Lattice imaging of extended defects and related phases in polycrystalline Sr(Ba)Fe18O27 (ferrous-W)

1981 ◽  
Vol 36 (2) ◽  
pp. 260

Lattice images of the niobium oxides, structures based on the linkage of octahedral groups in continuous networks, occasionally contain features recognizable as dislocations. Since lattice imaging enables the micro-structure to be resolved in great detail, at the level of local structural organization, it is possible to determine the configuration, and also to infer the chemical composition, of dislocated areas. By treating the niobium oxide ‘block’ structures as superstructures of the ReO 3 (DO 9 ) type, the topology of dislocations can be expressed by relations between the insertion (or deletion) of one or more half-planes of cations, or of oxygen atoms only, changes in the number of crystallographic shear plane interfaces between blocks or columns, changes in (idealized) dimensions and any requisite distortion in the third dimension. Mapping the structure around a dislocation, from the lattice image, is directly equivalent to plotting the Burgers’ circuit. In this way, the precise nature of a dislocating perturbation and its implications for the local chemical composition of the crystal can be directly identified. The method is exemplified by analysis of dislocations and of related extended defects of several types, associated with twinning phenomena, semicoherent intergrowth between different ReO 3 -type superstructures and arrays building up a low angle boundary. The essential features of the analysis are not restricted to structures of the niobium oxide type, but can be extended to other types of polyhedron networks.


Germanium niobium oxide, reported as Ge02. 9Nb20 5, is inherently nonstoichiometric since it appears to be isostructural with P 20 5. 9Nb20 5. To fit this structure, there must be vacant oxygen sites or some sites accommodating ‘interstitial’ metal atoms, in relatively high concentration, and the mode of incorporating a stoichiometric excess of cations should cast some light on other niobium oxide type structures which have a reported range of composition. The structure of germanium niobium oxide has been determined by a combination of three methods: lattice imaging electron microscopy, to establish that the non-stoichiometry was not attributable to extended defects; neutron diffraction, using the powder method and profile analysis, for particular evidence about the anion sublattice and distribution of cations; and X-ray diffraction, for an ab initio refined structure. It has been proved that the anion lattice is essentially complete, and that the cation excess is accommodated by inserting cations into a set of sites, with distorted octahedral coordination, in the square tunnels formed by the junctions between columnar elements of structure. Occupation of these octahedral sites precludes the occupation of adjacent tetrahedral cation sites, proper to the type structure. In consequence, there are constraints on the way that the two kinds of tunnel site can be occupied to produce the observed stoichiometric excess of cations. The resulting model can be generalized to interpret the metal-excess composition ranges found for other niobium oxide structures.


Author(s):  
J. Y. Koo ◽  
G. Thomas

High resolution electron microscopy has been shown to give new information on defects(1) and phase transformations in solids (2,3). In a continuing program of lattice fringe imaging of alloys, we have applied this technique to the martensitic transformation in steels in order to characterize the atomic environments near twin, lath and αmartensite boundaries. This paper describes current progress in this program.Figures A and B show lattice image and conventional bright field image of the same area of a duplex Fe/2Si/0.1C steel described elsewhere(4). The microstructure consists of internally twinned martensite (M) embedded in a ferrite matrix (F). Use of the 2-beam tilted illumination technique incorporating a twin reflection produced {110} fringes across the microtwins.


Author(s):  
D. R. Clarke ◽  
G. Thomas

Grain boundaries have long held a special significance to ceramicists. In part, this has been because it has been impossible until now to actually observe the boundaries themselves. Just as important, however, is the fact that the grain boundaries and their environs have a determing influence on both the mechanisms by which powder compaction occurs during fabrication, and on the overall mechanical properties of the material. One area where the grain boundary plays a particularly important role is in the high temperature strength of hot-pressed ceramics. This is a subject of current interest as extensive efforts are being made to develop ceramics, such as silicon nitride alloys, for high temperature structural applications. In this presentation we describe how the techniques of lattice fringe imaging have made it possible to study the grain boundaries in a number of refractory ceramics, and illustrate some of the findings.


Author(s):  
W. T. Donlon ◽  
S. Shinozaki ◽  
E. M. Logothetis ◽  
W. Kaizer

Since point defects have a limited solubility in the rutile (TiO2) lattice, small deviations from stoichiometry are known to produce crystallographic shear (CS) planes which accomodate local variations in composition. The material used in this study was porous polycrystalline TiO2 (60% dense), in the form of 3mm. diameter disks, 1mm thick. Samples were mechanically polished, ion-milled by conventional techniques, and initially examined with the use of a Siemens EM102. The electron transparent thin foils were then heat-treated under controlled atmospheres of CO/CO2 and H2 and reexamined in the same manner.The “as-received” material contained mostly TiO2 grains (∼5μm diameter) which had no extended defects. Several grains however, aid exhibit a structure similar to micro-twinned grains observed in reduced rutile. Lattice fringe images (Fig. 1) of these grains reveal that the adjoining layers are not simply twin related variants of a single TinO2n-1 compound. Rather these layers (100 - 250 Å wide) are alternately comprised of stoichiometric TiO2 (rutile) and reduced TiO2 in the form of Ti8O15, with the Ti8O15 layers on either side of the TiO2 being twin related.


Author(s):  
J.Y. Laval

The exsolution of magnetite from a substituted Yttrium Iron Garnet, containing an iron excess may lead to a transitional event. This event is characterized hy the formation of a transitional zone at the center of which the magnetite nucleates (Fig.1). Since there is a contrast between the matrix and these zones and since selected area diffraction does not show any difference between those zones and the matrix in the reciprocal lattice, it is of interest to analyze the structure of the transitional zones.By using simultaneously different techniques in electron microscopy, (oscillating crystal method microdiffraction and X-ray microanalysis)one may resolve the ionic process corresponding to the transitional event and image this event subsequently by high resolution technique.


Author(s):  
T. Baird ◽  
J.R. Fryer ◽  
S.T. Galbraith

Introduction Previously we had suggested (l) that the striations observed in the pod shaped crystals of β FeOOH were an artefact of imaging in the electron microscope. Contrary to this adsorption measurements on bulk material had indicated the presence of some porosity and Gallagher (2) had proposed a model structure - based on the hollandite structure - showing the hollandite rods forming the sides of 30Å pores running the length of the crystal. Low resolution electron microscopy by Watson (3) on sectioned crystals embedded in methylmethacrylate had tended to support the existence of such pores.We have applied modern high resolution techniques to the bulk crystals and thin sections of them without confirming these earlier postulatesExperimental β FeOOH was prepared by room temperature hydrolysis of 0.01M solutions of FeCl3.6H2O, The precipitate was washed, dried in air, and embedded in Scandiplast resin. The sections were out on an LKB III Ultramicrotome to a thickness of about 500Å.


Author(s):  
S. R. Herd ◽  
P. Chaudhari

Electron diffraction and direct transmission have been used extensively to study the local atomic arrangement in amorphous solids and in particular Ge. Nearest neighbor distances had been calculated from E.D. profiles and the results have been interpreted in terms of the microcrystalline or the random network models. Direct transmission electron microscopy appears the most direct and accurate method to resolve this issue since the spacial resolution of the better instruments are of the order of 3Å. In particular the tilted beam interference method is used regularly to show fringes corresponding to 1.5 to 3Å lattice planes in crystals as resolution tests.


Author(s):  
Edward A Kenik

Segregation of solute atoms to grain boundaries, dislocations, and other extended defects can occur under thermal equilibrium or non-equilibrium conditions, such as quenching, irradiation, or precipitation. Generally, equilibrium segregation is narrow (near monolayer coverage at planar defects), whereas non-equilibrium segregation exhibits profiles of larger spatial extent, associated with diffusion of point defects or solute atoms. Analytical electron microscopy provides tools both to measure the segregation and to characterize the defect at which the segregation occurs. This is especially true of instruments that can achieve fine (<2 nm width), high current probes and as such, provide high spatial resolution analysis and characterization capability. Analysis was performed in a Philips EM400T/FEG operated in the scanning transmission mode with a probe diameter of <2 nm (FWTM). The instrument is equipped with EDAX 9100/70 energy dispersive X-ray spectrometry (EDXS) and Gatan 666 parallel detection electron energy loss spectrometry (PEELS) systems. A double-tilt, liquid-nitrogen-cooled specimen holder was employed for microanalysis in order to minimize contamination under the focussed spot.


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