Amorphization at the Metal-Ceramic Interface in Nb – Al2O3 Composite Through Extensive Interphase Diffusion

1992 ◽  
Vol 271 ◽  
Author(s):  
Abhijit Ray ◽  
Shyam K. Samanta
Keyword(s):  
Electron Microscopy ◽  
Amorphous Phase ◽  
Impurity Content ◽  
Interfacial Region ◽  
Oxygen Impurity ◽  
High Concentration ◽  
Electron Microscopic ◽  
Ceramic Phase ◽  
Ceramic Particles ◽  
Metal Ceramic

ABSTRACTA novel, low temperature and pressureless bonding technique has been developed to fabricate Al2O3 coated Nb composite. The nature of the interface bond has been characterized by extensive electron microscopic investigation, and a phenomenological model has been developed to explain the mechanism of bond formation. In the present technique a suspension (in distilled water) of fine Al2O3 powder (mean particle size of 0.2μm) was applied on polished and cleaned Nb blocks. The coatings were air dried and the coated metals were heat treated at 1100°C to achieve bonding between the ceramic and the metal. The process was carried out in an argon atmosphere. To reduce the oxygen impurity content in argon, the gas was passed over Mg turnings at 300°C before its entry into the bonding apparatus. Control of oxygen impurity in the bonding atmosphere in conjunction with the use of fine ceramic particles led to enhancement of interfacial diffusion. Scanning electron microscopy of the bonded specimens showed a consolidated layer in the ceramic phase close to the metal-ceramic interface. Transmission electron microscopy of the metal-ceramic interfacial region rOevealed a distribution of Al2O3 particles in an amorphous phase containing varying amount of Al, Nb, and 0. Prior treatment with Mg was to reduce the oxygen impurity content below the equlibrium oxygen partial pressure (at 1100°C) of Al2O3. This would result in loss of oxygen from the surface of the ceramic particles. Thus a region, with high concentration of 0= vacancy would form along the surfaces of the particles. As a result of excessive oxygen depletion, further continuation of this process would lead to degeneration of the crystal structure of the regions along the surfaces of the Al2O3 particles. These regions along the Al2O3 particle surfaces may then act as easy diffusion paths for Nb. Extensive diffusion of the metal into the ceramic phase along these paths would lead to the formation of an amorphous phase along the ceramic particle surfaces. Eventually, this phase will occupy the voids in between the ceramic particles, that are close to the metal-ceramic interface, and thus bond them together with the metal.

Structural Instability of the Ceramic Coating in a Metal-Ceramic Composite Induced Through Control of Chemistry of the Bonding Atmosphere

1992 ◽  
Vol 280 ◽  
Author(s):  
Abhijit Ray
Keyword(s):  
Amorphous Phase ◽  
Bonding Temperature ◽  
Structural Instability ◽  
Processing Technique ◽  
High Concentration ◽  
Ceramic Phase ◽  
Enhanced Diffusion ◽  
Transmission Electron ◽  
Metal Ceramic ◽  
Novel Processing

ABSTRACTA novel processing technique has been developed to coat Al2O3 on Nb in an argon atmosphere with very low O2 content. It has been proposed1 that the low O2 content helped to increase the defect concentration in the ceramic phase resulting in an enhanced diffusion of Nb into Al2O3 at the metal-ceramic interface at a relatively low bonding temperature. A mathematical model has been developed1 to understand the effect of purified bonding atmosphere on interfacial diffusion. While diffraction studies in the transmission electron microscope revealed1 extensive amorphization at the metal-ceramic interface, EDX analysis showed1 that the interfacial amorphous phase has a very high concentration of O. Additionally, this phase is found to contain Al and Nb. The interfacial phase is formed due to the diffusion of Nb into the ceramic phase. The paradoxical phenomenon of O enrichment of the interfacial amorphous phase in a low O2 containing bonding atmosphere is due to the loss of gaseous oxides of Al from this phase. These oxides have relatively less proportion of O compared to Al2O3. Continuous loss of such oxides from the amorphous phase to the gaseous phase will, therefore, result in an O to Al ratio (in the amorphous phase) far exceeding that in Al2O3 (3:2).

scholarly journals Creation of Ni-B/Ni-P electroless coating on the WC particles without surface activator

2018 ◽  
Vol 23 (4) ◽  
pp. 347-352
Author(s):  
Ali Mahtab ◽  
Kamran Amini ◽  
Nader Mohammadian ◽  
Syed Amirhosein Emami ◽  
Mohammad Hosein Bina
Keyword(s):  
Electron Microscopy ◽  
Surface Preparation ◽  
Electroless Coating ◽  
Ceramic Particles ◽  
X Ray ◽  
Coating Morphology ◽  
Metal Ceramic ◽  
Coating Formation ◽  
Electroless Ni ◽  
Scanning Electron

One of the methods for improving metal-ceramic interface and suppression of agglomeration is the formation of a monolayer electroless coating on the particles. Investigations indicated that Ni-B monolayers should be first formed to develop in the next process an electroless Ni–P coating with the morphology of cauliflower. It was possible to produce a Ni-B layer on WC particles when a bath was heated at a temperature of 95 °C by using sodium borohydride and an appropriate stabilizer. Following this process, the Ni–P electroless coating was deposited on WC particles at 85 °C. In this way, two layers of electroless coating of Ni–B/Ni–P on the WC ceramic particles without using the surface activator were produced successfully. The coating morphology and surface analysis were performed by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The results showed that only the degreasing with acetone as a surface preparation of ceramic particles is sufficient to make a Ni–P or Ni–B coating. Electroless Ni–B coating with appropriate adhesion to the surface produces an acceptable surface for the electroless Ni – P coating formation.

Localization of immunolabels by electron microscopy and image averaging

1983 ◽  
Vol 41 ◽  
pp. 282-283
Author(s):  
J. Frank ◽  
P.-Y. Sizaret ◽  
A. Verschoor ◽  
J. Lamy
Keyword(s):  
Electron Microscopy ◽  
Single Particle ◽  
Attachment Site ◽  
Uranyl Acetate ◽  
Limulus Polyphemus ◽  
Resolution Limit ◽  
Electron Microscopic ◽  
Image Averaging ◽  
Top View ◽  
Better Than

The accuracy with which the attachment site of immunolabels bound to macromolecules may be localized in electron microscopic images can be considerably improved by using single particle averaging. The example studied in this work showed that the accuracy may be better than the resolution limit imposed by negative staining (∽2nm).The structure used for this demonstration was a halfmolecule of Limulus polyphemus (LP) hemocyanin, consisting of 24 subunits grouped into four hexamers. The top view of this structure was previously studied by image averaging and correspondence analysis. It was found to vary according to the flip or flop position of the molecule, and to the stain imbalance between diagonally opposed hexamers (“rocking effect”). These findings have recently been incorporated into a model of the full 8 × 6 molecule.LP hemocyanin contains eight different polypeptides, and antibodies specific for one, LP II, were used. Uranyl acetate was used as stain. A total of 58 molecule images (29 unlabelled, 29 labelled with antl-LPII Fab) showing the top view were digitized in the microdensitometer with a sampling distance of 50μ corresponding to 6.25nm.

Immunocytochemistry. A Review of Methodology for Electron Microscopic Applicaiton

1974 ◽  
Vol 32 ◽  
pp. 328-329
Author(s):  
Joseph E. Mazurkiewicz
Keyword(s):  
Electron Microscopy ◽  
Light Microscopy ◽  
Ultrastructural Level ◽  
Electron Microscopic ◽  
Biological Interest ◽  
Investigative Approach ◽  
Immunologic Activity ◽  
Dense Label

Immunocytochemistry is a powerful investigative approach in which one of the most exacting examples of specificity, that of the reaction of an antibody with its antigen, isused to localize tissue and cell specific molecules in situ. Following the introduction of fluorescent labeled antibodies in T950, a large number of molecules of biological interest had been studied with light microscopy, especially antigens involved in the pathogenesis of some diseases. However, with advances in electron microscopy, newer methods were needed which could reveal these reactions at the ultrastructural level. An electron dense label that could be coupled to an antibody without the loss of immunologic activity was desired.

An Electron Microscopic Study of an Avian Reovirus that Causes Arthritis

1971 ◽  
Vol 29 ◽  
pp. 254-255
Author(s):  
E, R. Walker ◽  
N. O. Olson ◽  
M. H. Friedman
Keyword(s):  
Electron Microscopy ◽  
Viral Genome ◽  
Inner Core ◽  
Avian Reovirus ◽  
Electron Microscopic ◽  
Outer Coat ◽  
Acid Type ◽  
Chicken Eggs ◽  
Icosahedral Particle ◽  
Mature Virus

An unidentified virus, responsible for an arthritic-like condition in chickens was studied by electron microscopy and other methods of viral investigation. It was characterized in chorio-allantoic membrane (CAM) lesions of embryonating chicken eggs and in tissue culture as to: 1) particle size; 2) structure; 3) mode of replication in the cell; and 4) nucleic acid type.The inoculated virus, coated and uncoated, is first seen in lysosomal-like inclusions near the nucleus; the virions appear to be uncoated in these electron dense inclusions (Figure 1), Although transfer of the viral genome from these inclusions is not observable, replicating virus and mature virus crystals are seen in the cytoplasm subsequent to the uncoating of the virions.The crystals are formed in association with a mass of fibrils 50 to 80 angstroms in diameter and a ribosome-studded structure that appears to be granular endoplasmic reticulum adapted to virus replication (Figure 2). The mature virion (Figure 3) is an icosahedral particle approximately 75 millimicrons in diameter. The inner core is 45 millimicrons, the outer coat 15 millimicrons, and the virion has no envelope.

A Comparative Study of Fractographic Replicas

1974 ◽  
Vol 32 ◽  
pp. 566-567
Author(s):  
Loren Anderson ◽  
Pat Pizzo ◽  
Glen Haydon
Keyword(s):  
Electron Microscopy ◽  
Electron Microscopic Examination ◽  
Direct Examination ◽  
Electron Microscopic ◽  
Reliable Technique ◽  
Service Failures ◽  
Transmission Electron ◽  
Mode Of Failure ◽  
Scanning Electron Microscopic ◽  
Scanning Electron

Transmission electron microscopy of replicas has long been used to study the fracture surfaces of components which fail in service. Recently, the scanning electron microscope (SEM) has gained popularity because it allows direct examination of the fracture surface. However, the somewhat lower resolution of the SEM coupled with a restriction on the sample size has served to limit the use of this instrument in investigating in-service failures. It is the intent of this paper to show that scanning electron microscopic examination of conventional negative replicas can be a convenient and reliable technique for determining mode of failure.

Electron Microscopic Observation of the Longitudinal Organization of Poly (p-Phenylene Terephthalamide) Fibers

1982 ◽  
Vol 40 ◽  
pp. 680-681
Author(s):  
Li Li-Sheng ◽  
L.F. Allard ◽  
W.C. Bigelow
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Scanning Electron Microscopy ◽  
Microscopic Observation ◽  
Electron Microscopic Observation ◽  
Electron Microscopic ◽  
Aromatic Polyamides ◽  
Radial Arrangement ◽  
Scanning Electron ◽  
Better Than

The aromatic polyamides form a class of fibers having mechanical properties which are much better than those of aliphatic polyamides. Currently, the accepted morphology of these fibers as proposed by M.G. Dobb, et al. is a radial arrangement of pleated sheets, with the plane of the pleats parallel to the axis of the fiber. We have recently obtained evidence which supports a different morphology of this type of fiber, using ultramicrotomy and ion-thinning techniques to prepare specimens for transmission and scanning electron microscopy.

Electron Microscopic Detection and Characterization of Nonhuman Primate Enteric Viruses

1982 ◽  
Vol 40 ◽  
pp. 306-307
Author(s):  
G. C. Smith ◽  
R. L. Heberling ◽  
S. S. Kalter
Keyword(s):  
Electron Microscopy ◽  
Animal Model ◽  
Nonhuman Primate ◽  
Clinical Condition ◽  
Intestinal Tract ◽  
Enteric Viruses ◽  
Electron Microscopic ◽  
Microscopic Detection

A number of viral agents are recognized as and suspected of causing the clinical condition “gastroenteritis.” In our attempts to establish an animal model for studies of this entity, we have been examining the nonhuman primate to ascertain what viruses may be found in the intestinal tract of “normal” animals as well as animals with diarrhea. Several virus types including coronavirus, adenovirus, herpesvirus, and picornavirus (Table I) were detected in our colony; however, rotavirus, astrovirus, and calicivirus have not yet been observed. Fecal specimens were prepared for electron microscopy by procedures reported previously.

A Scanning Electron Microscopic Study of the Uriniferous Tubules

1973 ◽  
Vol 31 ◽  
pp. 622-623
Author(s):  
Peter M. Andrews
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Renal Glomerulus ◽  
Electron Microscopic ◽  
Vascular Perfusion ◽  
Scanning Electron Microscopic Study ◽  
Scanning Electron Microscopic ◽  
Collecting Tubules ◽  
Bowman's Capsule ◽  
Scanning Electron

Although there have been a number of recent scanning electron microscopic reports on the renal glomerulus, the advantages of scanning electron microscopy have not yet been applied to a systematic study of the uriniferous tubules. In the present investigation, scanning electron microscopy was used to study the ultrastructural morphology of the proximal, distal, thin loop, and collecting tubules. Material for observation was taken from rat kidneys which were fixed by vascular perfusion, sectioned by either cutting or fracturing technigues, and critically point dried.The brush border characterising proximal tubules is first detected on the luminal surface of Bowman's capsule adjacent to the urinary pole orifice. In this region one frequently finds irregular microvilli characterized by broad and flattened bases with occasional bulbous structures protruding from their surfaces.

Studies of Circular DNA Using a New Electron Microscopic Technique

1973 ◽  
Vol 31 ◽  
pp. 596-597
Author(s):  
C. N. Gordon
Keyword(s):  
Electron Microscopy ◽  
Aqueous Salt Solution ◽  
Contour Length ◽  
Cleavage Surface ◽  
Mica Substrate ◽  
Electron Microscopic ◽  
Replica Technique ◽  
Circular Dna ◽  
Transmission Electron ◽  
Electron Microscopic Technique

Gordon and Kleinschmidt have described a new preparative technique for visualizing DNA by electron microscopy. This procedure, which is a modification of Hall's “mica substrate technique”, consists of the following steps: (a) K+ ions on the cleavage surface of native mica are exchanged for Al3+ ions by ion exchange. (b) The mica, with Al3+ in the exchange sites on the surface, is placed in a dilute aqueous salt solution of DNA for several minutes; during this period DNA becomes adsorbed on the surface. (c) The mica with adsorbed DNA is removed from the DNA solution, rinsed, dried and visualized for transmission electron microscopy by Hall's platinum pre-shadow replica technique.In previous studies of circular DNA by this technique, most of the molecules seen were either broken to linears or extensively tangled; in general, it was not possible to obtain suitably large samples of open extended molecules for contour length measurements.

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