Atomic Scale Characterization Of Interfaces And Defects In Non-Stoichiometricmulticomponent Oxides

1999 ◽  
Vol 5 (S2) ◽  
pp. 106-107
Author(s):  
S. Stemmer ◽  
S. K. Streiffer ◽  
A. Sane ◽  
T. J. Mazanec ◽  
N. D. Browning

The ability to obtain chemical information with (near) atomic resolution has recently become possible by a combined approach of Z-contrast imaging with electron energy-loss spectroscopy (EELS) in scanning transmission electron microscopes. This method is particularly interesting for the characterization of structure-property relationships in novel multicomponent oxides, which possess added functionality due to their high nonstoichiometry.In this paper we demonstrate the capabilities of this method in analyzing the microstructural mechanisms of accommodation of non-stoichiometry, using two example systems: (Ba,Sr)TiO3thin films for DRAM applications, grown by MOCVD with different amounts of excess titanium, and an oxygen-deficient perovskite ceramic, SrCoOx. The experiments were performed in a JEOL JEM 201 OF field emission transmission electron microscope, operating at 200 kV, equipped with an annular dark-field detector, scanning unit and a post-column imaging filter (Gatan GIF 200). This microscope has been demonstrated to achieve probe sizes of under 1.5 Å .

2006 ◽  
Vol 12 (S02) ◽  
pp. 1344-1345
Author(s):  
D Williams ◽  
M Watanabe

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2006


Nanoscale ◽  
2021 ◽  
Author(s):  
Sytze de Graaf ◽  
Majid Ahmadi ◽  
Ivan Lazić ◽  
Eric Bosch ◽  
Bart J. Kooi

Scanning transmission electron microscopy (STEM) is the most widespread adopted tool for atomic scale characterization of two-dimensional (2D) materials. However, damage free imaging of 2D materials with electrons has remained...


2021 ◽  
Vol 106 (1) ◽  
pp. 82-96 ◽  
Author(s):  
Lei Jin ◽  
Dimitrios Koulialias ◽  
Michael Schnedler ◽  
Andreas U. Gehring ◽  
Mihály Pósfai ◽  
...  

Abstract Pyrrhotites, characterized by the chemical formula Fe1–δS (0 < δ ≤ 1/8), represent an extended group of minerals that are derived from the NiAs-type FeS aristotype. They contain layered arrangements of ordered Fe vacancies, which are at the origin of the various magnetic signals registered from certain natural rocks and can act as efficient electrocatalysts in oxygen evolution reactions in ultrathin form. Despite extensive studies over the past century, the local structural details of pyrrhotite superstructures formed by different arrangements of Fe vacancies remain unclear, in particular at the atomic scale. Here, atomic-resolution high-angle annular dark-field imaging and nanobeam electron diffraction in the scanning transmission electron microscope are used to study natural pyrrhotite samples that contain commensurate 4C and incommensurate 4.91 ± 0.02C constituents. Local measurements of both the intensities and the picometer-scale shifts of individual Fe atomic columns are shown to be consistent with a model for the structure of 4C pyrrhotite, which was derived using X-ray diffraction by Tokonami et al. (1972). In 4.91 ± 0.02C pyrrhotite, 5C-like unequally sized nano-regions are found to join at anti-phase-like boundaries, leading to the incommensurability observed in the present pyrrhotite sample. This conclusion is supported by computer simulations. The local magnetic properties of each phase are inferred from the measurements. A discussion of perspectives for the quantitative counting of Fe vacancies at the atomic scale is presented.


2002 ◽  
Vol 8 (6) ◽  
pp. 475-486 ◽  
Author(s):  
Robert F. Klie ◽  
Nigel D. Browning

This article presents a comprehensive investigation of (La, Sr)FeO3 by correlated atomic resolution annular dark field imaging and electron energy loss spectroscopy. Here, the ability of these techniques to characterize point defect formation and phase transitions under reducing conditions in situ in the scanning transmission electron microscope is evaluated and the influence of oxygen vacancies on the structure–property relationships is discussed. In particular, the evolution of the Ruddlesden–Popper, Brownmillerite, and Aurivillius phases can be associated directly with the ionic and electronic conductivity of the bulk material under different thermodynamic conditions. These results lead naturally to an atomistic defect chemistry model to explain the high temperature ionic and electronic conductivity in this and other perovskite materials.


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.


2014 ◽  
Vol 1708 ◽  
Author(s):  
Nabraj Bhattarai ◽  
Subarna Khanal ◽  
Daniel Bahena ◽  
Robert L. Whetten ◽  
Miguel Jose-Yacaman

ABSTRACTThe synthesis of bimetallic magnetic nanoparticles is very challenging because of the agglomeration and non-uniform size. In this paper, we present the synthesis of monodispersed 3-5 nm sized thiolated bimetallic alloyed Au/Co nanoparticles with decahedral and icosahedral shape, their characterization using Cs-corrected scanning transmission electron microscopy (STEM) and magnetic measurements using superconducting quantum interference device (SQUID) magnetometer. The Z-contrast imaging and energy dispersive X-ray spectroscopy (EDS) mapping showed an inhomogeneous alloying with minor segregation between Au and Co at nanoscale and the SQUID measurement exhibited the ferromagnetic behavior.


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