X-ray Detector & EDS Comparisons in SEM/TEM/STEM
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The X-ray detector crystal is behind the EDS detector window, and is commonly made up of a lithium (Li) impregnated silicon (Si) wafer that is maintained at cold temperatures by liquid nitrogen (N2) stored in a Dewar located on the outside of the microscope.

The main requirements of EDS detectors for EMs are:
         i) Detect the entire energy range of x-rays, namely from 50 eV (Li-K) to incident beam energy of the microscope.
            i.a) For SEMs, the energy range of X-rays is up to 30 keV.
            i.b) For (S)TEMs with accelerating voltages up to 300 keV, the realistic energy range of X-rays is up to 50 keV.
         ii) High x-ray detection rates, resulting in reduced collection times.
         iii) Optimized physical geometry to maximize the x-ray collection by shortening the specimen-to-detector distance and leaving enough physical room for other detectors and accessories.

The background counts in TEM-EDS are much lower than those in SEM-EDS spectrum. Due to the high background counts in SEM-EDS, an artificial carbon (C) peak is always visible and thus a value of more than 2% carbon is normally measured even though there is no carbon in the specimen. This artefact is due to the window in the detector. The EDS windows are normally SATW windows and their material has a specific transmission profile with a strong absorption edge just above but very close to the C X-ray energy, resulting in an artificial peak at the C energy position. Therefore, it is the strong absorption of the background (continuum) X-rays that produces the artefact peak. Note that SATW detector windows are AP* ultrathin polymer windows manufactured by Moxtek and are almost supplied by all EDS detector companies. However, a TEM-EDS spectrum taken from the same specimen materials does not show such a artefact peak at the carbon energy because the spectrum consists mostly of characteristic X-rays.

Table 4532 lists the main reasons why EDS measurements in low-energy SEM or high-energy (S)TEM have not replaced each other.

Table 4532. Comparison between the EDS measurements in low-energy SEM and high-energy (S)TEM*.

Low-energy SEM
High-energy (S)TEM
Take-off angle
30 - 45° (for side-entry detectors) 11 - 26° (for side-entry detectors)
Spatial resolution
Greater than the probe size due to scattering of the beam in a thick specimen High: the same as the electron probe size due to thin TEM specimen and much higher energy of incident beam
Depth information
Is possible using various excitation voltages and modeling techniques such as Monte Carlo simulations Is impossible
X-ray generation
More Less
Count rate
High due to bulk materials Low due to thin film
Electron scattering
More Less
Background counts
High Low
Artificial peaks
More Less
Number of peaks in spectrum
Less due to lower accelerating voltages More due to higher accelerating voltages
Peak intensities
(Very) complicated, related to atomic-number, absorption effect, and fluorescence effect. (see page1746 and page1745). Very simple, just proportional to concentration and specimen thickness
Bremsstrahlung

Bremsstrahlung X-rays

For thin films in (S)TEM mode, the maximum of Bremsstrahlung is at lower energies [1].

Significant absorption No significant absorption
Cannot be ignored Can be ignored
Atomic-number correlation
Yes Yes
Overall characteristics
Worse Better

                                *Note: To have high spatial resolution, EDS measurement in (S)TEM has to be performed in STEM mode.

Note that the use of a large convergence angle, as occurs in the STEM mode with a focused probe minimizes the problem of channeling enhanced X-ray emission.

The schematics in Figure 4532 shows the electron optical column in a modern analytical electron microscope operated in STEM mode.

Schematics of the electron optical column in a modern analytical electron microscope operated in STEM mode

Figure 4532. Schematics of the electron optical column in a modern
analytical electron microscope operated in STEM mode.

 

 

[1] Ralf Terborg, Bruker.

 

 

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