Prospects for convergent beam electron diffraction with a 200kV cold field-emission transmission electron microscope

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):  
John F. Mansfield

One of the most important advancements of the transmission electron microscopy (TEM) in recent years has been the development of the analytical electron microscope (AEM). The microanalytical capabilities of AEMs are based on the three major techniques that have been refined in the last decade or so, namely, Convergent Beam Electron Diffraction (CBED), X-ray Energy Dispersive Spectroscopy (XEDS) and Electron Energy Loss Spectroscopy (EELS). Each of these techniques can yield information on the specimen under study that is not obtainable by any other means. However, it is when they are used in concert that they are most powerful. The application of CBED in materials science is not restricted to microanalysis. However, this is the area where it is most frequently employed. It is used specifically to the identification of the lattice-type, point and space group of phases present within a sample. The addition of chemical/elemental information from XEDS or EELS spectra to the diffraction data usually allows unique identification of a phase.


Author(s):  
J W Steeds

That the techniques of convergent beam electron diffraction (CBED) are now widely practised is evident, both from the way in which they feature in the sale of new transmission electron microscopes (TEMs) and from the frequency with which the results appear in the literature: new phases of high temperature superconductors is a case in point. The arrival of a new generation of TEMs operating with coherent sources at 200-300kV opens up a number of new possibilities.First, there is the possibility of quantitative work of very high accuracy. The small probe will essentially eliminate thickness or orientation averaging and this, together with efficient energy filtering by a doubly-dispersive electron energy loss spectrometer, will yield results of unsurpassed quality. The Bloch wave formulation of electron diffraction has proved itself an effective and efficient method of interpreting the data. The treatment of absorption in these calculations has recently been improved with the result that <100> HOLZ polarity determinations can now be performed on III-V and II-VI semiconductors.


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):  
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.


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.


1997 ◽  
Vol 3 (S2) ◽  
pp. 477-478
Author(s):  
M.G. Shlepr ◽  
G.A. Schrantz ◽  
A.L. Rivoli ◽  
G. Bajor

A recent process technology to manufacture bipolar junction transistors utilizes polysilicon emitters. Polysilicon is deposited, appropriately doped to form both NPN and PNP transistors, and exposed to temperatures that result in grain growth. Since polysilicon is in contact with Si( 100) at the emitter, base, and collector (Fig. 1), solid phase epitaxial regrowth might also occur. Production runs with this structure occasionally produce transistors with low current gain. High and low gain NPN and PNP transistors were characterized by transmission electron microscopy.Vertical sections through NPN/PNP transistor arrays were made by the wedge technique, low-angle ion milled to electron-transparency, and viewed at 200 KV. The grain size of the polysilicon on oxide was recorded and estimated. The extent of epitaxial regrowth was quantified for each of the Si (100) contact areas. Convergent Beam Electron Diffraction (CBED) was used to confirm the orientation of the presumed regrown polysilicon.


2011 ◽  
Vol 492 ◽  
pp. 112-117 ◽  
Author(s):  
Zi Wei Liu ◽  
Zhi Gang Zhang ◽  
Hua Li ◽  
Wei Wu ◽  
Jia Jie Hua ◽  
...  

The black-glazed shreds from Qingliangsi kiln were studied. The glaze and body micro- structures, compositions and crystal phases were observed and analyzed by field emission scanning electron, microscope multiple functions electron probe-energy spectrum instrument and field emission transmission electron microscope. The iron oxide crystal in oil spot was mainly the ε-Fe2O3 in the orientation of the zone axis [001], and also few content of ε-Fe2O3 in the orientation of the zone axis [412]. The brown oil spots on the glaze surface were aggregations of a great deal of iron oxide hematite crystals. Bodies of black-glazed shreds have high Al2O3(26.47 % ~ 30.48%) and low SiO2 (62.77% ~ 66.20%), which pertained to the typical recipe of north porcelain bodies. The glaze are attributed to calcium-alkali glaze, and according to the ratio of Al2O3:SiO2, it belongs to the crystallization glaze.


2006 ◽  
Vol 955 ◽  
Author(s):  
Zuzanna Liliental-Weber ◽  
X. Ni ◽  
H. Morkoc

ABSTRACTTransmission electron microscopy was used to study defects in lateral epitaxial layers of GaN which were overgrown on a template of a-plane (1120) GaN grown on (1102) r-plane Al2O3. A high density of basal stacking faults is formed in these layers because the c-planes of wurtzite structure are arranged along the growth direction. Density of these faults is decreasing at least by two orders of magnitude lower in the wings compared to the seed areas. Prismatic stacking faults and threading dislocations are also observed, but their densities drastically decrease in the wings. The wings grow with opposite polarities and the Ga-wing width is at least 6 times larger than N-wing and coalescence is rather difficult. Some tilt and twist was detected using Large Angle Convergent Beam Electron Diffraction.


1989 ◽  
Vol 159 ◽  
Author(s):  
V.P. Dravid ◽  
M.R. Notis ◽  
C.E. Lyman ◽  
A. Revcolevschi

ABSTRACTLow energy lamellar interfaces in the directionally solidified eutectic (DSE) NiO-ZrO2(CaO) have been investigated using transmission electron diffraction and imaging. The symmetry of this bicrystal and an aspect of interfacial relaxations in the form of symmetry lowering in-plane rigid body translation (RBT) have been explored by performing convergent beam electron diffraction (CBED) experiments of plan-view bicrystals. Edge-on interfaces have also been studied by conventional and high resolution transmission electron microscopy (CTEM and HRTEM respectively), and electron diffraction fine structure analysis. Despite certain experimental difficulties due to interfacial defects and strain, plan-view CBED patterns offered valuable information concerning bicrystal symmetry and indicated no symmetry lowering RBT in this bicrystal. The suitability of plan-view CBED is briefly discussed in view of its potential as a technique to determine bicrystal symmetry and RBT.


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