in cross-sectional transmission electron microscope specimen preparation

1992 ◽  
Vol 22 (2) ◽  
pp. 199-206 ◽  
Author(s):  
E. M. Zielinski ◽  
Bryan Tracy
Author(s):  
Geun-Hong Kim ◽  
Chang-Hwan Chun

Commercial diamond coated WC-Co cutting tool has been investigated by transmission electron microscope (TEM) to understand the nucleation and growth of diamond on WC substrate. Cross-sectional specimens have been prepared by mechanical polishing followed by ion milling. TEM observations have been performed using analytical TEM, JEM 4000FX (JEOL Ltd.).The surface of the coated diamond is composed of grains of 2 - 5 μm in diameter. Each main grain is formed by columnar subgrains of 10 - 50 nm in diameter with similar orientations. Cobalt, a binder in cemented carbide, within 5 μm in depth from the carbide surface has been found to be removed to increase the adhesion of diamond.One of diamond subgrains, which has been grown large in [001] orientation on WC grains is shown in Fig. 1. High density of twins are found on (111) plane starting from WC grain boundaries. It is thought that the interfacial stress between diamond layer and WC grains is accommodated by these twins.


1991 ◽  
Vol 254 ◽  
Author(s):  
L. A. Giannuzzi ◽  
P. R. Howell ◽  
H. W. Pickering ◽  
W. R. Bidter

AbstractA preparation technique for the production of cross-sectional transmission electron microscope (TEM) samples from the interdiffusion regions of Fe-Zn binary couples is described. To alleviate the problem of unequal ion milling rates between the Fe and Zn, a 0.75mm thick Fe sheet has been double plated with a thick electrodeposited Zn coating to achieve a total couple thickness of ˜3mm. After slicing the couple in cross-section, the Fe region of the sample is dimpled to perforation near the Fe-Zn interface. Final thinning for TEM analysis is obtained by ion milling using a liquid nitrogen cold stage and sector speed control. The ion milling procedure is stopped when the perforated hole in the Fe-side of the couple extends through the faster eroding Zn-side of the interface. This technique, in modified form, is expected to be suitable for commercial steels coated with Zn-based alloys.


1998 ◽  
Vol 4 (S2) ◽  
pp. 856-857
Author(s):  
David M. Longo ◽  
James M. Howe ◽  
William C. Johnson

The focused ion beam (FIB) has become an indispensable tool for a variety of applications in materials science, including that of specimen preparation for the transmission electron microscope (TEM). Several FIB specimen preparation techniques have been developed, but some problems result when FIB specimens are analyzed in the TEM. One of these is X-ray fluorescence from bulk material surrounding the thin membrane in FIB-prepared samples. This paper reports on a new FIB specimen preparation method which was devised for the reduction of X-ray fluorescence during energy dispersive X-ray spectroscopy (EDS) in the TEM.Figure 1 shows three membrane geometries that were investigated in this study on a single-crystal Si substrate with a RF sputter-deposited 50 nm Ni film. Membrane 1 is the most commonly reported geometry in the literature, with an approximately 20 urn wide trench and a membrane having a single wedge with a 1.5° incline.


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