HREM Studies of Some Phases in the ZrO2-Nb2O5 System

Author(s):  
Margareta Sundberg ◽  
Bengt-Olov Marinder

High resolution electron microscopy and x ray powder diffraction techniques were used to study samples of various compositions in the Nb2O5-rich part of the ZrO2-Nb2O5 system at 1500°C. A large number of fragments were also characterized by electron diffraction in combination with EDS analysis. Some HREM results concerning block structures formed in the above region have previously been reported.The x ray powder pattern of a ZrO2.9Nb2O5 sample indicated a phase isotypic with T-Nb2O5. The micrograph in Fig. 1, of a thin crystal fragment from that sample, illustrates a phase related to the UVO5 (m=2) structure type. The electron diffraction patterns showed an ordered commensurate phase (m=8) with unit cell dimensions similar to those reported for T-Nb2O5 and Ta30W2O81. The structure models of these two compounds are rather similar and differ mainly in the oxygen content.

2001 ◽  
Vol 16 (1) ◽  
pp. 101-107 ◽  
Author(s):  
Takeo Oku ◽  
Jan-Olov Bovin ◽  
Iwami Higashi ◽  
Takaho Tanaka ◽  
Yoshio Ishizawa

Atomic positions for Y atoms were determined by using high-resolution electron microscopy and electron diffraction. A slow-scan charge-coupled device camera which had high linearity and electron sensitivity was used to record high-resolution images and electron diffraction patterns digitally. Crystallographic image processing was applied for image analysis, which provided more accurate, averaged Y atom positions. In addition, atomic disordering positions in YB56 were detected from the differential images between observed and simulated images based on x-ray data, which were B24 clusters around the Y-holes. The present work indicates that the structure analysis combined with digital high-resolution electron microscopy, electron diffraction, and differential images is useful for the evaluation of atomic positions and disordering in the boron-based crystals.


Author(s):  
Sven Hovmöller ◽  
Linus Hovmöller Zou ◽  
Xiaodong Zou ◽  
Benjamin Grushko

Quasi-crystals shocked the crystallographic world when they were reported in 1984. We now know that they are not a rare exception, and can be found in many alloy systems. One of the richer systems for quasi-crystals and their approximants is Al−Co−Ni. A large series of pseudo-decagonal (PD) approximants have been found. Only two of them, PD4 and PD8, have been solved by X-ray crystallography. We report here the structures of PD1, PD2, PD3 and PD5, solved from the limited information that is provided by electron diffraction patterns, unit cell dimensions and high-resolution electron microscopy images.


Author(s):  
Xiaodong Zou ◽  
V.G. Zubkov ◽  
Gunnar Svensson ◽  
Sven Hovmöller

High resolution electron microscopy (HREM) combined with crystallographic image processing (CIP) is becoming a powerful technique for solving inorganic structures. With the image processing systems CRISP and ELD, running on a personal computer, this technique can be easily established in other laboratories. HREM images and electron diffraction patterns are digitized by a CCD camera and transferred into a PC. Phases and amplitudes are extracted from the Fourier transform of the HREM images. For thin crystals of metal oxides, the phases obtained by HREM and CIP inside the Scherzer resolution of the microscope are identical to the x-ray structure factor phases.Electron diffraction extends to much higher resolution than EM images (beyond 1 Å). The quality of the amplitudes is also higher than that from images, since ED data is not affected by the contract transfer function (CTF). Amplitudes extracted by ELD are close to x-ray diffraction amplitudes (within 30%).


1997 ◽  
Vol 53 (2) ◽  
pp. 221-230 ◽  
Author(s):  
A. R. Landa-Cánovas ◽  
S. Hansen ◽  
K. Ståhl

The structure of Sb0.9V1.1O4, antimony vanadium oxide, has been studied by powder X-ray diffraction, electron diffraction and high-resolution electron microscopy (HREM). The X-ray powder diffraction pattern showed only basic rutile reflections [a r = 4.6085 (1), c r = 3.0867 (1) Å] and the basic rutile structure was refined using the Rietveld method. A rutile superstructure was revealed when the sample was studied by electron diffraction. The electron diffraction patterns were indexed on the unit cell a = 21/2 a r , b = 21/2 b r , c = 2c r . Its space group, I41 md, was determined by means of convergent-beam electron diffraction (CBED). A structural model based on alternating cation ordering along c in the chains of edge-sharing octahedra is proposed and its electron diffraction patterns and HREM image are calculated and matched with the experimental ones.


1999 ◽  
Vol 55 (2) ◽  
pp. 255-257 ◽  
Author(s):  
X. Y. Yang ◽  
G. Y. Shi ◽  
X. M. Meng ◽  
H. L. Huang ◽  
Y. K. Wu

Using electron diffraction patterns and high-resolution electron microscopy (HREM), a trace 114R SiC in commercial α-SiC powder (mainly 6H SiC according to X-ray diffraction) has been discovered. In a hexagonal unit cell its stacking sequence is [(33)4(34)2]3, the periodicity along the c axis is 286.14 Å and a = b = 3.073 Å. 114R belongs to the structure series of (33) n34(33) m34 predicted theoretically by Pandey & Krishna [Mater. Sci. Eng. (1975), 20, 243–249] on the basis of the faulted matrix model.


Author(s):  
N. Uyeda ◽  
E. J. Kirkland ◽  
B. M. Siegel

The direct observation of structural change by high resolution electron microscopy will be essential for the better understanding of the damage process and its mechanism. However, this approach still involves some difficulty in quantitative interpretation mostly being due to the quality of obtained images. Electron diffraction, using crystalline specimens, has been the method most frequently applied to obtain a comparison of radiation sensitivity of various materials on the quantitative base. If a series of single crystal patterns are obtained the fading rate of reflections during the damage process give good comparative measures. The electron diffraction patterns also render useful information concerning the structural changes in the crystal. In the present work, the radiation damage of potassium tetracyano-platinate was dealt with on the basis two dimensional observation of fading rates of diffraction spots. KCP is known as an ionic crystal which possesses “one dimensional” electronic properties and it would be of great interest to know if radiation damage proceeds in a strongly asymmetric manner.


Author(s):  
Kenneth H. Downing ◽  
Robert M. Glaeser

The contrast observed in images of beam-sensitive, crystalline specimens is found to be significantly less than one would predict based on observations of electron diffraction patterns of the specimens. Factors such as finite coherence, inelastic scattering, and the limited MTF of the photographic emulsion account for some decrease in contrast. It appears, however, that most of the loss in signal is caused by motion of the specimen during exposure to the electron beam. The introduction of point and other defects in the crystal, resulting from radiation damage, causes bending and lateral motion, which degrade the contrast in the image. We have therefore sought to determine whether the beam-induced specimen motion can be reduced by reducing the area of the specimen which is illuminated at any one time.


Materials containing planar boundaries are of general interest and complete understanding of their structures is important. When direct imaging of the boundaries by, for instance, high-resolution electron microscopy, is impracticable, details of their structure and arrangement may be obtained from electron diffraction patterns. Such patterns are discussed in terms of those from intergrowth tungsten bronzes as specific examples. Fourier-transform calculations for proposed structures have been made to establish, in conjunction with optical-diffraction analogues, the features of the far-field diffraction patterns. These results have been compared with diffraction patterns obtained experimentally by transmission electron microscopy. The aim of the study, to show that the arrangement of the boundaries in these complicated phases can be deduced from their diffraction patterns without the need for high-resolution imaging, has been achieved. The steps to be taken to make these deductions are set out.


Reaction of bismuth metal with WO 3 in the absence of oxygen yields interesting bronze-like phases. From analytical electron microscopy and X-ray photoelectron spectroscopy, the product phases are found to have the general composition Bi x WO 3 with bismuth in the 3+ state. Structural investigations made with high resolution electron micrscopy and cognate techniques reveal that when x < 0.02, a perovskite bronze is formed. When x ≽ 0.02, however, intergrowth tungsten bronzes (i. t. b.) containing varying widths of the WO 3 slab are formed, the lattice periodicity being in the range 2.3-5.1 nm in a direction perpendicular to the WO 3 slabs. Image-matching studies indicate that the bismuth atoms are in the tunnels of the hexagonal tungsten bronze (h. t. b.) strips and the h. t. b. strips always remain one-tunnel wide. Annealed samples show a satellite structure around the superlattice spots in the electron diffraction patterns, possibly owing to ordering of the bismuth atoms in the tunnels. The i. t. b. phases show recurrent intergrowths extending up to 100 nm in several crystals. The periodicity varies considerably within the same crystal wherever there is disordered intergrowth, but unit cell dimensions can be assigned from X-ray and electron diffraction patterns. The maximum value of x in the i. t. b. phases is ca . 0.07 and there is no evidence for the i. t. b. phase progressively giving way to the h. t. b. phase with increase in x . Hexagonal tungsten bronzes that contain bismuth with x up to 0.02 can be formed by starting from hexagonal WO 3 , but the h. t. b. phase seems to be metastable. Optical, magnetic and electron transport properties of the i. t. b. phases have been measured and it appears that the electrons become itinerant when x > 0.05.


1993 ◽  
Vol 8 (11) ◽  
pp. 2785-2798 ◽  
Author(s):  
G.L. Skofronick ◽  
A.H. Carim ◽  
S.R. Foltyn ◽  
R.E. Muenchausen

Thick film (1.2 μm) YBCO superconductors grown by pulsed laser deposition on unbuffered and CeO2-buffered single crystal (001)-oriented yttria-stabilized zirconia (YSZ) substrates have been investigated. YBCO and YSZ react to form BaZrO3 (BZO), whereas YBCO and CeO2 react to form BaCeO3. Reaction phases were examined by θ-2θ and four-circle x-ray diffraction and high resolution electron microscopy. Three orientation relationships identified for the unbuffered films were (i) (001)YBCO ‖ (011)BZO ‖ (001)YSZ with [110]YBCO ‖ [100]BZO ‖ [100]YSZ, (ii) (001)YBCO ‖ (001)BZO ‖ (001)YSZ with [110]YBCO ‖ [100]BZO ‖ [100]YSZ, and (iii) (001)YBCO ‖ (001)BZO ‖ (001)YSZ with [100]YBCO ‖ [100]BZO ‖ [100]YSZ. The results suggest that for films grown at typical deposition temperatures, YBCO epitaxy is established before the interfacial reaction occurs. The presence of BaCeO3 in buffered films grown at high temperatures (790 °C) was confirmed by θ-2θ scans and selected area diffraction patterns.


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