Strain measurement by means of bend contour microscopy

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 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):  
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):  
J.M.K. Wiezorek ◽  
H.L. Fraser

Conventional methods of convergent beam electron diffraction (CBED) use a fully converged probe focused on the specimen in the object plane resulting in the formation of a CBED pattern in the diffraction plane. Large angle CBED (LACBED) uses a converged but defocused probe resulting in the formation of ‘shadow images’ of the illuminated sample area in the diffraction plane. Hence, low-spatial resolution image information and high-angular resolution diffraction information are superimposed in LACBED patterns which enables the simultaneous observation of crystal defects and their effect on the diffraction pattern. In recent years LACBED has been used successfully for the investigation of a variety of crystal defects, such as stacking faults, interfaces and dislocations. In this paper the contrast from coherent precipitates and decorated dislocations in LACBED patterns has been investigated. Computer simulated LACBED contrast from decorated dislocations and coherent precipitates is compared with experimental observations.


Author(s):  
P.A. Midgley ◽  
R. Vincent ◽  
D. Cherns

The oxygenation of YBa2Cu3O7−x (YBCO) leads to an orthorhombic distortion of the unit cell to accommodate the extra oxygen atom. This makes the formation of twins energetically favourable with CuO4 planar unit chains running alternately along the a and b axes of the parent tetragonal structure. The geometry of this twinning is such that four possible twin variants may co-exist with the twin boundaries lying in the (110) or (110) planes of the deformed structure. The traces of these planes are not mutually perpendicular and thus the crystal is strained to allow for the mismatch. It is to the nature of this strain field that this work has been addressed.Sintered samples were prepared by crushing and dispersing the resultant powder onto a very fine Cu mesh grid. Single crystals were chemically thinned to perforation. No discernible artefacts were seen and similar results were obtained with either method.


2011 ◽  
Vol 1295 ◽  
Author(s):  
X. H. Sang ◽  
A. Kulovits ◽  
J. Wiezorek

ABSTRACTAccurate Debye-Waller (DW) factors of chemically ordered β-NiAl (B2, cP2, ${\rm{Pm}}\bar 3 {\rm{m}}$) have been measured at different temperatures using an off-zone axis multi-beam convergent beam electron diffraction (CBED) method. We determined a cross over temperature below which the DW factor of Ni becomes smaller than that of Al of ~90K. Additionally, we measured for the first time DW factors and structure factors of chemically ordered γ1-FePd (L10, tP2, P4/mmm) at 120K. We were able to simultaneously determine all four anisotropic DW factors and several low order structure factors using different special off-zone axis multi-beam convergent beam electron diffraction patterns with high precision and accuracy. An electron charge density deformation map was constructed from measured X-ray diffraction structure factors for γ1-FePd.


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