TEM Z-contrast imaging with wide-angle hollow-cone illumination

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

High resolution scanning transmission electron microscopy (STEM) images with contrast sensitive to atomic number (Z-contrast) have been obtained with the use of a high-angle annular detector. The equivalent conventional transmission electron microscopy (TEM) dark-field mode reciprocally related to Z-contrast STEM is wide-angle hollow-cone illumination with an on-axis objective aperture. There are two ways to obtain hollow cone illumination; with an annular condenser aperture or by conically scanning the beam tilt coils. As in the case of STEM Z-contrast imaging, resolution with hollow-cone illumination should theoretically be higher than for phase contrast imaging in the same instrument.Philips CM30/STEM, CM12/STEM, and EM400T/FEG/STEM instruments have been used to investigate this imaging technique. The conical illumination dark-field mode is standard on the CM series and was implemented with a hybrid diffraction unit on the EM400. Commercial (SPI Supplies #1780) copper annular apertures with inner and outer diameters of 600 and 900 μm, respectively, spot welded to suitable supports for use as condenser apertures, resulted in cone angles too small to give good Z-contrast in the microprobe mode, because there is still a large diffraction contrast contribution.

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,


2020 ◽  
Vol 75 (11) ◽  
pp. 913-919
Author(s):  
Frank Krumeich

AbstractSince the 1970s, high-resolution transmission electron microscopy (HRTEM) is well established as the most appropriate method to explore the structural complexity of niobium tungsten oxides. Today, scanning transmission electron microscopy (STEM) represents an important alternative for performing the structural characterization of such oxides. STEM images recorded with a high-angle annular dark field (HAADF) detector provide not only information about the cation positions but also about the distribution of niobium and tungsten as the intensity is directly correlated to the local scattering potential. The applicability of this method is demonstrated here for the characterization of the real structure of Nb7W10O47.5. This sample contains well-ordered domains of Nb8W9O47 and Nb4W7O31 besides little ordered areas according to HRTEM results. Structural models for Nb4W7O31 and twinning occurring in this phase have been derived from the interpretation of HAADF-STEM images. A remarkable grain boundary between well-ordered domains of Nb4W7O31 and Nb8W9O47 has been found that contains one-dimensionally periodic features. Furthermore, short-range order observed in less ordered areas could be attributed to an intimate intergrowth of small sections of different tetragonal tungsten bronze (TTB) based structures.


2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.


Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4531
Author(s):  
Maria Meledina ◽  
Geert Watson ◽  
Alexander Meledin ◽  
Pascal Van Der Voort ◽  
Joachim Mayer ◽  
...  

Ru catalyst nanoparticles were encapsulated into the pores of a Cr-based metal-organic framework (MOF)—MIL-101. The obtained material, as well as the non-loaded MIL-101, were investigated down to the atomic scale by annular dark-field scanning transmission electron microscopy using low dose conditions and fast image acquisition. The results directly show that the used wet chemistry loading approach is well-fitted for the accurate embedding of the individual catalyst nanoparticles into the cages of the MIL-101. The MIL-101 host material remains crystalline after the loading procedure, and the encapsulated Ru nanoparticles have a metallic nature. Annular dark field scanning transmission electron microscopy, combined with EDX mapping, is a perfect tool to directly characterize both the embedded nanoparticles and the loaded nanoscale MOFs. The resulting nanostructure of the material is promising because the Ru nanoparticles hosted in the MIL-101 pores are prevented from agglomeration—the stability and lifetime of the catalyst could be improved.


2008 ◽  
Vol 112 (6) ◽  
pp. 1759-1763 ◽  
Author(s):  
Norihiko L. Okamoto ◽  
Bryan W. Reed ◽  
Shareghe Mehraeen ◽  
Apoorva Kulkarni ◽  
David Gene Morgan ◽  
...  

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.


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