Techniques for Transmission Electron Microscopy of Fiber-Matrix Interfaces in Aluminum Alloy-Boron Composites by Ion Erosio

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.

2018 ◽  
Vol 66 ◽  
pp. 151-165
Author(s):  
Morten Leth Hjuler ◽  
Vidar Folke Hansen ◽  
Ida Lykke Fabricius

Scanning and transmission electron microscopy (SEM and TEM) are capable of characterising the morphology and structure of sub-micron size substances attached to chalk particle surfaces. Some characteristics, however, may originate from sample preparation or reflect interaction between sample and the electron beam. Misinterpretation of surface features may lead to wrong conclusions regarding grain surface properties and cementation level and thus to erroneous characterisation of hydrocarbon reservoirs with respect to e.g. wettability, mechanical strength and maximum burial depth. In SEM, conductive coatings may mask surface details or generate artificial ornamentations, and carbon adhesive discs may cause the chalk surface to be covered with a thin carbon film. Electron beam acceleration voltage controls the degree of detail revealed by the electron beam, but in SEM a high electron beam acceleration voltage may provoke bending or curling of ultrathin particles. Recent organic filaments may be confused with clay flakes, and authigenic non-carbonate minerals may have formed in the pore fluid and settled during fluid removal. In TEM, the high acceleration voltage may cause beam damage to calcite and transform the outermost atomic layers into Ca oxide. Thin graphite membranes observed by TEM may be contamination from the carbon film supporting the sample, and overlapping chalk particles in samples formed by drying of a suspension may give the impression of being cemented together. In TEM residual adhesive from the ion-milling process can be confused with cementation features.


Author(s):  
R.R. Russell

Transmission electron microscopy of metallic/intermetallic composite materials is most challenging since the microscopist typically has great difficulty preparing specimens with uniform electron thin areas in adjacent phases. The application of ion milling for thinning foils from such materials has been quite effective. Although composite specimens prepared by ion milling have yielded much microstructural information, this technique has some inherent drawbacks such as the possible generation of ion damage near sample surfaces.


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):  
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.


Author(s):  
R. J. Lauf ◽  
H. Keating

The preparation of fragmented or particulate ceramic materials for transmission electron microscopy (TEM) examination has traditionally been difficult, particularly if a durable, permanent specimen is desired. Furthermore, most established methods for dealing with micron- and submicron-sized samples (e.g., dispersion in plastic films) do not permit selection of orientations or ion thinning. A technique has been developed that is useful for a variety of materials, permits the selection of specimen orientation, is compatible with ion milling requirements, and produces a durable specimen that can be reexamined later if necessary.


1997 ◽  
Vol 3 (S2) ◽  
pp. 413-414
Author(s):  
E.M. Hunt ◽  
J.M. Hampikian ◽  
N.D. Evans

Ion implantation can be used to alter the optical response of insulators through the formation of embedded nano-sized particles. Single crystal alumina has been implanted at ambient temperature with 50 keV Ca+ to a fluence of 5 x 1016 ions/cm2. Ion channeling, Knoop microhardness measurements, and transmission electron microscopy (TEM) indicate that the alumina surface layer was amorphized by the implant. TEM also revealed nano-sized crystals ≈7 - 8 nm in diameter as seen in Figure 1. These nanocrystals are randomly oriented, and exhibit a face-centered cubic structure (FCC) with a lattice parameter of 0.409 nm ± 0.002 nm. The similarity between this crystallography and that of pure aluminum (which is FCC with a lattice parameter of 0.404 nm) suggests that they are metallic aluminum nanocrystals with a slightly dilated lattice parameter, possibly due to the incorporation of a small amount of calcium.Energy-filtered transmission electron microscopy (EFTEM) provides an avenue by which to confirm the metallic nature of the aluminum involved in the nanocrystals.


2015 ◽  
Author(s):  
Ludmila L. Meisner ◽  
Alexey A. Neiman ◽  
Alexander I. Lotkov ◽  
Nikolai N. Koval ◽  
Viktor O. Semin ◽  
...  

1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky

AbstractThe demand for increasingly higher performance semiconductor products has stimulated the semiconductor industry to respond by producing devices with increasingly complex circuitry, more transistors in less space, more layers of metal, dielectric and interconnects, more interfaces, and a manufacturing process with nearly 1,000 steps. As all device features are shrunk in the quest for higher performance, the role of Transmission Electron Microscopy as a characterization tool takes on a continually increasing importance over older, lower-resolution characterization tools, such as SEM. The Ångstrom scale imaging resolution and nanometer scale chemical analysis and diffraction resolution provided by modem TEM's are particularly well suited for solving materials problems encountered during research, development, production engineering, reliability testing, and failure analysis. A critical enabling technology for the application of TEM to semiconductor based products as the feature size shrinks below a quarter micron is advances in specimen preparation. The traditional 1,000Å thick specimen will be unsatisfactory in a growing number of applications. It can be shown using a simple geometrical model, that the thickness of TEM specimens must shrink as the square root of the feature size reduction. Moreover, the center-targeting of these specimens must improve so that the centertargeting error shrinks linearly with the feature size reduction. To meet these challenges, control of the specimen preparation process will require a new generation of polishing and ion milling tools that make use of high resolution imaging to control the ion milling process. In addition, as the TEM specimen thickness shrinks, the thickness of surface amorphization produced must also be reduced. Gallium focused ion beam systems can produce hundreds of Ångstroms of amorphised surface silicon, an amount which can consume an entire thin specimen. This limitation to FIB milling requires a method of removal of amorphised material that leaves no artifact in the remaining material.


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