Reduction in Radiation Damage at Low Temperature

Author(s):  
R. F. Egerton

Previous low-temperature measurements of radiation damage in organic materials have been based on the diffraction pattern, changes in total scattering power, background in the X-ray emission spectrum or the O - 10 eV region of electron energy-loss spectra. Here we observe instead the 200-600 eV region of the energy-loss spectrum, which contains information relating to the concentration of carbon, nitrogen and oxygen present in a thin sample. Specimens were irradiated by 80 keV electrons in a JEM IOOB transmission microscope fitted with a specially-constructed specimen holder which could be cooled to 77°K by circulation of liquid nitrogen. Cooled apertures above and below the specimen reduce heat radiation and possible condensation of residual gases from the surroundings. For the dose rates (<0.4 mA cm"2) and specimen thicknesses (< 50 nm) employed here, temperature rise due to the electron beam is expected to be negligible7.

Author(s):  
C P Scott ◽  
A J Craven ◽  
C J Gilmore ◽  
A W Bowen

The normal method of background subtraction in quantitative EELS analysis involves fitting an expression of the form I=AE-r to an energy window preceding the edge of interest; E is energy loss, A and r are fitting parameters. The calculated fit is then extrapolated under the edge, allowing the required signal to be extracted. In the case where the characteristic energy loss is small (E < 100eV), the background does not approximate to this simple form. One cause of this is multiple scattering. Even if the effects of multiple scattering are removed by deconvolution, it is not clear that the background from the recovered single scattering distribution follows this simple form, and, in any case, deconvolution can introduce artefacts.The above difficulties are particularly severe in the case of Al-Li alloys, where the Li K edge at ~52eV overlaps the Al L2,3 edge at ~72eV, and sharp plasmon peaks occur at intervals of ~15eV in the low loss region. An alternative background fitting technique, based on the work of Zanchi et al, has been tested on spectra taken from pure Al films, with a view to extending the analysis to Al-Li alloys.


Author(s):  
Hiroki Kurata ◽  
Kazuhiro Nagai ◽  
Seiji Isoda ◽  
Takashi Kobayashi

Electron energy loss spectra of transition metal oxides, which show various fine structures in inner shell edges, have been extensively studied. These structures and their positions are related to the oxidation state of metal ions. In this sence an influence of anions coordinated with the metal ions is very interesting. In the present work, we have investigated the energy loss near-edge structures (ELNES) of some iron compounds, i.e. oxides, chlorides, fluorides and potassium cyanides. In these compounds, Fe ions (Fe2+ or Fe3+) are octahedrally surrounded by six ligand anions and this means that the local symmetry around each iron is almost isotropic.EELS spectra were obtained using a JEM-2000FX with a Gatan Model-666 PEELS. The energy resolution was about leV which was mainly due to the energy spread of LaB6 -filament. The threshole energies of each edges were measured using a voltage scan module which was calibrated by setting the Ni L3 peak in NiO to an energy value of 853 eV.


Author(s):  
Eckhard Quandt ◽  
Stephan laBarré ◽  
Andreas Hartmann ◽  
Heinz Niedrig

Due to the development of semiconductor detectors with high spatial resolution -- e.g. charge coupled devices (CCDs) or photodiode arrays (PDAs) -- the parallel detection of electron energy loss spectra (EELS) has become an important alternative to serial registration. Using parallel detection for recording of energy spectroscopic large angle convergent beam patterns (LACBPs) special selected scattering vectors and small detection apertures lead to very low intensities. Therefore the very sensitive direct irradiation of a cooled linear PDA instead of the common combination of scintillator, fibre optic, and semiconductor has been investigated. In order to obtain a sufficient energy resolution the spectra are optionally magnified by a quadrupole-lens system.The detector used is a Hamamatsu S2304-512Q linear PDA with 512 diodes and removed quartz-glas window. The sensor size is 13 μm ∗ 2.5 mm with an element spacing of 25 μm. Along with the dispersion of 3.5 μm/eV at 40 keV the maximum energy resolution is limited to about 7 eV, so that a magnification system should be attached for experiments requiring a better resolution.


1992 ◽  
Vol 259 ◽  
Author(s):  
Selmer S. Wong ◽  
Shouleh Nikzad ◽  
Channing C. Ahn ◽  
Aimee L. Smith ◽  
Harry A. Atwater

ABSTRACTWe have employed reflection electron energy loss spectrometry (REELS), a surface chemical analysis technique, in order to analyze contaminant coverages at the submonolayer level during low-temperature in situ cleaning of hydrogen-terminated Si(100). The chemical composition of the surface was analyzed by measurements of the C K, O K and Si L2,3 core loss intensities at various stages of the cleaning. These results were quantified using SiC(100) and SiO2 as reference standards for C and O coverage. Room temperature REELS core loss intensity analysis after sample insertion reveals carbon at fractional monolayer coverage. We have established the REELS detection limit for carbon coverage to be 5±2% of a monolayer. A study of temperature-dependent hydrocarbon desorption from hydrogen-terminated Si(100) reveals the absence of carbon on the surface at temperatures greater than 200°C. This indicates the feasibility of epitaxial growth following an in situ low-temperature cleaning and also indicates the power of REELS as an in situ technique for assessment of surface cleanliness.


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