Preparation of cross-sectional transmission electron microscopy samples by electron beam lithography and reactive ion etching

1989 ◽  
Vol 11 (1) ◽  
pp. 62-69 ◽  
Author(s):  
J. T. Wetzel
1990 ◽  
Vol 199 ◽  
Author(s):  
Jeffrey T. Wetzel ◽  
K. L. Kavanagh

ABSTRACTThis paper summarizes methods used to create cross-sectional samples for transmission electron microscopy and introduces another variant of the technique all of which rely upon some combination of lithographic patterning and reactive ion etching. The basic idea pursued in using these techniques was to form, from a preselected location, samples that had a large transparent area without use of mechanical polishing or ion milling. Samples were successfully prepared in this manner, but room for improvement remains due to the limited range of diffraction conditions available for imaging or diffraction pattern formation.


Author(s):  
V.P. Dravid ◽  
M.R. Notis ◽  
C.E. Lyman ◽  
A. Revcolevschi

Transmission electron microscopy (TEM), incorporating imaging, diffraction and spectrometry has contributed significantly to the understanding of the structure of crystalline interfaces. Traditionally, planar interfaces are investigated using cross-sectional views (electron beam parallel to the interface) of the specimen. However, plan-view TEM (PVTEM) has recently emerged as a viable and supplementary technique to cross-sectional TEM (XTEM). PVTEM enjoys certain definite advantages over XTEM. One important consideration is that the interface in a PV specimen is buried (sandwiched between two crystals) and is expected to be free of artefacts induced by specimen preparation procedures. Moreover, many multilayer electronic materials are amenable to PVTEM because they can be easily backthinned to electron transparency with virtually no damage to the internal interfaces. PV specimens clearly contain much larger interface area than XTEM specimens, which may be of great significance when statistics are considered. Apart from these considerations PVTEM studies can also offer specific information about the interface not always possible in XTEM. In this brief communication we report some of our results on imaging, diffraction and spectrometry of interfaces obtained by viewing the interfaces in the PV mode.


Author(s):  
G. G. Shaw

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.


Author(s):  
Joseph J. Comer ◽  
Charles Bergeron ◽  
Lester F. Lowe

Using a Van De Graaff Accelerator thinned specimens were subjected to bombardment by 3 MeV N+ ions to fluences ranging from 4x1013 to 2x1016 ions/cm2. They were then examined by transmission electron microscopy and reflection electron diffraction using a 100 KV electron beam.At the lowest fluence of 4x1013 ions/cm2 diffraction patterns of the specimens contained Kikuchi lines which appeared somewhat broader and more diffuse than those obtained on unirradiated material. No damage could be detected by transmission electron microscopy in unannealed specimens. However, Dauphiné twinning was particularly pronounced after heating to 665°C for one hour and cooling to room temperature. The twins, seen in Fig. 1, were often less than .25 μm in size, smaller than those formed in unirradiated material and present in greater number. The results are in agreement with earlier observations on the effect of electron beam damage on Dauphiné twinning.


Author(s):  
D. L. Callahan ◽  
Z. Ball ◽  
H. M. Phillips ◽  
R. Sauerbrey

Ultraviolet laser-irradiation can be used to induce an insulator-to-conductor phase transition on the surface of Kapton polyimide. Such structures have potential applications as resistors or conductors for VLSI applications as well as general utility electrodes. Although the percolative nature of the phase transformation has been well-established, there has been little definitive work on the mechanism or extent of transformation. In particular, there has been considerable debate about whether or not the transition is primarily photothermal in nature, as we propose, or photochemical. In this study, cross-sectional optical microscopy and transmission electron microscopy are utilized to characterize the nature of microstructural changes associated with the laser-induced pyrolysis of polyimide.Laser-modified polyimide samples initially 12 μm thick were prepared in cross-section by standard ultramicrotomy. Resulting contraction in parallel to the film surface has led to distortions in apparent magnification. The scale bars shown are calibrated for the direction normal to the film surface only.


Author(s):  
L. D. Peachey ◽  
J. P. Heath ◽  
G. Lamprecht

Biological specimens of cells and tissues generally are considerably thicker than ideal for high resolution transmission electron microscopy. Actual image resolution achieved is limited by chromatic aberration in the image forming electron lenses combined with significant energy loss in the electron beam due to inelastic scattering in the specimen. Increased accelerating voltages (HVEM, IVEM) have been used to reduce the adverse effects of chromatic aberration by decreasing the electron scattering cross-section of the elements in the specimen and by increasing the incident electron energy.


Author(s):  
F. Shaapur

Non-uniform ion-thinning of heterogenous material structures has constituted a fundamental difficulty in preparation of specimens for transmission electron microscopy (TEM). A variety of corrective procedures have been developed and reported for reducing or eliminating the effect. Some of these techniques are applicable to any non-homogeneous material system and others only to unidirectionalfy heterogeneous samples. Recently, a procedure of the latter type has been developed which is mainly based on a new motion profile for the specimen rotation during ion-milling. This motion profile consists of reversing partial revolutions (RPR) within a fixed sector which is centered around a direction perpendicular to the specimen heterogeneity axis. The ion-milling results obtained through this technique, as studied on a number of thin film cross-sectional TEM (XTEM) specimens, have proved to be superior to those produced via other procedures.XTEM specimens from integrated circuit (IC) devices essentially form a complex unidirectional nonhomogeneous structure. The presence of a variety of mostly lateral features at different levels along the substrate surface (consisting of conductors, semiconductors, and insulators) generally cause non-uniform results if ion-thinned conventionally.


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