Analysis of the Atomic-Scale Defect Chemistry at Interfaces in Fluorite Structured Oxides by Electron Energy Loss Spectroscopy

2001 ◽  
Vol 703 ◽  
Author(s):  
Y. Ito ◽  
Y Lei ◽  
N.D. Browning ◽  
T.J. Mazanec

ABSTRACTGd3+ doped Ce oxides are a major candidate for use as the electrolyte in solid oxide fuel cells operating at ∼500 °C. Here, the effect of the atomic structure on the local electronic properties, i.e. oxygen coordination and cation valence, at grain boundaries in the fluorite structured Gd0.2Ce0.8O2-x ceramic electrolyte is investigated by a combination of atomic resolution Z-contrast imaging and electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM). In particular, EELS analyses from grain boundaries reveals a complex interaction between segregation of the dopant (Gd3+), oxygen vacancies and the valence state of Ce. These results are similar to observations from fluorite-structured Yttria-Stabilized Zirconium (YSZ) bicrystal grain boundaries.

1993 ◽  
Vol 319 ◽  
Author(s):  
M.M. Mcgibbon ◽  
N.D. Browning ◽  
M.F. Chisholm ◽  
S.J. Pennycook ◽  
V. Ravikumar ◽  
...  

AbstractThe macroscopic properties of many materials are controlled by the structure and chemistry at grain boundaries. A basic understanding of the structure-property relationship requires a technique which probes both composition and chemical bonding on an atomic scale. The high-resolution Z-contrast imaging technique in the scanning transmission electron microscope (STEM) forms an incoherent image in which changes in atomic structure and composition can be interpreted intuitively. This direct image allows the electron probe to be positioned over individual atomic columns for parallel detection electron energy loss spectroscopy (EELS) at a spatial resolution approaching 0.22nm. In this paper we have combined the structural information available in the Z-contrast images with the bonding information obtained from the fine structure within the EELS edges to determine the grain boundary structure in a SrTiO3 bicrystal.


1994 ◽  
Vol 341 ◽  
Author(s):  
M. M. McGibbon ◽  
N. D. Browning ◽  
M. F. Chisholm ◽  
A. J. McGibbon ◽  
S. J. Pennycook ◽  
...  

AbstractThe macroscopic properties of many materials are controlled by the structure and chemistry at grain boundaries. A basic understanding of the structure-property relationship requires a technique which probes both composition and chemical bonding on an atomic scale. High-resolution Z-contrast imaging in the scanning transmission electron microscope (STEM) forms an incoherent image in which changes in atomic structure and composition across an interface can be interpreted directly without the need for preconceived atomic structure models (1). Since the Z-contrast image is formed by electrons scattered through high angles, parallel detection electron energy loss spectroscopy (PEELS) can be used simultaneously to provide complementary chemical information on an atomic scale (2). The fine structure in the PEEL spectra can be used to investigate the local electronic structure and the nature of the bonding across the interface (3). In this paper we use the complimentary techniques of high resolution Zcontrast imaging and PEELS to investigate the atomic structure and chemistry of a 25° symmetric tilt boundary in a bicrystal of the electroceramic SrTiO3.


2000 ◽  
Vol 07 (04) ◽  
pp. 475-494 ◽  
Author(s):  
O. STÉPHAN ◽  
A. GLOTER ◽  
D. IMHOFF ◽  
M. KOCIAK ◽  
C. MORY ◽  
...  

The basics of electron energy loss spectroscopy (EELS) performed in the context of a scanning transmission electron microscope are described. This includes instrumentation, information contained in an EELS spectrum, data acquisition and processing, and some illustrations by a few examples.


Author(s):  
H.S. von Harrach ◽  
J.A. Colling

A UHV-compatible parallel and serial detection system for electron energy-loss spectroscopy (EELS) has been developed for the VG HB501 field-emission scanning transmission electron microscope (STEM) using a 2-dimensional detector. As pointed out previously the charge coupled devices (CCD) available commercially are vastly superior, in terms of read-out noise, to linear photodiode arrays which are currently used for parallel EELS detection. This feature, together with the ability of operating as an imaging and storage device, makes the 2-dimensional CCD array an attractive choice for parallel EELS and low light-level imaging applications.The system reported here (Fig. 1) is an extension of the VG ELS501 sector magnetspectrometer used for serial EELS with many STEMS. It uses one quadrupole lens to magnify the energy-loss spectrum over a range of 2 to 0.1 eV per detector element. An electromagnetic deflector steers the spectrum to one of three YAG scintillators. Two of these scintillators with suitable masks are used for parallel EELS detection; the third is used for serial EELS and energy filtered STEM imaging via a lightguide and photomultiplier system by scanning the beam across a variable slit as in ELS 501 systems.


1997 ◽  
Vol 3 (S2) ◽  
pp. 871-872
Author(s):  
R.D. Leapman ◽  
S.B. Andrews

Perhaps the ultimate aim of analytical electron microscopy in biology is to detect single atoms or ions bound to isolated macromolecular assemblies and small cellular organelles rapidly frozen in their native state. Although the meaningful spatial resolution in such analyses is limited to ∽10 nm or more by radiation damage, the high intrinsic sensitivity of electron energy-loss spectroscopy (EELS) coupled with recent developments seems to make this rather ambitious goal—originally proposed some twenty years ago—within reach. Here we describe examples where EELS has been able to detect surprisingly small numbers of atoms in biological specimens and discuss some fundamental limits that are encountered as well as some possible strategies for circumventing these difficulties.In our laboratory we have used a scanning transmission electron microscope (STEM) equipped with a field-emission source and parallel-detection EELS because the probe size and collection efficiency of this instrument are optimized to give the lowest detectable number of atoms and lowest detectable atomic fraction.


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

The recent development of the Z-contrast imaging technique for the VG HB501 UX dedicated STEM, has added a high-resolution imaging facility to a microscope used mainly for microanalysis. This imaging technique not only provides a high-resolution reference image, but as it can be performed simultaneously with electron energy loss spectroscopy (EELS), can be used to position the electron probe at the atomic scale. The spatial resolution of both the image and the energy loss spectrum can be identical, and in principle limited only by the 2.2 Å probe size of the microscope. There now exists, therefore, the possibility to perform chemical analysis of materials on the scale of single atomic columns or planes.In order to achieve atomic resolution energy loss spectroscopy, the range over which a fast electron can cause a particular excitation event, must be less than the interatomic spacing. This range is described classically by the impact parameter, b, which ranges from ~10 Å for the low loss region of the spectrum to <1Å for the core losses.


Sign in / Sign up

Export Citation Format

Share Document