Electron Spectroscopy for Studying Chemical Bonding

1969 ◽  
Vol 13 ◽  
pp. 390-405 ◽  
Author(s):  
Ragnar Nordberg

The results reviewed in this article were obtained by means of the ESCA technique at the Institute of Physics, University of Uppsala, Uppsala, Sweden and at the Department of Physics, Vanderbilt University, Nashville, Tennessee, USA.The ESCA technique is basically the study of induced emission of photo and Auger electrons from a sample irradiated with x-rays. If the incident radiation is monochromatic (e.g. an x-ray emission line) the spectrum of these electrons gives precise information about the energy states of the electrons in the sample. To extract this information, high resolution electron spectroscopy is necessary. Instruments for such spectroscopy have therefore been extensively developed during the last decade.

1990 ◽  
Vol 34 ◽  
pp. 123-130 ◽  
Author(s):  
Tom Scimeca ◽  
Sei Fukushima ◽  
Kazuo Miyamura ◽  
Yohichi Gohshi

High resolution X-Ray Fluorescence Spectroscopy(HRXRFS) has been extensively used as a chemical bonding probe for both solids and gases for quite some time. However there have been virtually no HRXRFS studies reported on liquid phase systems and particularly on solution systems. This seems somewhat surprising not only because this is an unexplored area, but because much of chemistry and chemical bonding occurs in solution. Furthermore, since HRXRFS is a “photon in - photon out” technique, providing one uses relatively energetic x-rays, the experimental techniques for performing these types of measurements are relatively straightforward, especially when compared to techniques which utilize charged particles.


Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.


Author(s):  
Y. Y. Wang ◽  
H. Zhang ◽  
V. P. Dravid ◽  
H. Zhang ◽  
L. D. Marks ◽  
...  

Azuma et al. observed planar defects in a high pressure synthesized infinitelayer compound (i.e. ACuO2 (A=cation)), which exhibits superconductivity at ~110 K. It was proposed that the defects are cation deficient and that the superconductivity in this material is related to the planar defects. In this report, we present quantitative analysis of the planar defects utilizing nanometer probe xray microanalysis, high resolution electron microscopy, and image simulation to determine the chemical composition and atomic structure of the planar defects. We propose an atomic structure model for the planar defects.Infinite-layer samples with the nominal chemical formula, (Sr1-xCax)yCuO2 (x=0.3; y=0.9,1.0,1.1), were prepared using solid state synthesized low pressure forms of (Sr1-xCax)CuO2 with additions of CuO or (Sr1-xCax)2CuO3, followed by a high pressure treatment.Quantitative x-ray microanalysis, with a 1 nm probe, was performed using a cold field emission gun TEM (Hitachi HF-2000) equipped with an Oxford Pentafet thin-window x-ray detector. The probe was positioned on the planar defects, which has a 0.74 nm width, and x-ray emission spectra from the defects were compared with those obtained from vicinity regions.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


1998 ◽  
Vol 5 (3) ◽  
pp. 515-517 ◽  
Author(s):  
M. Frank ◽  
C. A. Mears ◽  
S. E. Labov ◽  
L. J. Hiller ◽  
J. B. le Grand ◽  
...  

Experimental results are presented obtained with a cryogenically cooled high-resolution X-ray spectrometer based on a 141 × 141 µm Nb-Al-Al2O3-Al-Nb superconducting tunnel junction (STJ) detector in an SR-XRF demonstration experiment. STJ detectors can operate at count rates approaching those of semiconductor detectors while still providing a significantly better energy resolution for soft X-rays. By measuring fluorescence X-rays from samples containing transition metals and low-Z elements, an FWHM energy resolution of 6–15 eV for X-rays in the energy range 180–1100 eV has been obtained. The results show that, in the near future, STJ detectors may prove very useful in XRF and microanalysis applications.


2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.


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