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Molecular Clusters in Mesoporous Materials as Precursors to Nanoparticles of a New Lacunar Ternary Compound Pd x Mo y P

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Abstract

Bimetallic clusters of composition Pd2Mo2(η5-C5H5)2(μ3-CO)2(μ2-CO)4(PR3)2 (R = ethyl or phenyl) were incorporated by impregnation from solution into two different silica matrices, amorphous xerogels and ordered SBA-15, and a study of their thermal decomposition under a reducing atmosphere is reported. With both matrices, a suitable thermal treatment afforded nanoparticles of a new bimetallic phosphide. Although nanoparticles of composition Pd x Mo y P, isostructural with Mo3P, were formed in both matrices, they were more uniformly distributed in the SBA-15 framework and showed a narrower size distribution. The samples have been characterized by powder XRD, chemical analysis, FT-IR spectroscopy, TEM and electron tomography (3D TEM).

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Acknowledgements

We are grateful to the Région Alsace (Doctoral grant to S. G.-V.), the Centre National de la Recherche Scientifique and the Ministère de la Recherche for support.

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Authors and Affiliations

  1. Laboratoire de Matériaux à Porosité Contrôlée (UMR 7016 CNRS, ENSCMu, UHA), 3 rue Alfred Werner, 68093, Mulhouse Cedex, France

    S. Grosshans-Vièles, J.-L. Paillaud & B. Lebeau

  2. Laboratoire de Chimie de Coordination, Institut de Chimie (UMR 7177 CNRS), Université Louis-Pasteur, 4 rue Blaise Pascal, 67070, Strasbourg Cedex, France

    S. Grosshans-Vièles, P. Croizat, P. Braunstein & J. Rosé

  3. IPCMS-GSI, UMR 7504 (CNRS, ULP) 23, rue du Loess, BP 43, 67034, Strasbourg, Cedex 2, France

    O. Ersen

  4. IPCMS-GMI, UMR 7504 (CNRS, ULP) 23, rue du Loess, BP 43, 67034, Strasbourg, Cedex 2, France

    S. Grosshans-Vièles & P. Rabu

  5. CIRIMAT UMR 5085 (CNRS, UPS, INPT), 118 route de Narbonne, 31062, Toulouse, Cedex 9, France

    C. Estournès

Authors
  1. S. Grosshans-Vièles
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  2. P. Croizat
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  3. J.-L. Paillaud
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  4. P. Braunstein
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  5. O. Ersen
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  6. J. Rosé
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  7. B. Lebeau
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  8. P. Rabu
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  9. C. Estournès
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Corresponding authors

Correspondence to J.-L. Paillaud, P. Braunstein, P. Rabu or C. Estournès.

Electronic supplementary material

Below is the link to the electronic supplementary material. Chemical nanoprobe analysis by energy-dispersive spectroscopy of X-rays (EDSX) of sample 1a, 1b, 2a and 2b are available together with a movie on the 3D tomography representation

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Grosshans-Vièles, S., Croizat, P., Paillaud, JL. et al. Molecular Clusters in Mesoporous Materials as Precursors to Nanoparticles of a New Lacunar Ternary Compound Pd x Mo y P. J Clust Sci 19, 73–88 (2008). https://doi.org/10.1007/s10876-007-0171-4

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  • DOI: https://doi.org/10.1007/s10876-007-0171-4

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