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Introduction Evolution of WDS technique Basics of WDS Diffraction Crystals Detectors & Geometry Comparison of EDS and WDS Qualitative Analysis Quantitative Analysis Mapping Summary
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Detectors and Geometry
Detectors
Detectors used in WDS are usually
of the gas proportional counter type (Fig. 3). Generally, X-ray photons are
diffracted into the detector through a collimator (receiving slit), entering
the counter through a thin window. They are then absorbed by atoms of the
counter gas. A photoelectron is ejected from each atom absorbing an X-ray.
The photoelectrons are accelerated to the central wire causing further
ionization events in the gas, so that an “avalanche” of electrons drawn to
the wire produces an electrical pulse. The detector potential is set so that
the amplitude of this pulse is proportional to the energy of the X-ray
photon that started the process. Electronic pulse height analysis is
subsequently performed on the pulses to filter out noise. There are two
types of gas proportional counters: sealed (SPC) and gas flow (FPC).
Generally, SPCs are used for high-energy X-ray lines, while FPCs are used
for low energy lines. Sealed proportional counters have a relatively thick
window (i.e. beryllium, ~50µm thick), in order to prevent leakage of the gas
(usually xenon or a xenon-CO2 mixture) which is sealed into the detector.
Gas flow proportional counters commonly use ultrathin (0.5 -1µm thick) mylar
or polypropylene windows, and the counter gas (usually P-10: argon with 10%
methane) flows through the detector at a constant rate.
Spectrometer
geometry
To maintain the correct
geometrical relationship between specimen, crystal and detector for the full
range of diffracted angles, it is necessary to maintain all three on the
Rowland circle. This is accomplished by a mechanical goniometer which moves
the crystal and detector so that correct diffraction conditions are
maintained. If a spectrometer is mounted with the Rowland circle vertical
(as is typical on dedicated microprobes), it is necessary to position the
sample height very accurately to maintain diffraction geometry. This is
achieved by adjusting the height of the sample and observing focus using an
optical microscope. In the SEM, accurate vertical positioning is not
critical because the spectrometer is mounted with the Rowland circle
horizontal and inclined, thus eliminating the need for an optical
microscope. To analyze for a particular element it is important that the
crystal and detector are positioned accurately and associated counting
electronics are set up correctly. In the past this was a tedious and complex
procedure, but automation and PC control have made WD operation very
straightforward, routine and reliable.
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