A New Numerical Model for Electron-Probe Analysis at High Depth Resolution

Author(s):  
P.-F. Staub ◽  
C. Bonnelle ◽  
F. Vergand ◽  
P. Jonnard

Characterizing dimensionally and chemically nanometric structures such as surface segregation or interface phases can be performed efficiently using electron probe (EP) techniques at very low excitation conditions, i.e. using small incident energies (0.5<E0<5 keV) and low incident overvoltages (1<U0<1.7). In such extreme conditions, classical analytical EP models are generally pushed to their validity limits in terms of accuracy and physical consistency, and Monte-Carlo simulations are not convenient solutions as routine tools, because of their cost in computing time. In this context, we have developed an intermediate procedure, called IntriX, in which the ionization depth distributions Φ(ρz) are numerically reconstructed by integration of basic macroscopic physical parameters describing the electron beam/matter interaction, all of them being available under pre-established analytical forms. IntriX’s procedure consists in dividing the ionization depth distribution into three separate contributions:

Author(s):  
Claude Merlet

In the last ten years the development of new X-ray depth distribution models in electron probe microanalysis (EPMA), has allowed to obtain accurate quantitative programs for stratified and massive samples. With these new quantitative methods, for the energy lines greater than 1keV and for massive samples, the results of the quantification are independent of the accelerating voltage (for an excited line). Nevertheless, for light elements, and for soft X-ray emission in complexe compounds, the choice of these optimum experimental conditions is not trivial. Moreover, the physical parameters and boundary conditions of the measurements are not well known.In an attempt to choose the optimum accelerating voltage, and to solve some difficulties in the quantification of low energy lines, a software (freeware) has been developed on PC and under the WINDOWS operating system. The calculation procedure is based upon the double partial gaussian profile ϕ(ρz) (recently developed for massive compounds). This description, flexible, precise and mathematically simple allows to compute rapidly the X-ray intensities. The program, which has been designed mainly for WDS electron probe, uses graphic simulations, and includes two sections:


Author(s):  
A. V. Somlyo ◽  
H. Shuman ◽  
A. P. Somlyo

Electron probe analysis of frozen dried cryosections of frog skeletal muscle, rabbit vascular smooth muscle and of isolated, hyperpermeab1 e rabbit cardiac myocytes has been used to determine the composition of the cytoplasm and organelles in the resting state as well as during contraction. The concentration of elements within the organelles reflects the permeabilities of the organelle membranes to the cytoplasmic ions as well as binding sites. The measurements of [Ca] in the sarcoplasmic reticulum (SR) and mitochondria at rest and during contraction, have direct bearing on their role as release and/or storage sites for Ca in situ.


Author(s):  
Delbert E. Philpott ◽  
David Leaffer

There are certain advantages for electron probe analysis if the sample can be tilted directly towards the detector. The count rate is higher, it optimizes the geometry since only one angle need be taken into account for quantitative analysis and the signal to background ratio is improved. The need for less tilt angle may be an advantage because the grid bars are not moved quite as close to each other, leaving a little more open area for observation. Our present detector (EDAX) and microscope (Philips 300) combination precludes moving the detector behind the microscope where it would point directly at the grid. Therefore, the angle of the specimen was changed in order to optimize the geometry between the specimen and the detector.


Author(s):  
Avril V. Somlyo ◽  
H. Shuman ◽  
A.P. Somlyo

This is a preliminary report of electron probe analysis of rabbit portal-anterior mesenteric vein (PAMV) smooth muscle cryosectioned without fixation or cryoprotection. The instrumentation and method of electron probe quantitation used (1) and our initial results with cardiac (2) and skeletal (3) muscle have been presented elsewhere.In preparations depolarized with high K (K2SO4) solution, significant calcium peaks were detected over the sarcoplasmic reticulum (Fig 1 and 2) and the continuous perinuclear space. In some of the fibers there were also significant (up to 200 mM/kg dry wt) calcium peaks over the mitochondria. However, in smooth muscle that was not depolarized, high mitochondrial Ca was found in fibers that also contained elevated Na and low K (Fig 3). Therefore, the possibility that these Ca-loaded mitochondria are indicative of cell damage remains to be ruled out.


Author(s):  
S.F. Corcoran

Over the past decade secondary ion mass spectrometry (SIMS) has played an increasingly important role in the characterization of electronic materials and devices. The ability of SIMS to provide part per million detection sensitivity for most elements while maintaining excellent depth resolution has made this technique indispensable in the semiconductor industry. Today SIMS is used extensively in the characterization of dopant profiles, thin film analysis, and trace analysis in bulk materials. The SIMS technique also lends itself to 2-D and 3-D imaging via either the use of stigmatic ion optics or small diameter primary beams.By far the most common application of SIMS is the determination of the depth distribution of dopants (B, As, P) intentionally introduced into semiconductor materials via ion implantation or epitaxial growth. Such measurements are critical since the dopant concentration and depth distribution can seriously affect the performance of a semiconductor device. In a typical depth profile analysis, keV ion sputtering is used to remove successive layers the sample.


Author(s):  
R. Packwood ◽  
M.W. Phaneuf ◽  
V. Weatherall ◽  
I. Bassignana

The development of specialized analytical instruments such as the SIMS, XPS, ISS etc., all with truly incredible abilities in certain areas, has given rise to the notion that electron probe microanalysis (EPMA) is an old fashioned and rather inadequate technique, and one that is of little or no use in such high technology fields as the semiconductor industry. Whilst it is true that the microprobe does not possess parts-per-billion sensitivity (ppb) or monolayer depth resolution it is also true that many times these extremes of performance are not essential and that a few tens of parts-per-million (ppm) and a few tens of nanometers depth resolution is all that is required. In fact, the microprobe may well be the second choice method for a wide range of analytical problems and even the method of choice for a few.The literature is replete with remarks that suggest the writer is confusing an SEM-EDXS combination with an instrument such as the Cameca SX-50. Even where this confusion does not exist, the literature discusses microprobe detection limits that are seldom stated to be as low as 100 ppm, whereas there are numerous element combinations for which 10-20 ppm is routinely attainable.


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