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Characterization of cobalt phosphide nanoparticles derived from molecular clusters in mesoporous silica

  • Paulin Buchwalter
  • Jacky Rosé
  • Bénédicte Lebeau
  • Ovidiu Ersen
  • Maria Girleanu
  • Pierre RabuEmail author
  • Pierre BraunsteinEmail author
  • Jean-Louis PaillaudEmail author
Research Paper

Abstract

The synthesis of well dispersed cobalt phosphide nanoparticles (NPs) in SBA-15 mesoporous silica by wet impregnation of the molecular cluster [Co4(CO)10(μ-dppa)] (1) (dppa = HN(PPh2)2) is described. The thermal activation of the silica impregnated precursor under a H2/N2 (5/95 %) stream at different temperatures to form NPs was studied and it was found that the size of the latter is limited in the 5.5–6.5 nm range by the size of the pores. The obtained materials were characterized by various analytical methods. The porosity and the structure of the mesoporous silica supports were analyzed by N2 adsorption/desorption and small-angle X-ray diffraction. The nanoparticles were characterized by wide-angle X-ray diffraction, transmission electron microscopy in conventional and scanning modes, electron tomography, energy-dispersive X-ray spectroscopy, and magnetic measurements. Cobalt phosphide NPs of few nanometers were observed in the pores of SBA-15.

Keywords

Nanoparticles Mesoporous silica Cobalt phosphide Electron microscopy Magnetism 

Notes

Acknowledgments

We are grateful to the Région Alsace (PhD grant to P. Buchwalter), the Centre National de la Recherche Scientifique and the Ministère de la Recherche for support. We also acknowledge support of the ci-FRC of Strasbourg. We wish to thank Dris Ihiawakrim, IPCMS Strasbourg, France, and Loïc Vidal, IS2M Mulhouse, France, for the transmission electron microscopy, and Laure Michelin, IS2M Mulhouse, France, for XRF analyses.

Supplementary material

11051_2013_2132_MOESM1_ESM.docx (2.3 mb)
Supplementary material 1 (DOCX 2,326 kb)

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© Springer Science+Business Media Dordrecht 2013

Authors and Affiliations

  1. 1.Equipe Matériaux à Porosité Contrôlée (MPC)Institut de Science des Matériaux de Mulhouse (IS2M), UMR CNRS 7361 – UHA, ENSCMuMulhouse CedexFrance
  2. 2.Laboratoire de Chimie de CoordinationInstitut de Chimie (UMR 7177 CNRS, UdS)Strasbourg CedexFrance
  3. 3.IPCMS (UMR 7504 CNRS, UdS) and NIEStrasbourg Cedex 2France

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