Synthesis, Characterization, and Nanocatalysis Application of Core–Shell Superparamagnetic Nanoparticles of Fe3O4@Pd
Ariel L. Cappelletti A , Paula M. Uberman B , Sandra E. Martín B , Martín E. Saleta C , Horacio E. Troiani C , Rodolfo D. Sánchez C , Raúl E. Carbonio D and Miriam C. Strumia A EA IMBIV-CONICET, Departamento de Química Orgánica, Facultad de Ciencias Químicas, Universidad Nacional de Córdoba, X5000HUA Córdoba, Argentina.
B INFIQC-CONICET, Departamento de Química Orgánica, Facultad de Ciencias Químicas, Universidad Nacional de Córdoba, X5000HUA Córdoba, Argentina.
C Centro Atómico Bariloche, Comisión Nacional de Energía Atómica and Instituto Balseiro, Universidad Nacional de Cuyo, 8400 San Carlos de Bariloche (RN), Argentina.
D INFIQC-CONICET, Departamento de Fisicoquímica, Facultad de Ciencias Químicas, Universidad Nacional de Córdoba, X5000HUA Córdoba, Argentina.
E Corresponding author. Email: mcs@fcq.unc.edu.ar
Australian Journal of Chemistry 68(10) 1492-1501 https://doi.org/10.1071/CH14722
Submitted: 19 December 2014 Accepted: 14 March 2015 Published: 21 May 2015
Abstract
There is a wide number of different synthetic methods to obtain magnetite (Fe3O4) superparamagnetic nanoparticles (SPNPs). However, only a few are able to produce very small and well defined SPNPs with narrow size distribution. We report a modification of the metal-complex decomposition in organic media method in which we replace iron(iii) acetylacetonate (Fe(Acac)3) with an iron–urea complex (Fe-Urea) as metal source for the synthesis. With this modification we were able to obtain small particle sizes with a good control in size distribution. The Fe-Urea complex is easy to prepare with excellent yields. Core–shell nanoparticles are then prepared using palladium(ii) acetylacetonate as a Pd source, to obtain a Pd0 shell stabilised by oleylamine. The core–shell superparamagnetic nanoparticles of Fe3O4@Pd-OA are extensively characterized by FT-IR, powder X-ray diffraction, transmission electron microscopy, UV-vis, thermogravimetric analysis/differential scanning calorimetry, and magnetic susceptibility measurements, and tested in a palladium-catalyzed cross-coupling Suzuki–Miyaura reaction with promising results.
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