Fe valence determination and Li elemental distribution in lithiated FeO0.7F1.3/C nanocomposite battery materials by electron energy loss spectroscopy (EELS)

Micron ◽  
2012 ◽  
Vol 43 (1) ◽  
pp. 22-29 ◽  
Author(s):  
F. Cosandey ◽  
D. Su ◽  
M. Sina ◽  
N. Pereira ◽  
G.G. Amatucci
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.


Author(s):  
Zhifeng Shao ◽  
Ruoya Ho ◽  
Andrew P. Somlyo

Electron energy loss spectroscopy (EELS) has been a powerful tool for high resolution studies of elemental distribution, as well as electronic structure, in thin samples. Its foundation for biological research has been laid out nearly two decades ago, and in the subsequent years it has been subjected to rigorous, but by no means extensive research. In particular, some problems unique to EELS of biological samples, have not been fully resolved. In this article we present a brief summary of recent methodological developments, related to biological applications of EELS, in our laboratory. The main purpose of this work was to maximize the signal to noise ratio (S/N) for trace elemental analysis at a minimum dose, in order to reduce the electron dose and/or time required for the acquisition of high resolution elemental maps of radiation sensitive biological materials.Based on the simple assumption of Poisson distribution of independently scattered electrons, it had been generally assumed that the optimum specimen thickness, at which the S/N is a maximum, must be the total inelastic mean free path of the beam electron in the sample.


2018 ◽  
Vol 24 (3) ◽  
pp. 214-220 ◽  
Author(s):  
Fernando C. Castro ◽  
Vinayak P. Dravid

AbstractCutting-edge research on materials for lithium ion batteries regularly focuses on nanoscale and atomic-scale phenomena. Electron energy-loss spectroscopy (EELS) is one of the most powerful ways of characterizing composition and aspects of the electronic structure of battery materials, particularly lithium and the transition metal mixed oxides found in the electrodes. However, the characteristic EELS signal from battery materials is challenging to analyze when there is strong overlap of spectral features, poor signal-to-background ratios, or thicker and uneven sample areas. A potential alternative or complementary approach comes from utilizing the valence EELS features (<20 eV loss) of battery materials. For example, the valence EELS features in LiCoO2 maintain higher jump ratios than the Li–K edge, most notably when spectra are collected with minimal acquisition times or from thick sample regions. EELS maps of these valence features give comparable results to the Li–K edge EELS maps of LiCoO2. With some spectral processing, the valence EELS maps more accurately highlight the morphology and distribution of LiCoO2 than the Li–K edge maps, especially in thicker sample regions. This approach is beneficial for cases where sample thickness or beam sensitivity limit EELS analysis, and could be used to minimize electron dosage and sample damage or contamination.


2010 ◽  
Vol 16 (S2) ◽  
pp. 1440-1441 ◽  
Author(s):  
KS Rao ◽  
N Pereira ◽  
G Amatucci ◽  
F Cosandey

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.


Author(s):  
H. Shuman

The distribution of elements in thin biological specimens can be determined at high resolution with electron energy loss spectroscopy (EELS). The advantage of EELS is that the signal is large, since roughly 50% of the characteristic ionization events can be observed, but this is accompanied by difficulties related to the generally large background and the more stringent requirements for ultrathin specimens in EELS than in electron probe X-ray microanalysis. Therefore it is generally necessary to use signal processing methods to extract absorption edge information in EELS.EELS can be used in two ways: to produce line spectra with a stationary or rastered probe, or to directly form energy-filtered electron microscope (EFEM) images representative of the elemental distribution.


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):  
David C. Joy ◽  
Suichu Luo ◽  
John R. Dunlap ◽  
Dick Williams ◽  
Siqi Cao

In Physics, Chemistry, Materials Science, Biology and Medicine, it is very important to have accurate information about the stopping power of various media for electrons, that is the average energy loss per unit pathlength due to inelastic Coulomb collisions with atomic electrons of the specimen along their trajectories. Techniques such as photoemission spectroscopy, Auger electron spectroscopy, and electron energy loss spectroscopy have been used in the measurements of electron-solid interaction. In this paper we present a comprehensive technique which combines experimental and theoretical work to determine the electron stopping power for various materials by electron energy loss spectroscopy (EELS ). As an example, we measured stopping power for Si, C, and their compound SiC. The method, results and discussion are described briefly as below.The stopping power calculation is based on the modified Bethe formula at low energy:where Neff and Ieff are the effective values of the mean ionization potential, and the number of electrons participating in the process respectively. Neff and Ieff can be obtained from the sum rule relations as we discussed before3 using the energy loss function Im(−1/ε).


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.


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