Observations on the Structure of Ta2O5

1972 ◽  
Vol 30 ◽  
pp. 540-541
Author(s):  
P. S. Kotval ◽  
C. J. Dewit
Keyword(s):  
Electron Microscope ◽  
Structural Features ◽  
Amorphous Structure ◽  
Polished Surface ◽  
Distilled Water ◽  
Anodic Films ◽  
Amorphous Films ◽  
Beam Heating ◽  
Diffraction Patterns ◽  
Hexagonal Arrays

The structure of Ta2O5 has been described in the literature in several different crystallographic forms with varying unit cell lattice parameters. Earlier studies on films of Ta2O5 produced by anodization of tantalum have revealed structural features which are not consistent with the parameters of “bulk” Ta2O5 crystalsFilms of Ta2O5 were prepared by anodizing a well-polished surface of pure tantalum sheet. The anodic films were floated off in distilled water, collected on grids, dried and directly examined in the electron microscope. In all cases the films were found to exhibit diffraction patterns representative of an amorphous structure. Using beam heating in the electron microscope, recrystallization of the amorphous films can be accomplished as shown in Fig. 1. As suggested by earlier work, the recrystallized regions exhibit diffraction patterns which consist of hexagonal arrays of main spots together with subsidiary rows of super lattice spots which develop as recrystallization progresses (Figs. 2a and b).

Electron microscopy and diffraction studies of polyimides

1983 ◽  
Vol 41 ◽  
pp. 28-29
Author(s):  
O.C. de Hodgins ◽  
K. R. Lawless ◽  
R. Anderson
Keyword(s):  
Electron Microscopy ◽  
Electron Microscope ◽  
Structural Features ◽  
Inert Atmosphere ◽  
Polyimide Films ◽  
Resolution Electron ◽  
The Matrix ◽  
High Resolution Electron Microscope ◽  
Diffraction Patterns ◽  
Polymeric Samples

Commercial polyimide films have shown to be homogeneous on a scale of 5 to 200 nm. The observation of Skybond (SKB) 705 and PI5878 was carried out by using a Philips 400, 120 KeV STEM. The objective was to elucidate the structural features of the polymeric samples. The specimens were spun and cured at stepped temperatures in an inert atmosphere and cooled slowly for eight hours. TEM micrographs showed heterogeneities (or nodular structures) generally on a scale of 100 nm for PI5878 and approximately 40 nm for SKB 705, present in large volume fractions of both specimens. See Figures 1 and 2. It is possible that the nodulus observed may be associated with surface effects and the structure of the polymers be regarded as random amorphous arrays. Diffraction patterns of the matrix and the nodular areas showed different amorphous ring patterns in both materials. The specimens were viewed in both bright and dark fields using a high resolution electron microscope which provided magnifications of 100,000X or more on the photographic plates if desired.

Comparison of Acrylamide and Agar Gels by Freeze-Etching

1977 ◽  
Vol 35 ◽  
pp. 606-607
Author(s):  
Russell L. Steere ◽  
Eric F. Erbe
Keyword(s):  
Electron Microscope ◽  
Sodium Hydroxide ◽  
Sodium Hypochlorite ◽  
Chromic Acid ◽  
Distilled Water ◽  
Thin Sheets ◽  
Acid Cleaning ◽  
Agar Gels ◽  
Freeze Etching ◽  
Water Cut

Thin sheets of acrylamide and agar gels of different concentrations were prepared and washed in distilled water, cut into pieces of appropriate size to fit into complementary freeze-etch specimen holders (1) and rapidly frozen. Freeze-etching was accomplished in a modified Denton DFE-2 freeze-etch unit on a DV-503 vacuum evaporator.* All samples were etched for 10 min. at -98°C then re-cooled to -150°C for deposition of Pt-C shadow- and C replica-films. Acrylamide gels were dissolved in Chlorox (5.251 sodium hypochlorite) containing 101 sodium hydroxide, whereas agar gels dissolved rapidly in the commonly used chromic acid cleaning solutions. Replicas were picked up on grids with thin Foimvar support films and stereo electron micrographs were obtained with a JEM-100 B electron microscope equipped with a 60° goniometer stage.Characteristic differences between gels of different concentrations (Figs. 1 and 2) were sufficiently pronounced to convince us that the structures observed are real and not the result of freezing artifacts.

Deviations from Ideal Decagonal Symmetry in Electron Diffraction Patterns of the “Decagonal” Phase in the Al-Co-Cu Alloy System

1991 ◽  
Vol 49 ◽  
pp. 914-915
Author(s):  
Atul S. Ramani ◽  
Earle R. Ryba ◽  
Paul R. Howell
Keyword(s):  
Electron Microscope ◽  
Alloy System ◽  
Nominal Composition ◽  
Dimensional Lattice ◽  
3 Dimensional ◽  
Decagonal Phase ◽  
Cu Alloy ◽  
Transmission Electron ◽  
Lattice Periodicity ◽  
Diffraction Patterns

The “decagonal” phase in the Al-Co-Cu system of nominal composition Al65CO15Cu20 first discovered by He et al. is especially suitable as a topic of investigation since it has been claimed that it is thermodynamically stable and is reported to be periodic in the dimension perpendicular to the plane of quasiperiodic 10-fold symmetry. It can thus be expected that it is an important link between fully periodic and fully quasiperiodic phases. In the present paper, we report important findings of our transmission electron microscope (TEM) study that concern deviations from ideal decagonal symmetry of selected area diffraction patterns (SADPs) obtained from several “decagonal” phase crystals and also observation of a lattice of main reflections on the 10-fold and 2-fold SADPs that implies complete 3-dimensional lattice periodicity and the fundamentally incommensurate nature of the “decagonal” phase. We also present diffraction evidence for a new transition phase that can be classified as being one-dimensionally quasiperiodic if the lattice of main reflections is ignored.

Methods for making stereoslides and -prints, with freeze-etched olfactory epithelium as example

1984 ◽  
Vol 42 ◽  
pp. 704-705
Author(s):  
Bert Ph. M. Menco ◽  
Ido F. Menco ◽  
Frans L.T. Verdonk
Keyword(s):  
Electron Microscope ◽  
Olfactory Epithelium ◽  
Three Dimensional ◽  
Supporting Cell ◽  
Structural Features ◽  
Extensive Study ◽  
Sprague Dawley ◽  
Freezing Method ◽  
Respiratory Epithelia ◽  
Three Dimensional Presentation

Previously we presented an extensive study of the distributions of intramembranous particles of structures in apical surfaces of nasal olfactory and respiratory epithelia of the Sprague-Dawley rat. For the same structures these distributions were compared in samples which were i) chemically fixed and cryo-protected with glycerol before cryo-fixation, after excision, and ii)ultra-rapidly frozen by means of the slam-freezing method. Since a three-dimensional presentation markedly improves visualization of structural features micrographs were presented as stereopairs. Two exposures were made by tiling the sample stage of the electron microscope 6° in either direction with an eucentric goniometer. The negatives (Agfa Pan 25 Professional) were reversed with Kodak Technical Pan Film 2415 developed in D76 1:1. The prints were made from these reversed negatives. As an example tight-junctional features of an olfactory supporting cell in a region where this cell conjoined with two other cells are presented (Fig. 1).

Slow-Scan CCD Observation of Backscattering Patterns in SEM

1992 ◽  
Vol 50 (2) ◽  
pp. 1308-1309
Author(s):  
F. Ouyang ◽  
D. A. Ray ◽  
O. L. Krivanek
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Dynamic Range ◽  
High Sensitivity ◽  
Lens System ◽  
Wide Dynamic Range ◽  
Peltier Cooler ◽  
Diffraction Patterns ◽  
Scanning Electron

Electron backscattering Kikuchi diffraction patterns (BKDP) reveal useful information about the structure and orientation of crystals under study. With the well focused electron beam in a scanning electron microscope (SEM), one can use BKDP as a microanalysis tool. BKDPs have been recorded in SEMs using a phosphor screen coupled to an intensified TV camera through a lens system, and by photographic negatives. With the development of fiber-optically coupled slow scan CCD (SSC) cameras for electron beam imaging, one can take advantage of their high sensitivity and wide dynamic range for observing BKDP in SEM.We have used the Gatan 690 SSC camera to observe backscattering patterns in a JEOL JSM-840A SEM. The CCD sensor has an active area of 13.25 mm × 8.83 mm and 576 × 384 pixels. The camera head, which consists of a single crystal YAG scintillator fiber optically coupled to the CCD chip, is located inside the SEM specimen chamber. The whole camera head is cooled to about -30°C by a Peltier cooler, which permits long integration times (up to 100 seconds).

Modern TEM systems architecture

1986 ◽  
Vol 44 ◽  
pp. 602-605
Author(s):  
U. Gross ◽  
P. Hagemann
Keyword(s):  
Electron Microscope ◽  
Information Gathering ◽  
Systems Architecture ◽  
Control Functions ◽  
Transmission Electron ◽  
New Information ◽  
Comprehensive Information ◽  
Scanning Transmission ◽  
Diffraction Patterns ◽  
Analytical Equipment

By addition of analytical equipment, scanning transmission accessories and data processing equipment the basic transmission electron microscope (TEM) has evolved into a comprehensive information gathering system. This extension has led to increased complexity of the instrument as compared with the straightforward imaging microscope, since in general new information capacity has required the addition of new control hardware. The increased operational complexity is reflected in a proliferation of knobs and buttons.In the conventional electron microscope design the operating panel of the instrument has distinct control elements to alter optical conditions of the microscope column in different modes. As a consequence a multiplicity of control functions has been inevitable. Examples of this are the three pairs of focus and magnification controls needed for TEM imaging, diffraction patterns, and STEM images.

Structures and crystallization of vacuum-deposited amorphous Se and Sb films

1990 ◽  
Vol 48 (4) ◽  
pp. 140-141
Author(s):  
Makoto Shiojiri ◽  
Toshiyuki Isshiki ◽  
Tetsuya Fudaba ◽  
Yoshihiro Hirota
Keyword(s):  
Monte Carlo ◽  
Electron Microscope ◽  
Monte Carlo Method ◽  
Computer Program ◽  
Radial Distribution ◽  
Film Formation ◽  
Amorphous State ◽  
Two Dimensional ◽  
Amorphous Films ◽  
Binding Condition

In hexagonal Se crystal each atom is covalently bound to two others to form an endless spiral chain, and in Sb crystal each atom to three others to form an extended puckered sheet. Such chains and sheets may be regarded as one- and two- dimensional molecules, respectively. In this paper we investigate the structures in amorphous state of these elements and the crystallization.HRTEM and ED images of vacuum-deposited amorphous Se and Sb films were taken with a JEM-200CX electron microscope (Cs=1.2 mm). The structure models of amorphous films were constructed on a computer by Monte Carlo method. Generated atoms were subsequently deposited on a space of 2 nm×2 nm as they fulfiled the binding condition, to form a film 5 nm thick (Fig. 1a-1c). An improvement on a previous computer program has been made as to realize the actual film formation. Radial distribution fuction (RDF) curves, ED intensities and HRTEM images for the constructed structure models were calculated, and compared with the observed ones.

Automatic analysis of Kikuchi diffraction patterns

1994 ◽  
Vol 52 ◽  
pp. 900-901
Author(s):  
H. Weiland ◽  
D. P. Field
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Spatial Resolution ◽  
Relevant Information ◽  
Crystalline Materials ◽  
Large Size ◽  
Transmission Electron ◽  
New Type ◽  
Diffraction Patterns ◽  
Orientation Determination

Recent advances in the automatic indexing of backscatter Kikuchi diffraction patterns on the scanning electron microscope (SEM) has resulted in the development of a new type of microscopy. The ability to obtain statistically relevant information on the spatial distribution of crystallite orientations is giving rise to new insight into polycrystalline microstructures and their relation to materials properties. A limitation of the technique in the SEM is that the spatial resolution of the measurement is restricted by the relatively large size of the electron beam in relation to various microstructural features. Typically the spatial resolution in the SEM is limited to about half a micron or greater. Heavily worked structures exhibit microstructural features much finer than this and require resolution on the order of nanometers for accurate characterization. Transmission electron microscope (TEM) techniques offer sufficient resolution to investigate heavily worked crystalline materials.Crystal lattice orientation determination from Kikuchi diffraction patterns in the TEM (Figure 1) requires knowledge of the relative positions of at least three non-parallel Kikuchi line pairs in relation to the crystallite and the electron beam.

Quantitative Electron Microscope with imaging plate

1994 ◽  
Vol 52 ◽  
pp. 408-409
Author(s):  
D. Shindo
Keyword(s):  
Electron Microscope ◽  
Dynamic Range ◽  
Processing System ◽  
Digital Data ◽  
Imaging Plate ◽  
Crystal Thickness ◽  
X Ray Diffraction ◽  
Resolution Electron ◽  
Electron Intensity ◽  
Diffraction Patterns

Imaging plate has good properties, i.e., a wide dynamic range and good linearity for the electron intensity. Thus the digital data (2048x1536 pixels, 4096 gray levels in log scale) obtained with the imaging plate can be used for quantification in electron microscopy. By using the image processing system (PIXsysTEM) combined with a main frame (ACOS3900), quantitative analysis of electron diffraction patterns and high-resolution electron microscope (HREM) images has been successfully carried out.In the analysis of HREM images observed with the imaging plate, quantitative comparison between observed intensity and calculated intensity can be carried out by taking into account the experimental parameters such as crystal thickness and defocus value. An example of HREM images of quenched Tl2Ba2Cu1Oy (Tc = 70K) observed with the imaging plate is shown in Figs. 1(b) - (d) comparing with a structure model proposed by x-ray diffraction study of Fig. 1 (a). The image was observed with a JEM-4000EX electron microscope (Cs =1.0 mm).

A program for simulation of changes in diffraction patterns with crystal rotations

1990 ◽  
Vol 48 (1) ◽  
pp. 544-545
Author(s):  
F.C. Mijlhoff ◽  
H.W. Zandbergenl
Keyword(s):  
Electron Microscope ◽  
Reciprocal Lattice ◽  
Extensive Training ◽  
Diffraction Mode ◽  
Diffraction Patterns ◽  
Electron Microscopist

Orientation of crystals for HREM is done in diffraction mode. To do this efficiently thorough knowledge of the electron microscope and the reciprocal lattice of the investigated material is essential. With respect to the electron microscope extensive training is required to obtain the ability to tilt a crystal in the desired orientation. Familiarity with the reciprocal lattice of the investigated materials has to be obtained by tilt experiments on a relatively large number of crystals in the electron microscope. Even for experienced electron microscopists this can be very time consuming.In order to be able to practice tilt experiments without using the electron microscope, a program to simulate the electron microscope in diffraction mode was developed. The inexperienced electron microscopist may use the program to practice tilting of crystals. The experienced microscopist can use the program to familiarize with the reciprocal lattice of materials, which have not been studied by him before.

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