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A journey through the secret life of nanoparticles: from 2D high resolution images to 3D oxidation state mapping

AuthorsTorruella, Pau; Arenal, Raúl; Yedra, Lluís; Estrader, Marta ; Salazar-Álvarez, G.; López-Ortega, Alberto; Nogués, Josep ; Midgley, Paul A.; Estradé, S.; Peiró, F.
Issue Date2016
CitationNanoBioMed 2016
AbstractElectron tomography has been used in the field of materials science for recovering the three dimensional (3D) structure of materials in the nanoscale. To add chemical information to this 3D volume, Energy Filtering TEM (EFTEM) is the widely spread technique. However, the selection of specific energy channels implies that significant information in the spectrum is lost. Instead, electron energy-loss spectroscopy (EELS) spectrum-images (SI) acquired in tomographic series retain all chemical information for 3D chemical reconstruction. In particular, the near edge energy losses (ELNES) contain information relative to the elemental coordination and thus, recovering of the oxidation state of a transition metal is also possible. In this work we will develop the concept of EELS spectrum volume (EELS-SV), a full EELS dataset in 4D, where every voxel of a whole volume contains a complete spectrum of energy losses. Our approach to EELS-SV reconstruction is based on the acquisition of spectrum images (SI) in tomographic mode SI, thus taking a single SI for every tilt angle and on the identification of independent components and the corresponding abundance maps (ICA analysis). We will prove the feasibility of EELS tomography from data acquired aberration corrected TEM’s but also in uncorrected instruments thanks to the use of multivariate analysis (MVA), and blind source separation (BSS) methods combined with advanced reconstruction algorithms. We have applied this approach to obtain 3D reconstruction of advanced metal oxide nanostructured materials as FexCo(3-x)O4/Co3O4mesoporous structures and bimagnetic FeOx/FeOy core/shell nanoparticles, for which the oxidation state of Fe can be discriminated in 3D.
DescriptionResumen del trabajo presentado a la NanoBioMed Conference, celebrada en Barcelona (España) del 22 al 24 de noviembre de 2016.-- et al.
Appears in Collections:(CIN2) Comunicaciones congresos
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