Electron microscopy investigations on the mineral lorándite (TlAsS2) from Allchar in Macedonia

Author(s):  
Tobias Necke ◽  
Maximilian Trapp ◽  
Stefan Lauterbach ◽  
Georg Amthauer ◽  
Hans-Joachim Kleebe

Abstract In this paper, we report on electron microscopy studies of single crystals of the natural mineral lorándite, TlAsS2. The main focus of this investigation was to address the question as to whether those lorándite crystals are chemically and structurally homogeneous, in order to be utilized as an effective neutrino detector within the lorándite experiment (LOREX) project. Apart from few secondary minerals, being present only at the surface of the lorándite samples, scanning electron microscopy (SEM) indicated homogeneous crystals. Similarly, transmission electron microscopy (TEM) imaging revealed a homogenous and undisturbed crystal structure, with the only exception of local coffee-bean contrasts; however, rarely observed. These specific contrast variations are known to be a typical strain indicator caused by a local deformation of the crystal lattice. Energy-dispersive X-ray spectroscopy (EDS) in conjunction with electron energy-loss spectroscopy (EELS) did not show any significant chemical difference when analysing regions on or off those coffee-bean features, indicating a chemically homogenous mineral. Since the presence of lattice disturbing secondary phase precipitates could be excluded by imaging and complementary chemical analysis, crystal defects such as dislocations and stacking faults or minor fluid inclusions are discussed as the probable origin of this local elastic strain. The experimental results confirm that the studied lorándite single crystals fulfil all structural and chemical requirements to be employed as the natural mineral that allows to determine solar neutrino fluxes. In addition, critical issues regarding the rather challenging sample preparation of lorándite are reported and a quantification of the maximum tolerable electron dose in the TEM is presented, since lorándite was found to be sensitive with respect to electron beam irradiation. Furthermore, the limits of EDS measurements due to peak overlapping are shown and discussed utilizing the case of Pb in lorándite. In this regard, a comparison with the Tl- and Pb-containing natural mineral hutchinsonite, TlPbAs5S9, is also included.

Author(s):  
G. G. Hembree ◽  
M. A. Otooni ◽  
J. M. Cowley

The formation of oxide structures on single crystal films of metals has been investigated using the REMEDIE system (for Reflection Electron Microscopy and Electron Diffraction at Intermediate Energies) (1). Using this instrument scanning images can be obtained with a 5 to 15keV incident electron beam by collecting either secondary or diffracted electrons from the crystal surface (2). It is particularly suited to studies of the present sort where the surface reactions are strongly related to surface morphology and crystal defects and the growth of reaction products is inhomogeneous and not adequately described in terms of a single parameter. Observation of the samples has also been made by reflection electron diffraction, reflection electron microscopy and replication techniques in a JEM-100B electron microscope.A thin single crystal film of copper, epitaxially grown on NaCl of (100) orientation, was repositioned on a large copper single crystal of (111) orientation.


Author(s):  
J. R. Heffelfinger ◽  
C. B. Carter

Transmission-electron microscopy (TEM), scanning-electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDS) were used to investigate the solid-state reaction between a thin yttria film and a (0001) α-alumina substrate. Systems containing Y2O3 (yttria) and Al2O3 (alumina) are seen in many technologically relevant applications. For example, yttria is being explored as a coating material for alumina fibers for metal-ceramic composites. The coating serves as a diffusion barrier and protects the alumina fiber from reacting with the metal matrix. With sufficient time and temperature, yttria in contact with alumina will react to form one or a combination of phases shown by the phase diagram in Figure l. Of the reaction phases, yttrium aluminum garnet (YAG) is used as a material for lasers and other optical applications. In a different application, YAG is formed as a secondary phase in the sintering of AIN. Yttria is added to AIN as a sintering aid and acts as an oxygen getter by reacting with the alumina in AIN to form YAG.


Author(s):  
J.G. Wen ◽  
K.K. Fung

Bi-based superconducting phases have been found to be members of a structural series represented by Bi2Sr2Can−1Cun−1On+4, n=1,2,3, and are referred to as 2201, 2212, 2223 phases. All these phases are incommensurate modulated structures. The super space groups are P2/b, NBbmb 2201, 2212 phases respectively. Pb-doped ceramic samples and single crystals and Y-doped single crystals have been studied by transmission electron microscopy.Modulated structures of all Bi-based superconducting phases are in b-c plane, therefore, it is the best way to determine modulated structure and c parameter in diffraction pattern. FIG. 1,2,3 show diffraction patterns of three kinds of modulations in Pb-doped ceramic samples. Energy dispersive X-ray analysis (EDAX) confirms the presence of Pb in the three modulated structures. Parameters c are 3 0.06, 38.29, 30.24Å, ie 2212, 2223, 2212 phases for FIG. 1,2,3 respectively. Their average space groups are all Bbmb.


Author(s):  
Seiji Isoda ◽  
Kimitsugu Saitoh ◽  
Sakumi Moriguchi ◽  
Takashi Kobayashi

On the observation of structures by high resolution electron microscopy, recording materials with high sensitivity and high quality is awaited, especially for the study of radiation sensitive specimens. Such recording material should be easily combined with the minimum dose system and cryoprotection method. Recently a new recording material, imaging plate, comes to be widely used in X-ray radiography and also in electron microscopy, because of its high sensitivity, high quality and the easiness in handling the images with a computer. The properties of the imaging plate in 100 to 400 kV electron microscopes were already discussed and the effectiveness was revealed.It is demanded to study the applicability of the imaging plate to high voltage electron microscopy. The quality of the imaging plate was investigated using an imaging plate system (JEOL EM-HSR100) equipped in a new Kyoto 1000kV electron microscope. In the system both the imaging plate and films can be introduced together into the camera chamber. Figure 1 shows the effect of accelerating voltage on read-out signal intensities from the imaging plate. The characteristic of commercially available imaging plates is unfortunately optimized for 100 to 200 keV electrons and then for 600 to 1000 keV electrons the signal is reduced. In the electron dose range of 10−13 to 10−10 C/cm2, the signal increases linearly with logarithm of electron dose in all acceralating volatges.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


Author(s):  
W.W. Adams ◽  
G. Price ◽  
A. Krause

It has been shown that there are numerous advantages in imaging both coated and uncoated polymers in scanning electron microscopy (SEM) at low voltages (LV) from 0.5 to 2.0 keV compared to imaging at conventional voltages of 10 to 20 keV. The disadvantages of LVSEM of degraded resolution and decreased beam current have been overcome with the new generation of field emission gun SEMs. In imaging metal coated polymers in LVSEM beam damage is reduced, contrast is improved, and charging from irregularly shaped features (which may be unevenly coated) is reduced or eliminated. Imaging uncoated polymers in LVSEM allows direct observation of the surface with little or no charging and with no alterations of surface features from the metal coating process required for higher voltage imaging. This is particularly important for high resolution (HR) studies of polymers where it is desired to image features 1 to 10 nm in size. Metal sputter coating techniques produce a 10 - 20 nm film that has its own texture which can obscure topographical features of the original polymer surface. In examining thin, uncoated insulating samples on a conducting substrate at low voltages the effect of sample-beam interactions on image formation and resolution will differ significantly from the effect at higher accelerating voltages. We discuss here sample-beam interactions in single crystals on conducting substrates at low voltages and also present the first results on HRSEM of single crystal morphologies which show some of these effects.


2012 ◽  
Vol 15 (1) ◽  
pp. 19 ◽  
Author(s):  
El-Shazly M. Duraia ◽  
G.W. Beall ◽  
Zulkhair A. Mansurov ◽  
Tatyana A. Shabanova ◽  
Ahmed E. Hannora

Elongated wire-like Zinc oxide, nanocombs and nanocrystals have been successfully synthesized on the silicon substrate from the metallic zinc as a starting material. The annealing temperature was as low as 450 ºC in argon atmosphere mixed with about 3% oxygen. Structural analysis using the X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) showed that the existence of two phases; nanowires and crystalline form. Moreover some nanoparticles aggregates were noticed to be attached in the bulk to the sides of the ZnO nanocrystals and sometimes these aggregate attached to the Zinc oxide hexagonal crystal and grow to form nanowire at different angles. Scanning electron microscopy (SEM) investigations for the zinc oxide nanostructure on the silicon substrate showed the formation of the nanocrystals in the gas flow direction and at the low energy sites over the silicon substrate. Photoluminescence (PL) measurements, performed at the room temperature, showed the existence of two basic emissions: narrow ultraviolet (UV) emission at 398 nm which attributed to the near band edge emission of the wide band gap and a very wide, more intensive, green emission at 471 nm corresponds to the crystal defects such as vacancies, interstitial sites in ZnO.


Author(s):  
K. Seshan ◽  
H.-R. Wenk

Asbestos fibre texture occurs in various mineral groups (e.g. chrysotile, crocidolite, tremolite, grunerite, tourmaline) and it has been established that at least chrysotile is carcinogenic. We are investigating various aspects of the asbestos structure, with transmission electron microscopy (TEM) (1) in order to develop methods for unequivocal asbestos identification using minute samples and also to determine defects responsible for the fibre structure in these minerals which often occur as large, we 11-developed single crystals.In order to do this, we have started by investigating clinoamphibole asbestos such as tremolite Ca2Mg5[Si8O22] (OH, F)2 and crocidolite Na2 (Mg, Al, Fe3+, Fe2+) (Si8O22) (OH, F )2 , from California localities. In crocidoli te - asbestos we observed a high density of very narrow microtwins parallel to the fibre axis [001] (Fig. 1). They are often only 50-100Å wide. Diffraction patterns display the typical twin arrangement of spots and although preliminary contrast experiments are not yet conclusive the twin plane appears to be (100).


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