scholarly journals Z-contrast imaging of catalysts in the 300 kV STEM

Author(s):  
S. J. Pennycook ◽  
D. E. Jesson ◽  
D. R. Liu

Z-contrast imaging in the scanning transmission electron microscope has become the accepted technique for imaging sub-nanometer catalyst clusters, utilizing the high angle annular detector introduced by Howie. The lack of coherent phase contrast effects greatly assists the identification of small clusters, especially near the resolution limit of the microscope. The choice of inner detector angle depends on the system being studied. The highest signal to noise ratio is obtained with the smallest inner detector angle, but increasing this angle significantly reduces the contribution of coherently scattered electrons, which is advantageous for crystalline support materials. In this case, small metal clusters may be unambiguosly distinguished from diffracting regions of the support, and their size distributions determined. Fig 1 compares two preparations of 1 wt% Pd on γ-Al2O3, prepared from palladium nitrate solution, and aged at 600°C for (a) 6 hours, and (b) 24 hours. Images were taken with a VG Microscopes HB501UX 100 kV STEM, using a probe size of ∼3Å The narrower size distribution resulting from the longer aging time is clearly observed.

2000 ◽  
Vol 6 (4) ◽  
pp. 343-352 ◽  
Author(s):  
S.J. Pennycook ◽  
B. Rafferty ◽  
P.D. Nellist

AbstractWe show that in the limit of a large objective (probe-forming) aperture, relevant to a spherical aberration corrected microscope, the Z-contrast image of a zone-axis crystal becomes an image of the 1s Bloch states. The limiting resolution is therefore the width of the Bloch states, which may be greater than that of the free probe. Nevertheless, enormous gains in image quality are expected from the improved contrast and signal-to-noise ratio. We present an analytical channeling model for the thickness dependence of the Z-contrast image in a zone-axis crystal, and show that, at large thicknesses, columnar intensities become proportional to the mean square atomic number, Z2.


2000 ◽  
Vol 6 (4) ◽  
pp. 343-352 ◽  
Author(s):  
S.J. Pennycook ◽  
B. Rafferty ◽  
P.D. Nellist

Abstract We show that in the limit of a large objective (probe-forming) aperture, relevant to a spherical aberration corrected microscope, the Z-contrast image of a zone-axis crystal becomes an image of the 1s Bloch states. The limiting resolution is therefore the width of the Bloch states, which may be greater than that of the free probe. Nevertheless, enormous gains in image quality are expected from the improved contrast and signal-to-noise ratio. We present an analytical channeling model for the thickness dependence of the Z-contrast image in a zone-axis crystal, and show that, at large thicknesses, columnar intensities become proportional to the mean square atomic number, Z2.


1999 ◽  
Vol 589 ◽  
Author(s):  
Y Kotaka ◽  
T. Yamazaki ◽  
Y Kikuchi ◽  
K. Watanabe

AbstractThe high-angle annular dark-field (HAADF) technique in a dedicated scanning transmission electron microscope (STEM) provides strong compositional sensitivity dependent on atomic number (Z-contrast image). Furthermore, a high spatial resolution image is comparable to that of conventional coherent imaging (HRTEM). However, it is difficult to obtain a clear atomic structure HAADF image using a hybrid TEM/STEM. In this work, HAADF images were obtained with a JEOL JEM-2010F (with a thermal-Schottky field-emission) gun in probe-forming mode at 200 kV. We performed experiments using Si and GaAs in the [110] orientation. The electron-optical conditions were optimized. As a result, the dumbbell structure was observed in an image of [110] Si. Intensity profiles for GaAs along [001] showed differences for the two atomic sites. The experimental images were analyzed and compared with the calculated atomic positions and intensities obtained from Bethe's eigen-value method, which was modified to simulate HAADF-STEM based on Allen and Rossouw's method for convergent-beam electron diffraction (CBED). The experimental results showed a good agreement with the simulation results.


1999 ◽  
Vol 589 ◽  
Author(s):  
Y. Ito ◽  
S. Stemmer ◽  
R. F. Klie ◽  
N. D. Browning ◽  
A. Sane ◽  
...  

AbstractThe high mobility of anion vacancies in oxygen deficient perovskite type materials makes these ceramics potential candidates for oxygen separation membranes. As a preliminary investigation of the defect chemistry in these oxides, we show here the analysis of SrCoO3−σ using atomic resolution Z-contrast imaging and electron energy loss spectroscopy in the scanning transmission electron microscope. In particular, after being subjected to oxidation/reduction cycles at high temperatures we find the formation of ordered microdomains with the brownmillerite structure.


2001 ◽  
Vol 7 (S2) ◽  
pp. 202-203
Author(s):  
T. Topuria ◽  
P. Möck ◽  
N.D. Browning ◽  
L.V. Titova ◽  
M. Dobrowolska ◽  
...  

CdSe/ZnSe based semiconductor quantum dot (Q D) structures are a promising candidate for optoelectronic device applications. However, key to the luminescence properties is the cation distribution and ordering on the atomic level within the CdSe QDs/agglomerates. Here the Z contrast imaging technique in the scanning transmission electron microscope (STEM) is employed to study multisheet (Cd,Zn,Mn)Se QD structures. Since Z-contrast is an incoherent imaging technique, problems associated with strain contrast in conventional TEM are avoided an accurate size and composition determinations can be made.For this work we used a JEOL JEM 201 OF field emission STEM/TEM. The sample was grown by molecular beam epitaxy in order to achieve vertical self-ordering of Cd rich quasi-2D platelet This sample comprises 8 sequences of 10 ML (2.83 nm)Zn0.9Mn0.1Se cladding layer and 0.3 ML (0.09 nm) CdSe sheet, a further 10 ML of Zn0.9Mn0.1Se, and a 50 nm ZnSe capping layer.


2000 ◽  
Vol 6 (S2) ◽  
pp. 100-101
Author(s):  
N. Dellby ◽  
O.L. Krivanek ◽  
A.R. Lupini

Electron probe formation in a scanning transmission electron microscope (STEM) has two properties that maximize the benefits of spherical aberration correction: the smallest and brightest probes are formed when all the geometric aberrations are set to zero, and the size of the probe is not greatly affected by the presence of chromatic aberration. This contrasts with the case of conventional, fixed-beam TEM (CTEM), in which optimized phase-contrast imaging demands a non-zero spherical aberration coefficient (Cs), and chromatic aberration constitutes a major resolution limit. As a result, a consensus is presently emerging that the benefits of aberration correction will be felt most strongly in STEM.Our efforts in Cs-corrected STEM have progressed from a proof-of-principle Cs corrector [1] to an optimized second-generation design [2]. The corrector in both cases is of the quadrupole-octupole type. The second-generation corrector uses separate quadrupoles and octupoles, and concentrates on maximizing the octupole strength.


1999 ◽  
Vol 583 ◽  
Author(s):  
S. J. Pennycook ◽  
Y. Yan ◽  
A. Norman ◽  
Y. Zhang ◽  
M. Al-Jassim ◽  
...  

AbstractIn the last ten years, the scanning transmission electron microscope (STEM) has become capable of forming electron probes of atomic dimensions making possible a new approach to high-resolution electron microscopy, Z-contrast imaging. Formed by mapping the intensity of high-angle scattered electrons as the probe is scanned across the specimen, the Z-contrast image represents a direct map of the specimen scattering power at atomic resolution. It is an incoherent image, and can be directly interpreted in terms of atomic columns. High angle scattering comes predominantly from the atomic nuclei, so the scattering cross section depends on atomic number (Z) squared. Z-contrast microscopy can therefore be used to study compositional ordering and segregation at the atomic scale. Here we present three examples of ordering: first, ferroelectric materials, second, III-V semiconductor alloys, and finally, cooperative segregation at a semiconductor grain boundary, where a combination of Z-contrast imaging with first principles theory provides a complete atomic-scale view of the sites and configurations of the segregant atoms.


Author(s):  
N. D. Browning ◽  
M. M. McGibbon ◽  
M. F. Chisholm ◽  
S. J. Pennycook

Characterization of grain boundaries in ceramics is complicated by the multicomponent nature of the materials, the presence of secondary phases, and the tendency for the grain boundary plane to “wander” on the length scale of a few nanometers. However, recent developments in the scanning transmission electron microscope (STEM) have now made it possible to correlate directly the structure, composition and bonding at grain boundaries on the atomic scale. This direct experimental characterization of grain boundaries is achieved through the combination of Z-contrast imaging (structure) and electron energy loss spectroscopy (EELS) (composition and bonding). For crystalline materials in zone-axis orientations, where the atomic spacing is larger than the probe size, the Z-contrast technique provides a direct image of the metal (high Z) columns. This image, being formed from only the high-angle scattering, can be used to position the electron probe with atomic precision for simultaneous EELS. Under certain collection conditions, the spectrum can have the same atomic spatial resolution as the image, thus permitting the spectra to be correlated with a known atomic location.


1995 ◽  
Vol 1 (6) ◽  
pp. 231-251 ◽  
Author(s):  
S.J. Pennycook ◽  
D.E. Jesson ◽  
M.F. Chisholm ◽  
N.D. Browning ◽  
A.J. McGibbon ◽  
...  

Z-contrast STEM using an annular detector can provide an intuitively interpretable, column-by-column, compositional map of crystals. Incoherent imaging reduces dynamical effects to second order so that the map directly reflects the positions of the atomic columns and their relative high-angle scattering power. This article outlines how these characteristics arise, presents some examples of the insights available from a direct image, and discusses recent developments of atomic-resolution microanalysis, direct structure retrieval by maximum entropy analysis, and Z-contrast imaging at 1.4 Å resolution using a 300-kV STEM.


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