Processing and characterization of lead magnesium tantalate ceramics

1997 ◽  
Vol 12 (10) ◽  
pp. 2617-2622 ◽  
Author(s):  
Mehmet A. Akbas ◽  
Peter K. Davies
Keyword(s):  
Relaxor Ferroelectrics ◽  
Dark Field ◽  
Processing Route ◽  
Chemical Ordering ◽  
Lead Magnesium ◽  
Resolution Imaging ◽  
Diffraction Patterns ◽  
Sintering Characteristics ◽  
Polar Clusters

Using a processing route that employed platinum crucibles, single phase ceramics of Pb(Mg1/3Ta2/3)O3 (PMT) relaxor ferroelectrics were prepared with densities greater than 95% of their theoretical value. The improvements in the sintering characteristics of this system that result from this route were reflected by the dielectric properties, at 182 K, which are similar to those reported for single crystal PMT. Contrast originating from nanosized polar clusters was evident in dark-field TEM images collected from the PMT ceramics at room temperature and showed little change upon cooling through the permittivity maximum. The electron diffraction patterns contained weak superlattice reflections at (h ± 1/2, k ± 1/2, l ± 1/2) that originate from a 1: 1 ordering of the B-site cations. High resolution imaging indicated that the length scale of the chemical ordering in PMT is essentially identical to niobate relaxors such as PMN, with the 1–2 nm ordered domains being surrounded by a disordered matrix.

New detection system for HAADE and holography in STEM

1992 ◽  
Vol 50 (1) ◽  
pp. 102-103
Author(s):  
Marian Mankos ◽  
Shi Yao Wang ◽  
J.K. Weiss ◽  
J.M. Cowley
Keyword(s):  
High Efficiency ◽  
Detection System ◽  
Dark Field ◽  
Light Signal ◽  
Bright Field ◽  
Transmitted Beam ◽  
Wide Range ◽  
Annular Dark Field ◽  
Resolution Imaging ◽  
Diffraction Patterns

A novel detection system has been designed and realized experimentally on the HB5 STEM instrument. Shadow images, diffraction patterns as well as high-angle annular dark field and bright field images are observed simultaneously with high efficiency using CCD and TV cameras. The microscope can be operated in a wide range of instrument modes which includes the implementation of new techniques for high resolution imaging.As shown in Fig. 1, the detection system has three triple choice stages. Diffracted beams can be collected by three P47 fast phosphor annular detectors inclined at 45 degree to the axis and having different inner and outer acceptance angles, which can be adjusted by the postspecimen lenses. The detector is observed through a window by a photomultiplier. The annular detectors have been used also for a new bright field STEM technique which utilizes the inner rim of the detectors to collect only the outermost annular part of the central beam and promises an improvement in resolution by a factor of about 1.6. Initial results show some promise (Fig. 2). The transmitted beam is then converted into a light signal in YAG and P47 detectors; optionally the central part of the beam can be detected in the EELS spectrometer. The generated light signal is reflected through a system of mirrors, exits the vacuum chamber and is collected with high efficiency by high aperture optical lenses.

Two Investigations into Grain Boundary Structure

1977 ◽  
Vol 35 ◽  
pp. 688-691
Author(s):  
P. Humble
Keyword(s):  
Grain Boundary ◽  
Dark Field ◽  
Boundary Structure ◽  
Boundary Dislocation ◽  
Bright Field ◽  
Intrinsic Structure ◽  
Weak Beam ◽  
Grain Boundary Structure ◽  
Independent Information ◽  
Diffraction Patterns

There has been sustained interest over the last few years into both the intrinsic (primary and secondary) structure of grain boundaries and the extrinsic structure e.g. the interaction of matrix dislocations with the boundary. Most of the investigations carried out by electron microscopy have involved only the use of information contained in the transmitted image (bright field, dark field, weak beam etc.). Whilst these imaging modes are appropriate to the cases of relatively coarse intrinsic or extrinsic grain boundary dislocation structures, it is apparent that in principle (and indeed in practice, e.g. (1)-(3)) the diffraction patterns from the boundary can give extra independent information about the fine scale periodic intrinsic structure of the boundary.In this paper I shall describe one investigation into each type of structure using the appropriate method of obtaining the necessary information which has been carried out recently at Tribophysics.

Zero-loss omega-filtered REM and RHEED on the new Zeiss 912

1991 ◽  
Vol 49 ◽  
pp. 616-617
Author(s):  
J.C.H. Spence ◽  
J. Mayer
Keyword(s):  
Electron Microscopy ◽  
Materials Science ◽  
Surface States ◽  
Ccd Camera ◽  
Dark Field ◽  
Ion Pump ◽  
Magnetic Imaging ◽  
Reflection Electron Microscopy ◽  
Diffraction Patterns ◽  
Large Background

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.

Formation Mechanisms for Multiply Twinned Particles During Nucleation in the Au/MICA System

1975 ◽  
Vol 33 ◽  
pp. 84-85
Author(s):  
Eal H. Lee ◽  
Helmut Poppa
Keyword(s):  
Deposition Time ◽  
High Vacuum ◽  
Dark Field ◽  
Ultra High Vacuum ◽  
Formation Mechanisms ◽  
Heat Treated ◽  
Cluster Density ◽  
Diffraction Patterns ◽  
Crystal Particle ◽  
Multiply Twinned Particles

The formation of thin films of gold on mica has been studied in ultra-high vacuum (5xl0-10 torr) . The mica substrates were heat-treated for 24 hours at 375°C, cleaved, and annealed for 15 minutes at the deposition temperature of 300°C prior to deposition. An impingement flux of 3x1013 atoms cm-2 sec-1 was used. These conditions were found to give high number densities of multiple twin particles and are based on a systematic series of nucleation experiments described elsewhere. Individual deposits of varying deposition time were made and examined by bright and dark field TEM after "cleavage preparation" of highly transparent specimens. In the early stages of growth, the films generally consist of small particles which are either single crystals or multiply twinned; a strong preference for multiply twinned particles was found whenever the particle number densities were high. Fig. 1 shows the stable cluster density ns and the variation with deposition time of multiple twin particle and single crystal particle densities, respectively. Corresponding micrographs and diffraction patterns are shown in Fig. 2.

Analysis of Dark-Field Images of Disordered Materials

1972 ◽  
Vol 30 ◽  
pp. 560-561
Author(s):  
J. M. Cowley
Keyword(s):  
Amorphous Materials ◽  
Careful Analysis ◽  
Dark Field ◽  
Minimum Diameter ◽  
Statistical Fluctuations ◽  
Bright Spots ◽  
Sufficient Detail ◽  
Random Arrangement ◽  
Diffraction Patterns ◽  
Imaging Conditions

Recently a number of authors have reported detail in dark-field images obtained from diffuse-scattering regions of electron diffraction patterns. Bright spots in images from short-range order diffuse peaks of disordered binary alloys have been interpreted as evidence for the existence of microdomains of ordered lattice or of segragated clusters of one component. Spotty contrast in dark field images of near-amorphous materials has been interpreted as evidence for the existense of microcrystals. Without a careful analysis of the imaging conditions such conclusions may be invalid. Usually the conditions of the experiment have not been specified in sufficient detail to allow evaluation of the conclusions.Elementary considerations show that even for a completely random arrangement of atoms the statistical fluctuations of density will give a spotty contrast with spots of minimum diameter determined by the dark field aperture size and other factors influencing the minimum resolvable distance under darkfield imaging conditions, including fluctuations and drift over long exposure times (resolution usually 10Å or more).

A Novel TEM Technique for Characterizing As-Grown CVD Diamond Films

1991 ◽  
Vol 49 ◽  
pp. 956-957 ◽  
Author(s):  
Z.L. Wang ◽  
J. Bentley ◽  
R.E. Clausing ◽  
L. Heatherly ◽  
L.L. Horton
Keyword(s):  
Diamond Films ◽  
Chemical Vapor ◽  
Growth Direction ◽  
Dark Field ◽  
Growth Surface ◽  
Specimen Preparation ◽  
Transmission Electron ◽  
Diffraction Patterns ◽  
First Time ◽  
Microstructural Studies

Microstructural studies by transmission electron microscopy (TEM) of diamond films grown by chemical vapor deposition (CVD) usually involve tedious specimen preparation. This process has been avoided with a technique that is described in this paper. For the first time, thick as-grown diamond films have been examined directly in a conventional TEM without thinning. With this technique, the important microstructures near the growth surface have been characterized. An as-grown diamond film was fractured on a plane containing the growth direction. It took about 5 min to prepare a sample. For TEM examination, the film was tilted about 30-45° (see Fig. 1). Microstructures of the diamond grains on the top edge of the growth face can be characterized directly by transmitted electron bright-field (BF) and dark-field (DF) images and diffraction patterns.

Characterization of frozen hydrated biological specimens by low-loss EELS

1992 ◽  
Vol 50 (2) ◽  
pp. 1572-1573
Author(s):  
Songquan Sun ◽  
Richard D. Leapman
Keyword(s):  
Water Content ◽  
Direct Method ◽  
Internal Standard ◽  
Dry Weight ◽  
Dark Field ◽  
Protein Solutions ◽  
Subcellular Compartment ◽  
Differential Shrinkage ◽  
Electron Energy Loss

Analyses of ultrathin cryosections are generally performed after freeze-drying because the presence of water renders the specimens highly susceptible to radiation damage. The water content of a subcellular compartment is an important quantity that must be known, for example, to convert the dry weight concentrations of ions to the physiologically more relevant molar concentrations. Water content can be determined indirectly from dark-field mass measurements provided that there is no differential shrinkage between compartments and that there exists a suitable internal standard. The potential advantage of a more direct method for measuring water has led us to explore the use of electron energy loss spectroscopy (EELS) for characterizing biological specimens in their frozen hydrated state.We have obtained preliminary EELS measurements from pure amorphous ice and from cryosectioned frozen protein solutions. The specimens were cryotransfered into a VG-HB501 field-emission STEM equipped with a 666 Gatan parallel-detection spectrometer and analyzed at approximately −160 C.

A New Detector System For The HB5 Stem Instrument

1985 ◽  
Vol 43 ◽  
pp. 134-135
Author(s):  
J.M. Cowley
Keyword(s):  
Dark Field ◽  
Detector System ◽  
Electron Holography ◽  
Small Specimen ◽  
Bright Field ◽  
Multiple Images ◽  
Practical Applications ◽  
Wide Range ◽  
Diffraction Patterns ◽  
Operational Modes

The HB5 STEM instrument at ASU has been modified previously to include an efficient two-dimensional detector incorporating an optical analyser device and also a digital system for the recording of multiple images. The detector system was built to explore a wide range of possibilities including in-line electron holography, the observation and recording of diffraction patterns from very small specimen regions (having diameters as small as 3Å) and the formation of both bright field and dark field images by detection of various portions of the diffraction pattern. Experience in the use of this system has shown that sane of its capabilities are unique and valuable. For other purposes it appears that, while the principles of the operational modes may be verified, the practical applications are limited by the details of the initial design.

TEM study of lanthanum aluminate

1990 ◽  
Vol 48 (4) ◽  
pp. 1060-1061
Author(s):  
C.Y. Yang ◽  
Z.R. Huang ◽  
Y.Q. Zhou ◽  
C.Z. Li ◽  
W.H. Yang ◽  
...  
Keyword(s):  
Domain Boundary ◽  
Point Group ◽  
Optical Microscope ◽  
Dark Field ◽  
Zone Axis ◽  
Superconducting Film ◽  
Ion Milling ◽  
Lanthanum Aluminate ◽  
Ring Diameter ◽  
Diffraction Patterns

Lanthanum aluminate(LaAlO3) single crystal as a substrate for high Tc superconducting film has attracted attention recently. We report here a transmission electron microscopy(TEM) study of the crystal structure and phase transformation of LaAlO3 by using Philips EM420 and EM430 microscopes. Single crystals of LaAlO3 were investigated first by optical microscope. Stripe-shaped domains of mm size are clearly seen(Fig.1a), and 90° domain boundary is also obvious. TEM specimens were prepared by mechanical grinding and polishing followed by ion-milling.Fig.lb shows μm size stripe domains of LaAlO3. Convergent beam electron diffraction patterns (CBED) from single domain were taken.Fig. 2a and Fig. 2c are [001] zone axis patterns which show a 4mm symmetry, and the (200) dark field of this zone axis gives 2mm symmetry(fig.2b). Therefore the point group of this crystal is either 4/mmm or m3m. The projection of the first order Laue zone(FOLZ) reflections on zero layer (fig. 2c) shows that the unit cell is face centered. A tetragonal unit ceil is chosen, with a=0.532nm and c=0.753nm, c being determined from the FOLZ ring diameter.

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