title   
  

Determining the stoichiometry of (K,Na)NbO(3) using optimized energy-dispersive x-ray spectroscopy and electron energy-loss spectroscopy analyses in a transmission electron microscope

Sturm, Saso and Bencan, Andreja and Gülgün, Mehmet Ali and Malic, Barbara and Kosec, Marija (2011) Determining the stoichiometry of (K,Na)NbO(3) using optimized energy-dispersive x-ray spectroscopy and electron energy-loss spectroscopy analyses in a transmission electron microscope. Journal of the American Ceramic Society, 94 (8). pp. 2633-2639. ISSN 0002-7820

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Official URL: http://dx.doi.org/10.1111/j.1551-2916.2011.04389.x

Abstract

This paper describes an optimized analytical procedure for determining the composition of alkaline niobate-based lead-free piezoceramics by energy-dispersive X-ray spectroscopy (EDXS) in a transmission electron microscope (TEM). To discriminate the material-specific composition from the artifacts introduced during the EDXS/TEM analyses, the effects of radiation damage and the absorption of the characteristic X-ray lines were studied in detail. The optimized, quantitative EDXS analysis was tested on sodium potassium niobate with the nominal composition K(0.5)Na(0.5)NbO(3) (KNN) by applying KNbO(3) and NaNbO(3) as standards. The results obtained indicate that KNbO(3) is more radiation sensitive than NaNbO(3). A similar degradation was confirmed in KNN, where the loss of potassium was higher than that of sodium. In addition, the degradation of the KNN was associated with a severe oxygen loss and the reduction of niobium. To achieve highly reliable, quantitative analyses and to preserve good counting statistics, the optimum conditions for the EDXS/TEM analyses were found at an electron dose rate of 0.4 pA/nm(2) and an acquisition time of around 200 s in the specimen thickness range between 30 and 200 nm.

Item Type:Article
Subjects:T Technology > TA Engineering (General). Civil engineering (General) > TA401-492 Materials of engineering and construction. Mechanics of materials
ID Code:17320
Deposited By:Mehmet Ali Gülgün
Deposited On:27 Oct 2011 16:29
Last Modified:27 Oct 2011 16:29

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