An Advanced Mechanical Dimpung Technique for the Preparation of TEM Specimens

1990 ◽  
Vol 199 ◽  
Author(s):  
Paul E. Fischione ◽  
James M. Howe

ABSTRACTFor materials that are conducive to pre-thinning by mechanical techniques, a combination of dimpling and ion milling is commonly employed to produce TEM specimens. In order to minimize artifacts induced by ion milling and to provide an increased electron-beam transparent area, new instrumentation for mechanical thinning has been developed. Examples illustrating the utilization of this instrument in the preparation of cross-sectional interfaces from layered samples are discussed.

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):  
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):  
W. Brünger

Reconstructive tomography is a new technique in diagnostic radiology for imaging cross-sectional planes of the human body /1/. A collimated beam of X-rays is scanned through a thin slice of the body and the transmitted intensity is recorded by a detector giving a linear shadow graph or projection (see fig. 1). Many of these projections at different angles are used to reconstruct the body-layer, usually with the aid of a computer. The picture element size of present tomographic scanners is approximately 1.1 mm2.Micro tomography can be realized using the very fine X-ray source generated by the focused electron beam of a scanning electron microscope (see fig. 2). The translation of the X-ray source is done by a line scan of the electron beam on a polished target surface /2/. Projections at different angles are produced by rotating the object.During the registration of a single scan the electron beam is deflected in one direction only, while both deflections are operating in the display tube.


Author(s):  
C.M. Sung ◽  
M. Levinson ◽  
M. Tabasky ◽  
K. Ostreicher ◽  
B.M. Ditchek

Directionally solidified Si/TaSi2 eutectic composites for the development of electronic devices (e.g. photodiodes and field-emission cathodes) were made using a Czochralski growth technique. High quality epitaxial growth of silicon on the eutectic composite substrates requires a clean silicon substrate surface prior to the growth process. Hence a preepitaxial surface cleaning step is highly desirable. The purpose of this paper is to investigate the effect of surface cleaning methods on the epilayer/substrate interface and the characterization of silicon epilayers grown on Si/TaSi2 substrates by TEM.Wafers were cut normal to the <111> growth axis of the silicon matrix from an approximately 1 cm diameter Si/TaSi2 composite boule. Four pre-treatments were employed to remove native oxide and other contaminants: 1) No treatment, 2) HF only; 3) HC1 only; and 4) both HF and HCl. The cross-sectional specimens for TEM study were prepared by cutting the bulk sample into sheets perpendicular to the TaSi2 fiber axes. The material was then prepared in the usual manner to produce samples having a thickness of 10μm. The final step was ion milling in Ar+ until breakthrough occurred. The TEM samples were then analyzed at 120 keV using the Philips EM400T.


Author(s):  
J.Y. Lee

In the oxidation of metals and alloys, microstructural features at the atomic level play an important role in the nucleation and growth of the oxide, but little is known about the atomic mechanisms of high temperature oxidation. The present paper describes current progress on crystallographic aspects of aluminum oxidation. The 99.999% pure, polycrystalline aluminum was chemically polished and oxidized in 1 atm air at either 550°C or 600°C for times from 0.5 hr to 4 weeks. Cross-sectional specimens were prepared by forming a sandwich with epoxy, followed by mechanical polishing and then argon ion milling. High resolution images were recorded in a <110>oxide zone-axis orientation with a JE0L JEM 200CX microscope operated at 200 keV.


Author(s):  
Julia T. Luck ◽  
C. W. Boggs ◽  
S. J. Pennycook

The use of cross-sectional Transmission Electron Microscopy (TEM) has become invaluable for the characterization of the near-surface regions of semiconductors following ion-implantation and/or transient thermal processing. A fast and reliable technique is required which produces a large thin region while preserving the original sample surface. New analytical techniques, particularly the direct imaging of dopant distributions, also require good thickness uniformity. Two methods of ion milling are commonly used, and are compared below. The older method involves milling with a single gun from each side in turn, whereas a newer method uses two guns to mill from both sides simultaneously.


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.


Author(s):  
Gunnar Zimmermann ◽  
Richard Chapman

Abstract Dual beam FIBSEM systems invite the use of innovative techniques to localize IC fails both electrically and physically. For electrical localization, we present a quick and reliable in-situ FIBSEM technique to deposit probe pads with very low parasitic leakage (Ipara &lt; 4E-11A at 3V). The probe pads were Pt, deposited with ion beam assistance, on top of highly insulating SiOx, deposited with electron beam assistance. The buried plate (n-Band), p-well, wordline and bitline of a failing and a good 0.2 μm technology DRAM single cell were contacted. Both cells shared the same wordline for direct comparison of cell characteristics. Through this technique we electrically isolated the fail to a single cell by detecting leakage between the polysilicon wordline gate and the cell diffusion. For physical localization, we present a completely in-situ FIBSEM technique that combines ion milling, XeF2 staining and SEM imaging. With this technique, the electrically isolated fail was found to be a hole in the gate oxide at the bad cell.


1992 ◽  
Vol 7 (8) ◽  
pp. 2225-2229 ◽  
Author(s):  
Z.G. Li ◽  
P.F. Carcia ◽  
P.C. Donohue

The microstructure of LaB6-base thick film resistors was investigated by cross-sectional transmission electron microscopy. The specimens were prepared by a technique that polished them to a thin wedge, thus avoiding ion-milling and permitting imaging over a distance of tens of microns. The resistor microstructure contained a finely divided electrically conductive phase of TaB2 and nonconducting crystals of CaTa4O11, formed during high temperature processing of glass and LaB6 ingredients of the thick film ink. Using higher surface area ingredients virtually suppressed the formation of CaTa4O11 crystals, and the microstructure became more uniform. Resistors made with higher surface area intermediates also had better voltage withstanding properties.


1989 ◽  
Vol 147 ◽  
Author(s):  
K. S. Jones ◽  
J. Yu ◽  
P. D. Lowen ◽  
D. Kisker

AbstractTransmission electron diffraction patterns of cross-sectional TEM samples of OMVPE ZnSe on GaAs indicate the existence of the hexagonal wurtzite phase in the epitaxial layers. The orientation relationship is (0002)//(111); (1120)//(220). Etching studies indicate the phase is internal not ion milling induced. The average wurtzite particle size is 80Å-120Å. Because of interplanar spacing matches it is easily overlooked. Electrical property measurements show a high resistivity (1010ω/square) which drops by four orders of magnitude upon rapid thermal annealing between 700°C and 900 °C for 3 sec. Implantation of Li and N have little effect on the electrical transport properties. The Li is shown to have a high diffusivity, a solid solubility of ≈1016/cm3 at 800°C and getters to the ZnSeA/aAs interface.


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