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It is a latent wish of any SEM/EDS (scanning electron microscope with an energy dispersive spectrometer) analyst to “see more” of the analyzed specimen, i.e. to improve the existing analytical figures of merit.
One key issue are the relatively poor limits of detection (not below 0.1 mass-%) provided by energy dispersive X-ray spectrometry (EDX) with the conventional electron excitation (ED-EPMA). This is a consequence of relatively low peak-to-background ratios and reduced energy resolution when compared to wavelength dispersive spectrometry (WD-EPMA). Recent technological developments make possible to equip the SEM with a wavelength dispersive spectrometer (WDS), so that
significantly better energy resolution can be attained. Also a relative new product that can be easily attached to a SEM/EDS system is a micro-focus X-ray source. Hence, it is possible to perform (micro-focus) X-ray fluorescence spectrometry (μ-XRF) and take advantage of the enhanced peak-to-background ratios (well suited for trace analysis). However, there are also some disadvantages: an increased measurement time and excitation with a high current in the 10s of nA range are usually required for WDS. μ-XRF provides more bulk information and poor limits of detection for light elements. By combining the advantages of these analytical techniques “seeing more” becomes possible.
A calibrated instrumental setup was specially developed for the purposes of accurate measurements of absolute X-ray spectra emitted by modern micro-focus, low-power X-ray tubes. By knowing all the instrumental parameters the spectra measured with the 16 m long setup are recalculated into emitted X-ray tube spectra in photons per eV per msr per nA per s.
Checking the performance of energy dispersive X-ray spectrometers as well as validation of the results obtained with energy dispersive X-ray spectrometry (EDX) at a scanning electron microscope (SEM) involve the use of (certified) reference and dedicated test materials. This paper gives an overview on the test materials mostly employed by SEM/EDX users and accredited laboratories as well as on those recommended in international standards. The new BAM reference material EDS-CRM, which is currently in the process of certification, is specifically designed for the characterization of EDS systems at a SEM through calibration of the spectrometer efficiency in analytical laboratories in a simple manner. The certification of the spectra by means of a reference EDS is described. The focus is on the traceability of EDS efficiency which is ensured by measurements of the absolute detection efficiency of silicon drift detectors (SDD) and Si(Li) detectors at the laboratory of the PTB using the electron storage ring BESSY II as a primary X-ray source standard. A new test material in development at BAM for testing the performance of an EDS in the energy range below 1 keV is also briefly presented.
The high specificity of the coherent (Rayleigh), as well as incoherent (Compton) X-ray scattering to the mean atomic number of a specimen to be analyzed by X-ray fluorescence (XRF), is exploited to gain more information on the chemical composition. Concretely, the evaluation of the Compton-to-Rayleigh intensity ratio from XRF spectra and its relation to the average atomic number of reference materials via a calibration curve can reveal valuable information on the elemental composition complementary to that obtained from the reference-free XRF analysis. Particularly for matrices of lower mean atomic numbers, the sensitivity of the approach is so high that it can be easily distinguished between specimens of mean atomic numbers differing from each other by 0.1. Hence, the content of light elements which are invisible for XRF, particularly hydrogen, or of heavier impurities/additives in light materials can be calculated 'by difference' from the scattering calibration curve. The excellent agreement between such an experimental, empirical calibration curve and a synthetically generated one, on the basis of a reliable physical model for the X-ray scattering, is also demonstrated. Thus, the feasibility of the approach for given experimental conditions and particular analytical questions can be tested prior to experiments with reference materials. For the present work a microfocus X-ray source attached on an SEM/EDX (scanning electron microscopy/energy dispersive X-ray spectroscopy) system was used so that the Compton-to-Rayleigh intensity ratio could be acquired with EDX spectral data for improved analysis of the elemental composition.