Preparation Techniques For Structural Characterization of Powdered and Composite Materials

1987 ◽  
Vol 115 ◽  
Author(s):  
Evelyn M. Ekmejian ◽  
John B. Bulko
Keyword(s):  
Zinc Oxide ◽  
Lattice Parameter Data ◽  
Chemical Properties ◽  
High Hardness ◽  
Lattice Parameter ◽  
Superior Performance ◽  
Ion Milling ◽  
Thin Sections ◽  
Preparation Techniques

ABSTRACTStandard preparation techniques such as ultramicrotomy and ion-milling are essential for obtaining accurate and detailed information about the structural and/or chemical properties of various categories of materials. The choice of a formulated matrix media has improved the preparation of thin sections of various powders ranging in degree of hardness from zinc oxide to tungsten carbide. This medium has shown superior performance when utilized in ion-milling powders and composites of high hardness such as boron carbide. This support vehicle has facilitated analysis of various geometric structures including hollow ceramic spheres. The homogeneity of chemically derived dielectric powders has been investigated by studying crystallite lattice parameter data derived from analysis of thin sections.

Improving transmission electron microscopy characterization of semiconductors by minimizing sample preparation artifacts

1992 ◽  
Vol 70 (10-11) ◽  
pp. 875-880 ◽  
Author(s):  
J. P. McCaffrey ◽  
G. I. Sproule ◽  
R. Sargent
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
Transmission Electron Microscopy Characterization ◽  
Silicon Based ◽  
Microscopy Characterization ◽  
Preparation Techniques

Techniques employed for the preparation of transmission electron microscopy (TEM) samples can introduce artifacts that obscure subtle detail in the materials being studied. Traditional semiconductor sample preparation techniques rely heavily on ion milling, which leaves amorphous layers on ion milled surfaces and some intermixing across interfaces, thus degrading the TEM images of these samples. Experimental results of the extent of this amorphization and intermixing are presented for silicon-based semiconductor samples, and methods to minimize these effects are suggested. These methods include variations in ion milling parameters that reduce the extent of the artifacts, and improvements in the small-angle cleavage technique that eliminate these artifacts completely.

Microtomy of spherical Al2O3 powders

1983 ◽  
Vol 41 ◽  
pp. 74-75
Author(s):  
E.J. Jenkins ◽  
D.S. Tucker ◽  
J.J. Hren
Keyword(s):  
Thin Film ◽  
Size Range ◽  
Particle Aggregation ◽  
Ion Milling ◽  
Thin Sections ◽  
Α Phase ◽  
Convenient Means ◽  
Van Der Waals Attraction ◽  
Negative Feature ◽  
Film Substrate

The size range of mineral and ceramic particles of one to a few microns is awkward to prepare for examination by TEM. Electrons can be transmitted through smaller particles directly and larger particles can be thinned by crushing and dispersion onto a substrate or by embedding in a film followed by ion milling. Attempts at dispersion onto a thin film substrate often result in particle aggregation by van der Waals attraction. In the present work we studied 1-10 μm diameter Al2O3 spheres which were transformed from the amprphous state to the stable α phase.After the appropriate heat treatment, the spherical powders were embedded in as high a density as practicable in a hard EPON, and then microtomed into thin sections. There are several advantages to this method. Obviously, this is a rapid and convenient means to study the microstructure of serial slices. EDS, ELS, and diffraction studies are also considerably more informative. Furthermore, confidence in sampling reliability is considerably enhanced. The major negative feature is some distortion of the microstructure inherent to the microtoming operation; however, this appears to have been surprisingly small. The details of the method and some typical results follow.

The Immuno-Electron Microscopic Localization of the Mo-Fe Protein Component of Nitrogenase in Cells of Azotobacter Vinelandii

1973 ◽  
Vol 31 ◽  
pp. 574-575
Author(s):  
J. T. Stasny ◽  
R. C. Burns ◽  
R. W. F. Hardy
Keyword(s):  
Cellular Localization ◽  
Direct Evidence ◽  
Azotobacter Vinelandii ◽  
Intracellular Localization ◽  
Protein Component ◽  
Electron Microscopic ◽  
Thin Sections ◽  
Fe Protein ◽  
Intracytoplasmic Membranes

Structure-functlon studies of biological N2-fixation have correlated the presence of the enzyme nitrogenase with increased numbers of intracytoplasmic membranes in Azotobacter. However no direct evidence has been provided for the internal cellular localization of any nitrogenase. Recent advances concerned with the crystallizatiorTand the electron microscopic characterization of the Mo-Fe protein component of Azotobacter nitrogenase, prompted the use of this purified protein to obtain antibodies (Ab) to be conjugated to electron dense markers for the intracellular localization of the protein by electron microscopy. The present study describes the use of ferritin conjugated to goat antitMo-Fe protein immunoglobulin (IgG) and the observations following its topical application to thin sections of N2-grown Azotobacter.

An Electron Microscope Study of Interdiffusion and Compound Formation in Ta-Au Thin Films

1973 ◽  
Vol 31 ◽  
pp. 32-33 ◽  
Author(s):  
T. C. Tisone ◽  
S. Lau
Keyword(s):  
Electron Microscope ◽  
Electron Microscope Study ◽  
Thermally Grown Oxide ◽  
Ion Milling ◽  
Compound Formation ◽  
Technology Application ◽  
Transmission Electron ◽  
Before And After ◽  
Au Thin Films

In a study of the properties of a Ta-Au metallization system for thin film technology application, the interdiffusion between Ta(bcc)-Au, βTa-Au and Ta2M-Au films was studied. Considered here is a discussion of the use of the transmission electron microscope(TEM) in the identification of phases formed and characterization of the film microstructures before and after annealing.The films were deposited by sputtering onto silicon wafers with 5000 Å of thermally grown oxide. The film thicknesses were 2000 Å of Ta and 2000 Å of Au. Samples for TEM observation were prepared by ultrasonically cutting 3mm disks from the wafers. The disks were first chemically etched from the silicon side using a HNO3 :HF(19:5) solution followed by ion milling to perforation of the Au side.

Characterization of carbides in M50NiL

1991 ◽  
Vol 49 ◽  
pp. 606-607
Author(s):  
L. S. Lin ◽  
K. P. Gumz ◽  
A. V. Karg ◽  
C. C. Law
Keyword(s):  
Temperature Effects ◽  
Base Composition ◽  
Lattice Parameter ◽  
Control Surface ◽  
Carbide Formation ◽  
Particle Sizes ◽  
Low Carbon ◽  
Fee Structure ◽  
Heat Treated

Carbon and temperature effects on carbide formation in the carburized zone of M50NiL are of great importance because they can be used to control surface properties of bearings. A series of homogeneous alloys (with M50NiL as base composition) containing various levels of carbon in the range of 0.15% to 1.5% (in wt.%) and heat treated at temperatures between 650°C to 1100°C were selected for characterizations. Eleven samples were chosen for carbide characterization and chemical analysis and their identifications are listed in Table 1.Five different carbides consisting of M6C, M2C, M7C3 and M23C6 were found in all eleven samples examined as shown in Table 1. M6C carbides (with least carbon) were found to be the major carbide in low carbon alloys (<0.3% C) and their amounts decreased as the carbon content increased. In sample C (0.3% C), most particles (95%) encountered were M6C carbide with a particle sizes range between 0.05 to 0.25 um. The M6C carbide are enriched in both Mo and Fe and have a fee structure with lattice parameter a=1.105 nm (Figure 1).

Cryomicroscopy of multiphase latices

1991 ◽  
Vol 49 ◽  
pp. 1060-1061
Author(s):  
O. L. Shaffer ◽  
M.S. El-Aasser ◽  
C. L. Zhao ◽  
M. A. Winnik ◽  
R. R. Shivers
Keyword(s):  
Electron Microscopy ◽  
Radiation Damage ◽  
Freeze Fracture ◽  
Particle Morphology ◽  
Second Stage ◽  
Transmission Electron ◽  
Important Approach ◽  
Carbon Coated ◽  
Preparation Techniques

Transmission electron microscopy is an important approach to the characterization of the morphology of multiphase latices. Various sample preparation techniques have been applied to multiphase latices such as OsO4, RuO4 and CsOH stains to distinguish the polymer phases or domains. Radiation damage by an electron beam of latices imbedded in ice has also been used as a technique to study particle morphology. Further studies have been developed in the use of freeze-fracture and the effect of differential radiation damage at liquid nitrogen temperatures of the latex particles embedded in ice and not embedded.Two different series of two-stage latices were prepared with (1) a poly(methyl methacrylate) (PMMA) seed and poly(styrene) (PS) second stage; (2) a PS seed and PMMA second stage. Both series have varying amounts of second-stage monomer which was added to the seed latex semicontinuously. A drop of diluted latex was placed on a 200-mesh Formvar-carbon coated copper grid.

TEM characterization of silicon epitaxial layer grown on Si-TaS2, eutectic composites

1991 ◽  
Vol 49 ◽  
pp. 802-803
Author(s):  
C.M. Sung ◽  
M. Levinson ◽  
M. Tabasky ◽  
K. Ostreicher ◽  
B.M. Ditchek
Keyword(s):  
Substrate Surface ◽  
Bulk Sample ◽  
Surface Cleaning ◽  
Native Oxide ◽  
Czochralski Growth ◽  
Ion Milling ◽  
Cross Sectional ◽  
Cleaning Methods ◽  
Field Emission Cathodes

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.

Comparison of Ion-Milling Techniques For Cross-Sectional TEM of Semiconductors

1985 ◽  
Vol 43 ◽  
pp. 166-167
Author(s):  
Julia T. Luck ◽  
C. W. Boggs ◽  
S. J. Pennycook
Keyword(s):  
Analytical Techniques ◽  
Sample Surface ◽  
Ion Milling ◽  
Cross Sectional ◽  
Reliable Technique ◽  
Near Surface ◽  
Transmission Electron ◽  
Thin Region ◽  
Transient Thermal

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.

CBED analysis of impurity distributions in AlN

1990 ◽  
Vol 48 (4) ◽  
pp. 214-215
Author(s):  
Daniel Callahan ◽  
G. Thomas
Keyword(s):  
Aluminum Nitride ◽  
Bulk Material ◽  
Strong Dependence ◽  
Lattice Parameter ◽  
Promising Technique ◽  
Nitride Ceramics ◽  
Surface Phases ◽  
Convergent Beam ◽  
Oxygen Impurities

Oxygen impurities may significantly influence the properties of nitride ceramics with a strong dependence on the microstructural distribution of the impurity. For example, amorphous oxygen-rich grain boundary phases are well-known to cause high-temperature mechanical strength degradation in silicon nitride whereas solutionized oxygen is known to decrease the thermal conductivity of aluminum nitride. Microanalytical characterization of these impurities by spectral methods in the AEM is complicated by reactions which form oxygen-rich surface phases not representative of the bulk material. Furthermore, the impurity concentrations found in higher quality ceramics may be too low to measure by EDS or PEELS. Consequently an alternate method for the characterization of impurities in these ceramics has been investigated.Convergent beam electron diffraction (CBED) is a promising technique for the study of impurity distributions in aluminum nitride ceramics. Oxygen is known to enter into stoichiometric solutions with AIN with a consequent decrease in lattice parameter.

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