Inner Shell Ionization by 60 keV Electrons, Application to Microanalysis

Author(s):  
Y. Kihn ◽  
J. Sevely ◽  
B. Jouffrey

By using a Castaing-Henry filtering device adapted on a Siemens Elmiskop I electron microscope, we have directly observed plasmon and inner shell excitations by 60 keV electrons on electron energy loss spectra. Inner shell excitation edges have been detected up to 1900 eV.By comparing L and K inner shell excitation profiles in the case of Magnesium, Aluminium and Silicon, it is concluded that the optical selection rules, △1 = ±1, explain the shape of the spectrum after the edge in a first approximation.

Author(s):  
J. Bentley ◽  
G. L. Lehman ◽  
P. S. Sklad

Microanalysis using inner shell ionization edges in electron energy loss spectra obtained in an analytical electron microscope is now well established. In order to assess true edge profiles and obtain integrated intensities of the inner shell ionization edges of interest, it is first necessary to subtract the background. The background arises from the tails of preceding ionization edges, multiple plasmon excitations and valence electron excitations.


Author(s):  
John J. Godleski ◽  
Rebecca C. Stearns ◽  
Emil J. Millet

The Zeiss CEM902, energy filtering electron microscope, can be used to image the structure of unstained 30 nm sections of biologic materials, to image the distribution of selected elements in such sections, and to determine electron energy loss spectra (EELS) of elements in areas as small as 10 nm. Although the integrated computer in the latest version of the CEM902 can collect and display signals from the scintillation detector for recording EELS, our instrument did not have this capability. Therefore, we have added a Leading Edge Model D personal computer with a 20 Mbyte hard disk, Hercules compatible graphics display adapter, and a programmable gain analog to digital converter board (Metrabyte DAS16-G1) to collect and analyze voltage signals corresponding to changes in accelerating voltage and changes in the signal from the photomultiplier tube (PMT) of the scintillation detector. With this board, the gain on the PMT channel is dynamically adjusted for optimal resolution. Software is designed to monitor and display voltages, store data on the hard disk, display spectra with adjustable axes, as well as subtract spectra and determine areas beneath regions of interest.Canine alveolar macrophages with ingested cobalt oxide particles were fixed with 2.5% glutaraldehyde in 0.164M phosphate buffer, post-fixed in 1% OsO4 in 0.lM Na cacodylate buffer, dehydrated through alcohols, embedded in araldite, and sectioned at 30nm. Sections were assessed with our CEM902 as described above. The spectral range of 500 to 900 electron volts while focused on acobalt oxide particle at 20,000x is illustrated in Figure 1 .


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):  
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.


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