Electron Microscopy Study on Zirconia and Alumina Ceramic Powders Synthesized by Microwave Plasma Pyrolysis

1992 ◽  
Vol 269 ◽  
Author(s):  
Kurt E. Sickafus ◽  
Dieter Vollath ◽  
Ravi Varma

ABSTRACTMorphology, chemistry and microstructure of zirconia and alumina based ceramic powders synthesized by microwave plasma pyrolysis were studied by transmission electron microscopy. Electron diffraction was used to determine the phases present, while conventional bright field and dark field imaging were used to characterize grain size and density variations. Materials analyzed in this study were either pure zirconia, pure alumina, or a ternary zirconia-yttria-alumina oxide. Solid spheres, hollow spheres, and fragments of hollow spheres were observed. All three modifications of zirconia were observed in the pure zirconia powder. In alumina, the predominant phase was cubic, gamma alumina. In the ternary oxide, most structures exhibited cubic zirconia diffraction patterns. Energy dispersive x-ray spectroscopy revealed chemical inhomogeneities in the ternary oxide powder.

1992 ◽  
Vol 269 ◽  
Author(s):  
Dieter Vollath ◽  
Ravi Varma ◽  
Kurt E. Sickafus

ABSTRACTPyrolytically prepared ceramic powders usually exhibit excellent homogeneity and small grain sizes. The energy efficiency of those methods for synthesis is, particularly in systems heated electrically, very poor. The situation can be improved drastically using a microwave plasma as a source of energy. This has been confirmed by the synthesis of alumina- and zirconia-based ceramic powders for which an efficiency of more than 80% was found. Aqueous solutions of nitrates of zirconium, yttrium, and aluminum were used as starting materials. Electron microscopy revealed that, through proper selection of the experimental conditions, it is possible to obtain nanocrystalline powders with cubic structure. Because of the extreme conditions during synthesis, it is possible to prepare solid solutions in systems without solubility.


2001 ◽  
Vol 16 (2) ◽  
pp. 489-502 ◽  
Author(s):  
M. A. Zurbuchen ◽  
J. Lettieri ◽  
Y. Jia ◽  
D. G. Schlom ◽  
S. K. Streiffer ◽  
...  

Portions of the same epitaxial (103)-oriented SrBi2Nb2O9 film grown on (111) SrTiO3 for which we recently reported the highest remanent polarization (Pr) ever achieved in SrBi2Nb2O9 (or SrBi2Ta2O9) films, i.e., Pr = 15.7 μC/cm2, have been characterized microstructurally by plan-view and cross-sectional transmission electron microscopy (TEM) along three orthogonal viewing directions. SrBi2Nb2O9 grows with its c axis tilted 57° from the substrate surface normal in a three-fold twin structure about the substrate [111], with the growth twins' c axes nominally aligned with the three 〈100〉 SrTiO3 directions. (103) SrBi2Nb2O9 films with and without an underlying epitaxial SrRuO3 bottom electrode have been studied. Dark-field TEM imaging over a 12 μm2 area shows no evidence of second phases (crystalline or amorphous). A high density of out-of-phase boundaries exists in the films.


Author(s):  
C. R. Hills ◽  
T. V. Nordstrom

The aging sequence in precipitation hardening Ni-2 w/o Be has been studied by transmission electron microscopy as a function of time at temperatures of 400°C, 565°C, 650°C and 750°C. The microstructural changes at different stages in the aging sequence were analyzed by a combination of electron diffraction and dark field microscopy. Prior to aging, the alloy was solution annealed at 1100°C for 6 hrs. Subsequent examination of the solution annealed material showed no evidence of either continuous or discontinuous precipitation.The precipitation sequence following aging at 400°C and 565 °C was found to be:This is analogous to that reported for the widely studied copper-beryllium1 and copper-zinc-beryllium2 systems. Precipitation commences with the nucleation of coherent platlet G. P. zones parallel to {001} matrix planes. As aging proceeds, the intermediate semicoherent γ precipitate is formed continuously from the G. P. zones.


2007 ◽  
Vol 1040 ◽  
Author(s):  
Luke Owuor Nyakiti ◽  
Jharna Chaudhuri ◽  
Ed A Kenik ◽  
Peng Lu ◽  
James H Edgar

AbstractIn the present study, the type and densities of defects in AlN crystals grown on 6H-SiC seeds by the sublimation-recombination method were assessed. The positions of the defects in AlN were first identified by defect selective etching (DSE) in molten NaOH-KOH at 400 °C for 2 minutes. Etching produced pits of three different sizes: 1.77 ìm, 2.35 ìm , and 2.86 ìm. The etch pits were either aligned together forming a sub-grain boundary or randomly distributed. The smaller etch pits were either isolated or associated with larger etch pits. After preparing cross-sections of the pits by the focused ion beam (FIB) technique, transmission electron microscopy (TEM) was performed to determine which dislocation type (edge, mixed or screw) produced a specific etch pit sizes. Preliminary TEM bright field and dark field study using different zone axes and diffraction vectors indicates an edge dislocation with a Burgers vector 1/3 is associated with the smallest etch pit size.


Author(s):  
Douglas C. Barker

A number of satisfactory methods are available for the electron microscopy of nicleic acids. These methods concentrated on fragments of nuclear, viral and mitochondrial DNA less than 50 megadaltons, on denaturation and heteroduplex mapping (Davies et al 1971) or on the interaction between proteins and DNA (Brack and Delain 1975). Less attention has been paid to the experimental criteria necessary for spreading and visualisation by dark field electron microscopy of large intact issociations of DNA. This communication will report on those criteria in relation to the ultrastructure of the (approx. 1 x 10-14g) DNA component of the kinetoplast from Trypanosomes. An extraction method has been developed to eliminate native endonucleases and nuclear contamination and to isolate the kinetoplast DNA (KDNA) as a compact network of high molecular weight. In collaboration with Dr. Ch. Brack (Basel [nstitute of Immunology), we studied the conditions necessary to prepare this KDNA Tor dark field electron microscopy using the microdrop spreading technique.


Author(s):  
J. Langmore ◽  
M. Isaacson ◽  
J. Wall ◽  
A. V. Crewe

High resolution dark field microscopy is becoming an important tool for the investigation of unstained and specifically stained biological molecules. Of primary consideration to the microscopist is the interpretation of image Intensities and the effects of radiation damage to the specimen. Ignoring inelastic scattering, the image intensity is directly related to the collected elastic scattering cross section, σɳ, which is the product of the total elastic cross section, σ and the eficiency of the microscope system at imaging these electrons, η. The number of potentially bond damaging events resulting from the beam exposure required to reduce the effect of quantum noise in the image to a given level is proportional to 1/η. We wish to compare η in three dark field systems.


Author(s):  
Akira Tanaka ◽  
David F. Harling

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.


Author(s):  
M. Jose Yacaman

In the Study of small metal particles the shape is a very Important parameter. Using electron microscopy Ino and Owaga(l) have studied the shape of twinned particles of gold. In that work electron diffraction and contrast (dark field) experiments were used to produce models of a crystal particle. In this work we report a method which can give direct information about the shape of an small metal particle in the amstrong- size range with high resolution. The diffraction pattern of a sample containing small metal particles contains in general several systematic and non- systematic reflections and a two-beam condition can not be used in practice. However a N-beam condition produces a reduced extinction distance. On the other hand if a beam is out of the bragg condition the effective extinction distance is even more reduced.


Author(s):  
J.C.H. Spence ◽  
J. Mayer

The Zeiss 912 is a new fully digital, side-entry, 120 Kv TEM/STEM instrument for materials science, fitted with an omega magnetic imaging energy filter. Pumping is by turbopump and ion pump. The magnetic imaging filter allows energy-filtered images or diffraction patterns to be recorded without scanning using efficient parallel (area) detection. The energy loss intensity distribution may also be displayed on the screen, and recorded by scanning it over the PMT supplied. If a CCD camera is fitted and suitable new software developed, “parallel ELS” recording results. For large fields of view, filtered images can be recorded much more efficiently than by Scanning Reflection Electron Microscopy, and the large background of inelastic scattering removed. We have therefore evaluated the 912 for REM and RHEED applications. Causes of streaking and resonance in RHEED patterns are being studied, and a more quantitative analysis of CBRED patterns may be possible. Dark field band-gap REM imaging of surface states may also be possible.


Author(s):  
D.P. Bazett-Jones ◽  
F.P. Ottensmeyer

It has been shown for some time that it is possible to obtain images of small unstained proteins, with a resolution of approximately 5Å using dark field electron microscopy (1,2). Applying this technique, we have observed a uniformity in size and shape of the 2-dimensional images of pure specimens of fish protamines (salmon, herring (clupeine, Y-l) and rainbow trout (Salmo irideus)). On the basis of these images, a model for the 3-dimensional structure of the fish protamines has been proposed (2).The known amino acid sequences of fish protamines show stretches of positively charged arginines, separated by regions of neutral amino acids (3). The proposed model for protamine structure (2) consists of an irregular, right-handed helix with the segments of adjacent arginines forming the loops of the coil.


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