High-resolution annular dark-field STEM imaging

Author(s):  
Sean Hillyard ◽  
John Silcox

Annular dark field STEM imaging has become an important tool as both a high resolution imaging technique showing Z-contrast, and as a way to locate the probe on the specimen while simultaneously recording other data such as electron energy loss spectra. It is intrinsically quantitative since image data can be recorded directly from linear detectors into digital memory Experiments on simple samples,and a multislice simulation approach backed by experimental evidence has been used to explore the image dependence on experimental factors such as inner detector angles and other elements in the imagingprocess Earlier work demonstrated marked thickness dependence in high Z specimens.In annular dark field imaging, the resolvable spatial resolution is roughly equal to the size of the electron probe One important factor in forming a small probe, and therefore in getting high resolution images, is an electron gun with a small virtual source size. An example is shown in Figure 1, which plots the relativestrengths of the 2.9Å and 2.1 Å fringes taken from experimental images of InP (100) What is seen is that the 2.1Å fringe intensity, at the extreme limits of resolution for this probe (approx 2.2Å in size), changes greatly in comparison with the more easily resolvable 2.9Å fringe as the source demagnification, in effect the source size, is changed.

Author(s):  
M. Kelly ◽  
D.M. Bird

It is well known that strain fields can have a strong influence on the details of HREM images. This, for example, can cause problems in the analysis of edge-on interfaces between lattice mismatched materials. An interesting alternative to conventional HREM imaging has recently been advanced by Pennycook and co-workers where the intensity variation in the annular dark field (ADF) detector is monitored as a STEM probe is scanned across the specimen. It is believed that the observed atomic-resolution contrast is correlated with the intensity of the STEM probe at the atomic sites and the way in which this varies as the probe moves from cell to cell. As well as providing a directly interpretable high-resolution image, there are reasons for believing that ADF-STEM images may be less suseptible to strain than conventional HREM. This is because HREM images arise from the interference of several diffracted beams, each of which is governed by all the excited Bloch waves in the crystal.


Author(s):  
Z. L. Wang ◽  
J. Bentley

The success of obtaining atomic-number-sensitive (Z-contrast) images in scanning transmission electron microscopy (STEM) has shown the feasibility of imaging composition changes at the atomic level. This type of image is formed by collecting the electrons scattered through large angles when a small probe scans across the specimen. The image contrast is determined by two scattering processes. One is the high angle elastic scattering from the nuclear sites,where ϕNe is the electron probe function centered at bp = (Xp, yp) after penetrating through the crystal; F denotes a Fourier transform operation; D is the detection function of the annular-dark-field (ADF) detector in reciprocal space u. The other process is thermal diffuse scattering (TDS), which is more important than the elastic contribution for specimens thicker than about 10 nm, and thus dominates the Z-contrast image. The TDS is an average “elastic” scattering of the electrons from crystal lattices of different thermal vibrational configurations,


Author(s):  
J. H. Butler ◽  
G. M. Brown

High resolution Imaging of zeolites is difficult because these materials are very susceptible to Irradiation damage. It is now well known that dehydrated samples are more stable under the electron beam. Thus the most successful high resolution studies of zeolites to date have been on samples which were freeze-fractured and subsequently dehydrated via heating in a vacuum oven. Electron microscopy was then performed using a combination of low Incident beam currents and sensitive detectors. One problem with this method is that zeolites fracture along cleavage planes and therefore are deposited on microscope grids In a particular orientation. This limits the range of viewing angles. Here we describe a method of sample preparation via ultramlctrotomy as well as the establishment of suitable FEG/STEM Imaging conditions which permit the observation of small (7-14 A diameter) Pt particles within Individual zeolite channels using the method of Z-contrast as applied with a high-angle annular dark field detector. This method allows observation over all crystalline orientations for relatively long exposures to the beam.


Author(s):  
R.A. Herring ◽  
M.E. Twigg

Hollow cone illumination using a large C2 blocked-aperture (bl apt) in the conventional TEM (CTEM) can remove the beams within the zero-order Laue zone (ZOLZ) thereby making lattice images more simply interpretable. Dark-field (DF) hollow cone illumination has the added advantage of enhancing the Z-contrast within the lattice image, since the electrons contributing to the image must be scattered over a large angle (approximately 10 mrad). Both of these imaging methods have been explored, using a 600 um C2 bl apt and objective aperture sizes of 70, 20 and 10 um, and are reported in this paper.Much interest has been generated by the report of Pennycook [1] on STEM Z-contrast imaging using annular dark-field. In earlier work ,it was noted that CTEM hollow cone imaging and STEM annular dark-field imaging are related via reciprocity [2] (Fig. 1). In addition, Zernike has shown the advantages of hollow cone illumination in optical phase-contrast microscopy [3]. The electron-optical analogues to these optical techniques are now possible because of the low Cs values achieved in modern TEMs.


2009 ◽  
Vol 15 (3) ◽  
pp. 213-221 ◽  
Author(s):  
Thomas Riedl ◽  
Thomas Gemming ◽  
Kathrin Dörr ◽  
Martina Luysberg ◽  
Klaus Wetzig

AbstractThis article presents a (scanning) transmission electron microscopy (TEM) study of Mn valency and its structural origin at La0.7Sr0.3MnO3/SrTiO3(0 0 1) thin film interfaces. Mn valency deviations can lead to a breakdown of ferromagnetic order and thus lower the tunneling magnetoresistance of tunnel junctions. Here, at the interface, a Mn valency reduction of 0.16 ± 0.10 compared to the film interior and an additional feature at the low energy-loss flank of the Mn-L3 line have been observed. The latter may be attributed to an elongation of the (0 0 1) plane spacing at the interface detected by geometrical phase analysis of high-resolution images. Regarding the interface geometry, high-resolution high-angle annular dark-field scanning TEM images reveal an atomically sharp interface in some regions whereas the transition appears broadened in others. This can be explained by the presence of steps. The performed measurements indicate that, among the various structure-related influences on the valency, the atomic layer termination and the local oxygen content are most important.


1997 ◽  
Vol 3 (S2) ◽  
pp. 1147-1148 ◽  
Author(s):  
E.J. Kirkland

Z-contrast produces an image that varies strongly with atomic number and offers limited chemical sensitivity. The annular dark field scanning transmission microscope (ADF-STEM) has recently been used to produce Z-contrast images at high resolution. In a STEM the electron beam is focused into a small probe at the specimen plane and scanned across the specimen. The electrons scattered at high angle are collected by an annular detector to produce a signal that approximately varies as Z11.5 to Z2. The only commercial supplier of dedicated STEM'S (VG-Microscopes, now Thermo) has recently discontinued production, so it is worth considering how to produce an equivalent Z-contrast image in a conventional transmission electron microscope (CTEM).The reciprocity theorem states that the STEM and CTEM are equivalent if the source and detector are interchanged (reciprocity hold for all orders of elastic scattering so it is not necessary to restrict this discussion to weakly scattering specimens).


Author(s):  
S. Hillyard ◽  
Y.-P. Chen ◽  
W.J. Schaff ◽  
L.F. Eastman ◽  
J. Silcox

Annular dark field imaging in the scanning transmission electron microscope (STEM) exhibits both high resolution and Z-contrast. It is intrinsically quantitative since image data can be recorded directly from linear detectors into digital memory. Annular dark field imaging has been used, along with energy filtered imaging to correct for sample thickness variation, to map out the In concentration in InxGa1-xAs quantum wells with near atomic resolution and sensitivity. This approach is similar to “chemical lattice imaging”, which maps out composition variation using a conventional transmission electron microscope image and a vector pattern recognition algorithm.The quantum wells were grown by molecular-beam epitaxy (MBE). Figure 1 shows a typical high resolution annular dark field image of a 50 Å wide nominal In0.3Ga0.7As/GaAs quantum well. The linescan in figure 2 gives the actual numbers making up the image. Barring contaminants and lattice imperfections, the change in intensity with position is caused by two things: variation of In concentration and thickness.


2005 ◽  
Vol 876 ◽  
Author(s):  
Huiping Xu ◽  
Laurent Menard ◽  
Anatoly Frenkel ◽  
Ralph Nuzzo ◽  
Duane Johnson ◽  
...  

AbstractOur direct density function-based simulations of Ru-, Pt- and mixed Ru-Pt clusters on carbon-based supports reveal that substrates can mediate the PtRu5 particles [1]. Oblate structure of PtRu5 on C has been found [2]. Nevertheless, the cluster-substrate interface interactions are still unknown. In this work, we present the applications of combinations of quantitative z-contrast imaging and high resolution electron microscopy in investigating the effect of different substrates and ligand shells on metal particles. Specifically, we developed a relatively new and powerful method to determine numbers of atoms in a nanoparticle as well as three-dimensional structures of particles including size and shape of particles on the substrates by very high angle (~96mrad) annular dark-field (HAADF) imaging [2-4] techniques. Recently, we successfully synthesize icosahedra Au13 clusters with mixed ligands and cuboctahedral Au13 cores with thiol ligands, which have been shown by TEM to be of sub-nanometer size (0.84nm) and highly monodisperse narrow distribution. X-ray absorption and UV-visible spectra indicate many differences between icosahedra and cuboctahedral Au13 cores. Particles with different ligands show different emissions and higher quantum efficiency has been found in Au11 (PPH3) SC12)2C12. We plan to deposit those ligands-protected gold clusters onto different substrates, such as, TiO2 and graphite, etc. Aforementioned analysis procedure will be performed for those particles on the substrates and results will be correlated with that of our simulations and activity properties. This approach will lead to an understanding of the cluster-substrates relationship for consideration in real applications.


Author(s):  
Akira Tanaka ◽  
David F. Harling

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.


Author(s):  
Earl J. Kirkland ◽  
Robert J. Keyse

An ultra-high resolution pole piece with a coefficient of spherical aberration Cs=0.7mm. was previously designed for a Vacuum Generators HB-501A Scanning Transmission Electron Microscope (STEM). This lens was used to produce bright field (BF) and annular dark field (ADF) images of (111) silicon with a lattice spacing of 1.92 Å. In this microscope the specimen must be loaded into the lens through the top bore (or exit bore, electrons traveling from the bottom to the top). Thus the top bore must be rather large to accommodate the specimen holder. Unfortunately, a large bore is not ideal for producing low aberrations. The old lens was thus highly asymmetrical, with an upper bore of 8.0mm. Even with this large upper bore it has not been possible to produce a tilting stage, which hampers high resolution microscopy.


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