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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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Evolution of the WDS technique
The development
of WD spectrometers goes back long before ED detectors became widely
available in the early 1970s.
The first
electron probe microanalyzer (EPMA) was developed during the 1940s and used
an optical microscope to observe the position and focus of the electron beam
on the sample. Later, WD spectrometers were fitted to SEMs which allowed the
specimen to be positioned more precisely under the electron beam and also
made possible a visual picture of the distribution of a chosen element – the
X-ray map.
On early
commercial WDS spectrometers, all of the spectrometer mechanisms had to be
moved by hand, and the operator had to physically exchange the crystals to
cover the spectrum. The output from counters, recorded against time was sent
to a chart recorder, and all the peak identification, peak and background
measurements, and matrix corrections were done by hand.
The advent of
desktop computers and precision stepper motors in the late 1970s made
possible the mechanization of the spectrometer and the SEM stage. With these
changes, WDS analysis became significantly less cumbersome. However, the
initial setup for an analysis and the entire data reduction process were
still tedious and time-consuming. Analysis parameters had to be optimized
for each element and type of sample. Computers of that generation were not
particularly user-friendly. Data for ED and WD were beginning to be
combined, but automatic peak identification of the ED spectrum was not
routine, and combined ED and WD analyses were unduly complicated. The
situation changed somewhat in the mid-1980s, when data processing became
fully automated. However, setup for the analysis remained virtually
unchanged.
The
current generation of WDS spectrometers with their advanced control and
analysis software make the technique considerably easier to use.
Multi-crystal spectrometers now change crystals on-the-fly rather than first
moving to a specified position on the Rowland circle, flipping to the
appropriate crystal, and moving back to the correct position on the circle
for analysis of the desired element. Software has been developed for quick,
easy qualitative analysis by WDS. Operating parameters for the detectors
have been optimized and entered into the software so that analysis setup is
quick for the vast majority of samples. Comparing WD and ED spectra and
combining WD and ED analysis is now routine and easy.
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