scholarly journals Electron energy-loss spectroscopic tomography of FexCo(3−x)O4 impregnated Co3O4 mesoporous particles: unraveling the chemical information in three dimensions

The Analyst ◽  
2016 ◽  
Vol 141 (16) ◽  
pp. 4968-4972 ◽  
Author(s):  
L. Yedra ◽  
A. Eljarrat ◽  
R. Arenal ◽  
L. López-Conesa ◽  
E. Pellicer ◽  
...  

Electron energy-loss spectroscopy-spectrum image (EELS-SI) tomography is a powerful tool to investigate the three dimensional chemical configuration in nanostructures.

2017 ◽  
Vol 8 (45) ◽  
pp. 6927-6937 ◽  
Author(s):  
Ruchi Pal ◽  
Arun K. Sikder ◽  
Kei Saito ◽  
Alison M. Funston ◽  
Jayesh R. Bellare

Electron energy loss spectroscopy (EELS) allows imaging as well as extraction of spatially resolved chemical information and this review presents how EELS can be ap plied to polymeric systems.


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.


2013 ◽  
Vol 19 (4) ◽  
pp. 1036-1049 ◽  
Author(s):  
Huolin L. Xin ◽  
Christian Dwyer ◽  
David A. Muller ◽  
Haimei Zheng ◽  
Peter Ercius

AbstractFinding a faster alternative to tilt-series electron tomography is critical for rapidly evolving fields such as the semiconductor industry, where failure analysis could greatly benefit from higher throughput. We present a theoretical and experimental evaluation of scanning confocal electron energy-loss microscopy (SCEELM) using valence-loss signals, which is a promising technique for the reliable reconstruction of materials with sub-10-nm resolution. Such a confocal geometry transfers information from the focused portion of the electron beam and enables rapid three-dimensional (3D) reconstruction by depth sectioning. SCEELM can minimize or eliminate the missing-information cone and the elongation problem that are associated with other depth-sectioning image techniques in a transmission electron microscope. Valence-loss SCEELM data acquisition is an order of magnitude faster and requires little postprocessing compared with tilt-series electron tomography. With postspecimen chromatic aberration (Cc) correction, SCEELM signals can be acquired in parallel in the direction of energy dispersion with the aid of a physical pinhole. This increases the efficiency by 10×–100×, and can provide 3D resolved chemical information for multiple core-loss signals simultaneously.


Author(s):  
Ondrej L. Krivanek ◽  
Chris E. Meyer ◽  
Marcel Tencé

Elemental maps, that is images showing the concentration of different elements in a sample, can be obtained in an electron microscope equipped with an electron energy-loss spectrometer (EELS) by acquiring and processing data in three dimensions: spatial coordinates x and y, and the energy loss ΔE. Since the electron detector is necessarily at most a two-dimensional one, acquiring all the required data at the same time is not possible. Instead, one can either use an imaging electron spectrometer and acquire a series of whole images at one energy at a time, or use a small probe in a scanning-transmission electron microscope (STEM), and acquire the data image-point by image-point. With a serial-detection spectrometer the data at each image-point must be recorded sequentially, while with a parallel-detection spectrometer a whole spectrum can be recorded at the same time.The two approaches are illustrated schematically in figure 1. The individual sampling points in the three- dimensional volume have been called voxels (by analogy with two-dimensional pixels).


Author(s):  
R. M. Briber

Analytical electron microscopy has progressed in recent years such that quantitative chemical information can be obtained from very small volumes of sample. In principle, the composition of regions on the order of a few namometers in both diameter and thickness can be determined using energy dispersive x-ray analysis (EDS) and electron energy loss spectroscopy (EELS) [1,2], In the case of organic polymers the limitations to quantitative microanalysis are generally due to the sample and not to the instrument. Radiation damage induced mass loss often proves to be the constraining factor in obtaining quantitative information from small volumes of sample [3], The principles and processes of radiation damage in organic materials and polymers can be found in various review articles [4,5].The principles underlying both analytical x-ray spectroscopy and electron energy loss spectroscopy are closely related. When an electron in the incident beam loses energy (i.e. inelastically scattered) by "knocking" out an inner shell electron from an atom present in the sample there are two aspects that are of value for compositional analysis.


Author(s):  
P. Trebbia ◽  
P. Ballongue ◽  
C. Colliex

An effective use of electron energy loss spectroscopy for chemical characterization of selected areas in the electron microscope can only be achieved with the development of quantitative measurements capabilities.The experimental assembly, which is sketched in Fig.l, has therefore been carried out. It comprises four main elements.The analytical transmission electron microscope is a conventional microscope fitted with a Castaing and Henry dispersive unit (magnetic prism and electrostatic mirror). Recent modifications include the improvement of the vacuum in the specimen chamber (below 10-6 torr) and the adaptation of a new electrostatic mirror.The detection system, similar to the one described by Hermann et al (1), is located in a separate chamber below the fluorescent screen which visualizes the energy loss spectrum. Variable apertures select the electrons, which have lost an energy AE within an energy window smaller than 1 eV, in front of a surface barrier solid state detector RTC BPY 52 100 S.Q. The saw tooth signal delivered by a charge sensitive preamplifier (decay time of 5.10-5 S) is amplified, shaped into a gaussian profile through an active filter and counted by a single channel analyser.


Author(s):  
C. Colliex ◽  
P. Trebbia

The physical foundations for the use of electron energy loss spectroscopy towards analytical purposes, seem now rather well established and have been extensively discussed through recent publications. In this brief review we intend only to mention most recent developments in this field, which became available to our knowledge. We derive also some lines of discussion to define more clearly the limits of this analytical technique in materials science problems.The spectral information carried in both low ( 0<ΔE<100eV ) and high ( >100eV ) energy regions of the loss spectrum, is capable to provide quantitative results. Spectrometers have therefore been designed to work with all kinds of electron microscopes and to cover large energy ranges for the detection of inelastically scattered electrons (for instance the L-edge of molybdenum at 2500eV has been measured by van Zuylen with primary electrons of 80 kV). It is rather easy to fix a post-specimen magnetic optics on a STEM, but Crewe has recently underlined that great care should be devoted to optimize the collecting power and the energy resolution of the whole system.


Author(s):  
R. F. Egerton

An important parameter governing the sensitivity and accuracy of elemental analysis by electron energy-loss spectroscopy (EELS) or by X-ray emission spectroscopy is the signal/noise ratio of the characteristic signal.


Author(s):  
R.D. Leapman ◽  
C.R. Swyt

The intensity of a characteristic electron energy loss spectroscopy (EELS) image does not, in general, directly reflect the elemental concentration. In fact, the raw core loss image can give a misleading impression of the elemental distribution. This is because the measured core edge signal depends on the amount of plural scattering which can vary significantly from region to region in a sample. Here, we show how the method for quantifying spectra due to Egerton et al. can be extended to maps.


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