Topochemical conversion of the discontinuous-zone-axis to form bismuth titanate oriented polycrystal nanocomposites

Author(s):  
Yan Wang ◽  
Dandan Yang ◽  
Minggang Yao ◽  
Lijie Li ◽  
Zhuonan Huang ◽  
...  
Keyword(s):  

A topochemical transformation of discontinuous band axis has been found in the preparation of bismuth titanate.

Author(s):  
J. S. Lally ◽  
R. J. Lee

In the 50 year period since the discovery of electron diffraction from crystals there has been much theoretical effort devoted to the calculation of diffracted intensities as a function of crystal thickness, orientation, and structure. However, in many applications of electron diffraction what is required is a simple identification of an unknown structure when some of the shape and orientation parameters required for intensity calculations are not known. In these circumstances an automated method is needed to solve diffraction patterns obtained near crystal zone axis directions that includes the effects of systematic absences of reflections due to lattice symmetry effects and additional reflections due to double diffraction processes.Two programs have been developed to enable relatively inexperienced microscopists to identify unknown crystals from diffraction patterns. Before indexing any given electron diffraction pattern, a set of possible crystal structures must be selected for comparison against the unknown.


Author(s):  
J W Steeds ◽  
R Vincent

We review the analytical powers which will become more widely available as medium voltage (200-300kV) TEMs with facilities for CBED on a nanometre scale come onto the market. Of course, high performance cold field emission STEMs have now been in operation for about twenty years, but it is only in relatively few laboratories that special modification has permitted the performance of CBED experiments. Most notable amongst these pioneering projects is the work in Arizona by Cowley and Spence and, more recently, that in Cambridge by Rodenburg and McMullan.There are a large number of potential advantages of a high intensity, small diameter, focussed probe. We discuss first the advantages for probes larger than the projected unit cell of the crystal under investigation. In this situation we are able to perform CBED on local regions of good crystallinity. Zone axis patterns often contain information which is very sensitive to thickness changes as small as 5nm. In conventional CBED, with a lOnm source, it is very likely that the information will be degraded by thickness averaging within the illuminated area.


Author(s):  
M.T. Otten ◽  
P.R. Buseck

ALCHEMI (Atom Location by CHannelling-Enhanced Microanalysis) is a TEM technique for determining site occupancies in single crystals. The method uses the channelling of incident electrons along specific crystallographic planes. This channelling results in enhanced x-ray emission from the atoms on those planes, thereby providing the required site-occupancy information. ALCHEMI has been applied with success to spinel, olivine and feldspar. For the garnets, which form a large group of important minerals and synthetic compounds, the channelling effect is weaker, and significant results are more difficult to obtain. It was found, however, that the channelling effect is pronounced for low-index zone-axis orientations, yielding a method for assessing site occupancies that is rapid and easy to perform.


Author(s):  
C. M. Sung ◽  
D. B. Williams

Researchers have tended to use high symmetry zone axes (e.g. <111> <114>) for High Order Laue Zone (HOLZ) line analysis since Jones et al reported the origin of HOLZ lines and described some of their applications. But it is not always easy to find HOLZ lines from a specific high symmetry zone axis during microscope operation, especially from second phases on a scale of tens of nanometers. Therefore it would be very convenient if we can use HOLZ lines from low symmetry zone axes and simulate these patterns in order to measure lattice parameter changes through HOLZ line shifts. HOLZ patterns of high index low symmetry zone axes are shown in Fig. 1, which were obtained from pure Al at -186°C using a double tilt cooling holder. Their corresponding simulated HOLZ line patterns are shown along with ten other low symmetry orientations in Fig. 2. The simulations were based upon kinematical diffraction conditions.


Author(s):  
E. Silva ◽  
R. Scozia

The purpose in obtaining zone axis pattern map (zap map) from a given material is to provide a quick and reliable tool to identify cristaline phases, and crystallographic directions, even in small particles. Bend contours patterns and Kossel lines patterns maps from Zr single crystal in the [0001] direction have been presented previously. In the present communication convergent beam electron diffraction (CBED) zap map of Zr will be shown. CBED patterns were obtained using a Philips microscope model EM300, which was set up to carry out this technique. Convergent objective upper pole piece for STEM and some electronic modifications in the lens circuits were required, furthermore the microscope was carefully cleaned and it was operated at a vacuum eminently good.CBED patterns in the Zr zap map consist of zero layer disks, showing fine details within them which correspond to intersecting set of higher order Laue zone (HOLZ) deficiency lines.


Author(s):  
H. Brigitte Krause ◽  
Yonglin Qian

A polycrystalline specimen of nominal formula EuGaAl with unknown crystal structure was investigated by various electron microscope techniques; EDS-, SED-, and CBED data were taken on a Philips 400 electron microscope operated at 100kV, HREM data on a Hitachi 9000 microscope operated at 300kV. The EDS data confirmed the composition for the bulk of the material but, in addition, revealed particles with other fractions of the elements. Only the EuGaAl particles were further investigated. The unit cell was determined to be orthorhombic with a ratio: a/b=0.969(2) , a/c=0.234(2) and b/c=0.234(2). The lattice constants are a=4.54(5)Ȧ, b=4.68Ȧ and c=19.97(20)Ȧ. Based on systematic extinctions for hkl reflections with h+l=2n+l, the unit cell was found to be b-centered. CBED patterns of the [001], [100], and [010] zone axes are shown in Fig. 1. The zone axis patterns are in agreement with the above stated data except for diffused (2m+l,2n+l,0)- reflections, not compatible with the above stated systematic absences. But these occurred only occasionally in conjunction with a complicated noncommensurate superlattice pattern.


Author(s):  
E D Boyes ◽  
L Hanna

A VG HB501 FEG STEM has been modified to provide track whilst tilt [TWIT] facilities for controllably tilting selected and initially randomly aligned nanometer-sized particles into the high symmetry zone-axis orientations required for microdiffraction, lattice imaging and chemical microanalysis at the unit cell level. New electronics display in alternate TV fields and effectively in parallel on split [+VTR] or adjacent externally synchronized screens, the micro-diffraction pattern from a selected area down to <1nm2 in size, together with the bright field and high angle annular dark field [HADF] STEM images of a much wider [˜1μm] area centered on the same spot. The new system makes it possible to tilt each selected and initially randomly aligned small particle into a zone axis orientation for microdiffraction, or away from it to minimize orientation effects in chemical microanalysis. Tracking of the inevitable specimen movement with tilt is controlled by the operator, with realtime [60Hz] update of the target designation in real space and the diffraction data in reciprocal space. The spot mode micro-DP and images of the surrounding area are displayed continuously. The regular motorized goniometer stage for the HB501STEM is a top entry design but the new control facilities are almost equivalent to having a stage which is eucentric with nanometric precision about both tilt axes.


Author(s):  
Y. Kikuchi ◽  
N. Hashikawa ◽  
F. Uesugi ◽  
E. Wakai ◽  
K. Watanabe ◽  
...  

In order to measure the concentration of arsenic atoms in nanometer regions of arsenic doped silicon, the HOLZ analysis is carried out underthe exact [011] zone axis observation. In previous papers, it is revealed that the position of two bright lines in the outer SOLZ structures on the[011] zone axis is little influenced by the crystal thickness and the background intensity caused by inelastic scattering electrons, but is sensitive to the concentration of As atoms substitutbnal for Siatomic site.As the result, it becomes possible to determine the concentration of electrically activated As atoms in silicon within an observed area by means of the simple fitting between experimental result and dynamical simulatioan. In the present work, in order to investigate the distribution of electrically activated As in silicon, the outer HOLZ analysis is applied using a nanometer sized probe of TEM equipped with a FEG.Czodiralsld-gown<100>orientated p-type Si wafers with a resistivity of 10 Ώ cm are used for the experiments.TheAs+ implantation is performed at a dose of 5.0X1015cm-2at 25keV.


Author(s):  
Philip D. Hren

The pattern of bend contours which appear in the TEM image of a bent or curled sample indicates the shape into which the specimen is bent. Several authors have characterized the shape of their bent foils by this method, most recently I. Bolotov, as well as G. Möllenstedt and O. Rang in the early 1950’s. However, the samples they considered were viewed at orientations away from a zone axis, or at zone axes of low symmetry, so that dynamical interactions between the bend contours did not occur. Their calculations were thus based on purely geometric arguments. In this paper bend contours are used to measure deflections of a single-crystal silicon membrane at the (111) zone axis, where there are strong dynamical effects. Features in the bend contour pattern are identified and associated with a particular angle of bending of the membrane by reference to large-angle convergent-beam electron diffraction (LACBED) patterns.


Author(s):  
J. M. Zuo ◽  
A. L. Weickenmeier ◽  
R. Holmestad ◽  
J. C. H. Spence

The application of high order reflections in a weak diffraction condition off the zone axis center, including those in high order laue zones (HOLZ), holds great promise for structure determination using convergent beam electron diffraction (CBED). It is believed that in this case the intensities of high order reflections are kinematic or two-beam like. Hence, the measured intensity can be related to the structure factor amplitude. Then the standard procedure of structure determination in crystallography may be used for solving unknown structures. The dynamic effect on HOLZ line position and intensity in a strongly diffracting zone axis is well known. In a weak diffraction condition, the HOLZ line position may be approximated by the kinematic position, however, it is not clear whether this is also true for HOLZ intensities. The HOLZ lines, as they appear in CBED patterns, do show strong intensity variations along the line especially near the crossing of two lines, rather than constant intensity along the Bragg condition as predicted by kinematic or two beam theory.


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