Crystallographic Characterization of Dislocation Loops in Irradiated Tungsten

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):  
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):  
R. J. Lauf

Fuel particles for the High-Temperature Gas-Cooled Reactor (HTGR) contain a layer of pyrolytic silicon carbide to act as a miniature pressure vessel and primary fission product barrier. Optimization of the SiC with respect to fuel performance involves four areas of study: (a) characterization of as-deposited SiC coatings; (b) thermodynamics and kinetics of chemical reactions between SiC and fission products; (c) irradiation behavior of SiC in the absence of fission products; and (d) combined effects of irradiation and fission products. This paper reports the behavior of SiC deposited on inert microspheres and irradiated to fast neutron fluences typical of HTGR fuel at end-of-life.


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):  
H. Brigitte Krause ◽  
Yonglin Qian

A polycrystalline specimen of nominal formula EuGaAl with unknown crystal structure was investigated by various electron microscope techniques; EDS-, SED-, and CBED data were taken on a Philips 400 electron microscope operated at 100kV, HREM data on a Hitachi 9000 microscope operated at 300kV. The EDS data confirmed the composition for the bulk of the material but, in addition, revealed particles with other fractions of the elements. Only the EuGaAl particles were further investigated. The unit cell was determined to be orthorhombic with a ratio: a/b=0.969(2) , a/c=0.234(2) and b/c=0.234(2). The lattice constants are a=4.54(5)Ȧ, b=4.68Ȧ and c=19.97(20)Ȧ. Based on systematic extinctions for hkl reflections with h+l=2n+l, the unit cell was found to be b-centered. CBED patterns of the [001], [100], and [010] zone axes are shown in Fig. 1. The zone axis patterns are in agreement with the above stated data except for diffused (2m+l,2n+l,0)- reflections, not compatible with the above stated systematic absences. But these occurred only occasionally in conjunction with a complicated noncommensurate superlattice pattern.


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):  
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):  
E. Hendarto ◽  
S.L. Toh ◽  
J. Sudijono ◽  
P.K. Tan ◽  
H. Tan ◽  
...  

Abstract The scanning electron microscope (SEM) based nanoprobing technique has established itself as an indispensable failure analysis (FA) technique as technology nodes continue to shrink according to Moore's Law. Although it has its share of disadvantages, SEM-based nanoprobing is often preferred because of its advantages over other FA techniques such as focused ion beam in fault isolation. This paper presents the effectiveness of the nanoprobing technique in isolating nanoscale defects in three different cases in sub-100 nm devices: soft-fail defect caused by asymmetrical nickel silicide (NiSi) formation, hard-fail defect caused by abnormal NiSi formation leading to contact-poly short, and isolation of resistive contact in a large electrical test structure. Results suggest that the SEM based nanoprobing technique is particularly useful in identifying causes of soft-fails and plays a very important role in investigating the cause of hard-fails and improving device yield.


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