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Quantitative Energy Dispersive X-ray Microanalysis of Electron Beam-Sensitive Alloyed Nanoparticles

Published online by Cambridge University Press:  03 March 2008

Nadi Braidy ,
Zygmunt J. Jakubek ,
Benoit Simard  and
Gianluigi A. Botton
Nadi Braidy
Affiliation:
Department of Materials Science and Engineering, McMaster University and the Brockhouse Institute for Materials Research, Hamilton, ON L8S 4L7, Canada
Zygmunt J. Jakubek
Affiliation:
National Research Council of Canada, Steacie Institute for Molecular Sciences, Ottawa, ON K1A 0R6, Canada
Benoit Simard
Affiliation:
National Research Council of Canada, Steacie Institute for Molecular Sciences, Ottawa, ON K1A 0R6, Canada
Gianluigi A. Botton
Affiliation:
Department of Materials Science and Engineering, McMaster University and the Brockhouse Institute for Materials Research, Hamilton, ON L8S 4L7, Canada
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Abstract

An energy dispersive X-ray spectrometry (EDXS) method is developed to evaluate the composition of alloyed nanoparticles (NPs) where one of the alloying elements is removed under the electron beam during microanalysis with a transmission electron microscope (TEM). The method is demonstrated for alloyed Au-Ag NPs of a diameter ranging from 6 to 20 nm produced by laser evaporation of a water-suspended Ag-Au powder mixture of varying composition. Series of EDXS spectra are recorded for 30 NPs from samples with five different Ag:Au ratios revealing Ag depletion from NPs during electron irradiation. By studying the evolution of NPs composition as a function of dose, the initial Ag content for each NP is extrapolated. The rate of Ag depletion is discussed in terms of sputtering and knock-on damage. On average, approximately one Ag atom is lost from the NP for each Ag L X-ray detected. To assess the limitations of microanalysis in these sensitive nanoscale structures, the concept of detectability limit is adapted to our method. This benchmark is then evaluated for Ag in Au-Ag NPs of various sizes and acquisition times. This study should be regarded as a guide for the design of analytical TEM measurements of beam-sensitive NPs.

Keywords

nanoparticlesanalytical TEMenergy dispersive X-ray spectrometryelectron-beam damagesilvergold
Type
Research Article
Information
Microscopy and Microanalysis , Volume 14 , Issue 2 , April 2008 , pp. 166 - 175
Copyright
© 2008 Microscopy Society of America

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