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FIB Preparation of a NiO Wedge-Lamella and STEM X-Ray Microanalysis for the Determination of the Experimental k(O-Ni) Cliff-Lorimer Coefficient

Published online by Cambridge University Press:  03 January 2013

Aldo Armigliato ,
Stefano Frabboni ,
Gian Carlo Gazzadi  and
Rodolfo Rosa
Aldo Armigliato*
Affiliation:
CNR-IMM Institute, Via P.Gobetti, 101 40129 Bologna, Italy
Stefano Frabboni
Affiliation:
Dipartimento di Fisica, Università di Modena e Reggio Emilia, Via G. Campi 213/A, 41100 Modena (Italy) and CNR-Istituto di Nanoscienze-S3, via G. Campi 213/A, 41100 Modena, Italy CNR-Istituto di Nanoscienze-S3, via G. Campi 213/a, 41100 Modena, Italy
Gian Carlo Gazzadi
Affiliation:
CNR-Istituto di Nanoscienze-S3, via G. Campi 213/a, 41100 Modena, Italy
Rodolfo Rosa
Affiliation:
Dipartimento di Scienze Statistiche, Università di Bologna, Via Belle Arti, 40126 Bologna, Italy
*
*Corresponding author: E-mail: [email protected]
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Abstract

A method for the fabrication of a wedge-shaped thin NiO lamella by focused ion beam is reported. The starting sample is an oxidized bulk single crystalline, ⟨100⟩ oriented, Ni commercial standard. The lamella is employed for the determination, by analytical electron microscopy at 200 kV of the experimental k(O-Ni) Cliff-Lorimer (G. Cliff & G.W. Lorimer, J Microsc103, 203–207, 1975) coefficient, according to the extrapolation method by Van Cappellen (E. Van Cappellen, Microsc Microstruct Microanal1, 1–22, 1990). The result thus obtained is compared to the theoretical k(O-Ni) values either implemented into the commercial software for X-ray microanalysis quantification of the scanning transmission electron microscopy/energy dispersive spectrometry equipment or calculated by the Monte Carlo method. Significant differences among the three values are found. This confirms that for a reliable quantification of binary alloys containing light elements, the choice of the Cliff-Lorimer coefficients is crucial and experimental values are recommended.

Keywords

FIB lamellaanalytical electron microscopynickel-oxide filmsCliff-Lorimer factorextrapolation methodMonte Carlo simulation
Type
Software, Techniques and Equipment Development
Information
Microscopy and Microanalysis , Volume 19 , Issue 1 , February 2013 , pp. 79 - 84
Copyright
Copyright © Microscopy Society of America 2013

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