Advanced light element and low energy X-ray line analysis using Energy Dispersive Spectrometry (EDS) with Silicon Drift Detectors (SDD)
Abstract
Introduction: Characterization at the micro- to nano-scale is crucial for understanding many processes in earth, planetary, material and biological sciences. The composition of thin electron transparent samples can be analyzed in the nm-range using transmission electron microscopes (TEM) or, specific sample holders provided, in the field emission scanning electron microscope (FE-SEM). Nevertheless both methods often require complex sample preparation. An alternative method is to analyze bulk samples with a FE-SEM. In order to decrease the excitation volume for generated X-rays, low accelerating voltages (HV<10) are required. Consequently, only low to intermediate energy X-ray lines can be evaluated and many peak overlaps have to be deconvoluted since the high energy range is not available. Methods: A BRUKER Quantax EDS system with an XFlash Silicon Drift Detector acquired EDS spectra in spectrum images. To separate overlapping peaks, an extended atomic database [1] was used. For single channel EDS the electron beam current, solid angle, take-off angle and exposure time can be optimized to investigate the element composition. Multiple SDD setups ensure an even higher efficiency and larger collection angles for the X-ray analysis than single channel detectors. Shadowing effects are minimized in element distribution maps so that samples can be investigated quickly and sometimes in a close to natural state, with little preparation. A new type of EDS detector, the annular four channel SDD (XFlash 5060F), is placed between the pole piece and sample. It covers a very large solid angle (1.1 sr) and allows sufficient data collection at low beam currents on beam sensitive samples with substantial surface topography. Examples of applications: Results demonstrate that SDD-based EDS analysis contributes essential information on the structure at the micro- to nano scale of the investigated sample types. These include stardust analogue impact experiments [2], Chicxulub asteroid impactites [3,4], ore characterization of the Sudbury igneous complex [5], biomineralization in bacteria and insects [6], and characterization of ceramics [7] and ceramic metal joints [8]. We conclude that improvements in SDD and pulse processor technology including multi-detector and multi-segment options provide new insights because a vast amount of detailed information can be collected in a short period of time. Using the XFlash QUAD 5060F, samples can be analyzed rapidly at low beam current without carbon coating. [1] A. Assmann, A. and M. Wendt 2003. Spectrochim. Acta Part B, 58: 711-716. [2] A.T. Kearsley et al. 2013. 44th LPSC, 18-22.03.2013, The Woodlands, USA: #1910. [3] P. Schulte et al. 2010. Science 327: 1214-1218. [4] M. Nelson et al. 2012. GCA 86: 1-20. [5] Salge et al. 2013. LPI Contrib .No. 1737: 89. [6] M. Falke et al. 2013. EURO BioMat. 23-24.04.2013, Weimar, Germany. [7] H. Yurdakul et al. 2013.accepted for MC 2013, 25-30.08.2013, Regensburg, Germany [8] O. Tunckan 2010. PhD thesis. Anadolu University, Eskisehir, Turkey.
- Publication:
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AGU Fall Meeting Abstracts
- Pub Date:
- December 2013
- Bibcode:
- 2013AGUFM.V53B2796S
- Keywords:
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- 5112 PHYSICAL PROPERTIES OF ROCKS Microstructure;
- 3954 MINERAL PHYSICS X-ray;
- neutron;
- and electron spectroscopy and diffraction;
- 3694 MINERALOGY AND PETROLOGY Instruments and techniques;
- 0419 BIOGEOSCIENCES Biomineralization