The observation of edge dislocation loops by high resolution lattice imaging

Author(s):  
D.G. Howitt ◽  
T.E. Mitchell

IntroductionThe characterization of small defects by diffraction contrast methods in the electron microscope becomes uncertain when the image widths approach the dimensions of the defect. In the case of small defect aggretates, it becomes difficult not only to distinguish between interstitial and vacancy character but also between volume and planar defects.These small defect aggregates, or rather the disturbances that they produce, can also be investigated by lattice imaging where the interference of two or more beams, whose phases have been disturbed by the defect, produces an image. The images obtained in this way, although not a one-to-one mapping of the atomic arrangement, do bear an unique relationship to it; however, this uniqueness is lost in an electron micrograph since the phase relationships are not recorded. The image interpretation therefore relies upon the effect that the phase relationships have on the image intensity being sufficient to distinguish between likely candidates for the atomic distribution, since the image intensities from this type of microscopy are not in general straightforward to predict.

Author(s):  
Robert C. Rau

Previous work has shown that post-irradiation annealing, at temperatures near 1100°C, produces resolvable dislocation loops in tungsten irradiated to fast (E > 1 MeV) neutron fluences of about 4 x 1019 n/cm2 or greater. To crystallographically characterize these loops, tilting experiments were carried out in the electron microscope on a polycrystalline specimen which had been irradiated to 1.5 × 1021 n/cm2 at reactor ambient temperature (∼ 70°C), and subseouently annealed for 315 hours at 1100°C. This treatment produced large loops averaging 1000 Å in diameter, as shown in the micrographs of Fig. 1. The orientation of this grain was near (001), and tilting was carried out about axes near [100], [10] and [110].


Author(s):  
Mitsuo Ohtsuki ◽  
Michael Sogard

Structural investigations of biological macromolecules commonly employ CTEM with negative staining techniques. Difficulties in valid image interpretation arise, however, due to problems such as variability in thickness and degree of penetration of the staining agent, noise from the supporting film, and artifacts from defocus phase contrast effects. In order to determine the effects of these variables on biological structure, as seen by the electron microscope, negative stained macromolecules of high density lipoprotein-3 (HDL3) from human serum were analyzed with both CTEM and STEM, and results were then compared with CTEM micrographs of freeze-etched HDL3. In addition, we altered the structure of this molecule by digesting away its phospholipid component with phospholipase A2 and look for consistent changes in structure.


Author(s):  
R. F. Schneidmiller ◽  
W. F. Thrower ◽  
C. Ang

Solid state materials in the form of thin films have found increasing structural and electronic applications. Among the multitude of thin film deposition techniques, the radio frequency induced plasma sputtering has gained considerable utilization in recent years through advances in equipment design and process improvement, as well as the discovery of the versatility of the process to control film properties. In our laboratory we have used the scanning electron microscope extensively in the direct and indirect characterization of sputtered films for correlation with their physical and electrical properties.Scanning electron microscopy is a powerful tool for the examination of surfaces of solids and for the failure analysis of structural components and microelectronic devices.


Author(s):  
T. C. Tisone ◽  
S. Lau

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.


Author(s):  
Ruchama Baum ◽  
J.T. Seto

The ribonucleic acid (RNA) of paramyxoviruses has been characterized by biochemical and physiochemical methods. However, paramyxovirus RNA molecules have not been studied by electron microscopy. The molecular weights of these single-stranded viral RNA molecules are not known as yet. Since electron microscopy has been found to be useful for the characterization of single-stranded RNA, this investigation was initiated to examine the morphology and length measurements of paramyxovirus RNA's.Sendai virus Z strain and Newcastle disease virus (NDV), Milano strain, were used. For these studies it was necessary to develop a method of extracting RNA molecules from purified virus particles. Highly purified Sendai virus was treated with pronase (300 μg/ml) at 37°C for 30 minutes and the RNA extracted by the sodium dodecyl sulfate (SDS)-phenol procedure.


Author(s):  
George Guthrie ◽  
David Veblen

The nature of a geologic fluid can often be inferred from fluid-filled cavities (generally <100 μm in size) that are trapped during the growth of a mineral. A variety of techniques enables the fluids and daughter crystals (any solid precipitated from the trapped fluid) to be identified from cavities greater than a few micrometers. Many minerals, however, contain fluid inclusions smaller than a micrometer. Though inclusions this small are difficult or impossible to study by conventional techniques, they are ideally suited for study by analytical/ transmission electron microscopy (A/TEM) and electron diffraction. We have used this technique to study fluid inclusions and daughter crystals in diamond and feldspar.Inclusion-rich samples of diamond and feldspar were ion-thinned to electron transparency and examined with a Philips 420T electron microscope (120 keV) equipped with an EDAX beryllium-windowed energy dispersive spectrometer. Thin edges of the sample were perforated in areas that appeared in light microscopy to be populated densely with inclusions. In a few cases, the perforations were bound polygonal sides to which crystals (structurally and compositionally different from the host mineral) were attached (Figure 1).


Author(s):  
A. Carlsson ◽  
J.-O. Malm ◽  
A. Gustafsson

In this study a quantum well/quantum wire (QW/QWR) structure grown on a grating of V-grooves has been characterized by a technique related to chemical lattice imaging. This technique makes it possible to extract quantitative information from high resolution images.The QW/QWR structure was grown on a GaAs substrate patterned with a grating of V-grooves. The growth rate was approximately three monolayers per second without growth interruption at the interfaces. On this substrate a barrier of nominally Al0.35 Ga0.65 As was deposited to a thickness of approximately 300 nm using metalorganic vapour phase epitaxy . On top of the Al0.35Ga0.65As barrier a 3.5 nm GaAs quantum well was deposited and to conclude the structure an additional approximate 300 nm Al0.35Ga0.65 As was deposited. The GaAs QW deposited in this manner turns out to be significantly thicker at the bottom of the grooves giving a QWR running along the grooves. During the growth of the barriers an approximately 30 nm wide Ga-rich region is formed at the bottom of the grooves giving a Ga-rich stripe extending from the bottom of each groove to the surface.


Author(s):  
R. Gotthardt ◽  
A. Horsewell ◽  
F. Paschoud ◽  
S. Proennecke ◽  
M. Victoria

Fusion reactor materials will be damaged by an intense field of energetic neutrons. There is no neutron source of sufficient intensity at these energies available at present, so the material properties are being correlated with those obtained in irradiation with other irradiation sorces. Irradiation with 600 MeV protons produces both displacement damage and impurities due to nuclear reactions. Helium and hydrogen are produced as gaseous impurities. Other metallic impurities are also created . The main elements of the microstructure observed after irradiation in the PIREX facility, are described in the following paragraphs.A. Defect clusters at low irradiation doses: In specimens irradiated to very low doses (1021-1024 protons.m-2), so that there is no superimposition of contrast, small defect clusters have been observed by the weak beam technique. Detailed analysis of the visible contrast (>0.5 nm diameter) revealed the presence of stacking fault tetrahedra, dislocation loops and a certain number of unidentified clusters . Typical results in Cu and Au are shown in Fig. 1.


Author(s):  
L. J. Sykes ◽  
J. J. Hren

In electron microscope studies of crystalline solids there is a broad class of very small objects which are imaged primarily by strain contrast. Typical examples include: dislocation loops, precipitates, stacking fault tetrahedra and voids. Such objects are very difficult to identify and measure because of the sensitivity of their image to a host of variables and a similarity in their images. A number of attempts have been made to publish contrast rules to help the microscopist sort out certain subclasses of such defects. For example, Ashby and Brown (1963) described semi-quantitative rules to understand small precipitates. Eyre et al. (1979) published a catalog of images for BCC dislocation loops. Katerbau (1976) described an analytical expression to help understand contrast from small defects. There are other publications as well.


Author(s):  
J. E. O'Neal ◽  
S. M. L. Sastry ◽  
J. W. Davis

The radiation-induced defect structure and nonequilibrium phase precipitation were studied in T1-6A1-4V (an alpha-beta titanium alloy), irradiated at 450 ± 30°C in row VII of the EBR-II to a fluence of 3.0 × 1021 neutrons/cm2 (En > 0.1 MeV). The Irradiation-induced defect microstructures were examined using bright-field, conventional dark-field, and weak-beam dark-field techniques. The nature of dislocations and dislocation loops was determined by standard-contrast experiments under two-beam conditions, and the small defect clusters were identified using the line-of-contrast criterion and black-white vector orientation criterion.


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