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Resolving material-specific structures within Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles using anomalous small-angle X-ray scattering

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Here it is demonstrated that multiple-energy, anomalous small-angle X-ray scattering (ASAXS) provides significant enhancement in sensitivity to internal material boundaries of layered nanoparticles compared with the traditional modeling of a single scattering energy, even for cases in which high scattering contrast naturally exists. Specifically, the material-specific structure of monodispersed Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles is determined, and the contribution of each component to the total scattering profile is identified with unprecedented clarity. We show that Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles with a diameter of 8.2 ± 0.2 nm consist of a core with a composition near Fe₃O₄ surrounded by a (Mn(x)Fe(1-x))₃O₄ shell with a graded composition, ranging from x ≈ 0.40 at the inner shell toward x ≈ 0.46 at the surface. Evaluation of the scattering contribution arising from the interference between material-specific layers additionally reveals the presence of Fe₃O₄ cores without a coating shell. Finally, it is found that the material-specific scattering profile shapes and chemical compositions extracted by this method are independent of the original input chemical compositions used in the analysis, revealing multiple-energy ASAXS as a powerful tool for determining internal nanostructured morphology even if the exact composition of the individual layers is not known a priori.

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KRYCKA, L. kathryn, BORCHERS, Julie a., SALAZAR-ALVAREZ, German, LÓPEZ-ORTEGA, Alberto, ESTRADER I BOFARULL, Marta, ESTRADÉ ALBIOL, Sònia, WINKLER, Elin, ZYSLER, Roberto d., SORT, Jordi, PEIRÓ MARTÍNEZ, Francisca, BARÓ, M. d., KAO, C. c., NOGUÉS, Josep. Resolving material-specific structures within Fe₃O₄|γ-Mn₂O₃ core|shell nanoparticles using anomalous small-angle X-ray scattering. _ACS Nano_. 2013. Vol. 7, núm. 2, pàgs. 921-931. [consulta: 14 de gener de 2026]. ISSN: 1936-0851. [Disponible a: https://hdl.handle.net/2445/176409]

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