New reference and test materials for the characterization of energy dispersive X-ray spectrometers at scanning electron microscopes
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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.
KeywordsEDX EDS Performance check SEM Test materials Spectrometer efficiency
Thanks are due to European Metrology Research Programme (EMRP) for funding the SurfChem project (http://www.emrp-surfchem.bam). The EMRP is jointly funded by the EMRP participating countries within EURAMET and the European Union. Many discussions with Dr. M. Procop are gratefully acknowledged by V.-D. H. The authors thank also Dr. W. Bremser (BAM-1.4) for the first evaluation of the homogeneity and stability measurements and Dr. V. Wachtendorf (BAM-7.5) for carrying out the climatic tests.
- 5.Procop M (1996) A simple procedure to check the spectral response of an EDX detector. Mikrochim Acta Suppl 13:473–477Google Scholar
- 7.ISO 15632 (2012) Microbeam analysis—selected instrumental performance parameters for the specification and checking of energy-dispersive X-ray spectrometers for use in electron probe microanalysis. ISO, GeneveGoogle Scholar
- 9.ISO/IEC 17025 (2005) General requirements for the competence of testing and calibration laboratories. ISO, GeneveGoogle Scholar
- 10.BAM Webshop, https://www.webshop.bam.de/, Reference Materials/Test Materials
- 11.Kim KJ, Jang JS, Kim AS, Suh JK, Chung Y-D, Hodoroaba V-D, Wirth T, Unger WES, Kang HJ, Lee YH, Sykes DE, Wang M, Wang H, Ogiwara T, Nishio M, Tanuma S, Simons D, Szakal C, Osborn W, Gorham JM, Steel EB, Terauchi S-y, Kurokawa A, Fujimoto T, Jordaan W, Jeong CS, Havelund R, Spencer S, Shard A, Streeck C, Beckhoff, Eicke A, Terborg R (2014) CCQM-P140 pilot study; Quantitative surface analysis of multi-element alloy films by depth profiling. Metrologia, submittedGoogle Scholar
- 20.Alvisi M, Blome M, Griepentrog M, Hodoroaba V-D, Karduck P, Mostert M, Nacucchi M, Procop M, Rohde M, Scholze F, Statham P, Terborg R, Thiot JF (2006) The determination of the efficiency of energy dispersive X-ray spectrometers by a new reference material. Microsc Microanal 12:406–415CrossRefGoogle Scholar
- 22.Burgess S, Li X, Holland J (2013) High spatial resolution energy dispersive X-ray spectrometry in the SEM and the detection of light elements including lithium. Microsc Anal 27(4):S8–S13, EUGoogle Scholar