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Introduction Fundamentals of the TEM technique Beam-sample interaction The Analytical TEM Detector Protection Qualitative Analysis Quantitative Analysis Microanalysis Examples (1) Microanalysis Examples (2) Microanalysis Examples (3) Summary
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Qualitative Analysis in the AEM
Many analytical observations in the AEM are qualitative. Often, it is only
necessary to distinguish between phases and it is not necessary to calculate
elemental concentrations. Spectra may be collected at up to 0 - 40 keV range
as this aids in the identification of K lines of elements that may have
overlapping L or M peaks in a lower range e.g. Pb and Mo. It is easier to
detect small peaks from minor elements when the background is smooth.
Counting for longer periods of time increases total counts, which reduces
statistical scatter in the background. Increased counts can also be achieved
by increasing probe current or analyzing thicker parts of the specimen,
although this involves some sacrifice in spatial resolution. Peak visibility
is improved by having good detector resolution, which improves peak to
background. To avoid false identifications, spurious peaks need to be
eliminated by good collimation and design of sample holder.
The limit of
detectability for an element, expressed as the minimum mass fraction (MMF),
depends on the other elements present in the sample, microscope kV, detector
resolution and the number of counts recorded in the spectrum. The MMF is
usually calculated as the largest concentration that could be attributed to
statistical fluctuations alone. By reducing statistical fluctuations, the
MMF is improved. In a TEM, the total volume of material analyzed is
determined by the probe diameter and specimen thickness. Therefore the total
mass of material excited by the probe can be very small and masses as small
as 10-19g can be measured with EDS.
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