Synthesis of nanoscale antimony particles L. Balan & A. Dailly & R. Schneider & D. Billaud & P. Willmann & J. Olivier-Fourcade & J.-C. Jumas Published online: 26 October 2006 # Springer Science + Business Media B.V. 2006 Abstract For the search of new negative electrodes of Li-ion batteries, a low-temperature method has been developed for the preparation of nanoscale antimony particles which uses an alkoxide-activated sodium hydride as reducing agent of antimony pentachloride. X-ray diffraction and TEM studies confirm the obtaining of amorphous Sb nanoparticles dispersed in an organic matrix. 121 Sb Mössbauer spectroscopy gives evidence for the occurrence of interactions between antimony and the matrix. These interactions are modified by the washing treatments. Key words nanosized antimony particles . amorphous antimony . 121 Sb Mössbauer spectroscopy 1 Introduction The increasing demand of electric energy for many applications motivates an intensive research for Lithium-ion batteries. Improvement of their electrochemical performances to obtain higher specific capacity, better cycleability, large reversibility and good safety requires the search of new electrode materials. In particular the research of new negative Hyperfine Interact (2005) 165: 101–106 DOI 10.1007/s10751-006-9252-2 L. Balan : A. Dailly : D. Billaud (*) Laboratoire de Chimie du Solide Minéral (UMR 7555 CNRS)Université Henri Poincaré Nancy I, BP 239, 54506 Vandoeuvre les Nancy Cedex, France e-mail: Denis.Billaud@lcsm.uhp-nancy.fr R. Schneider Laboratoire de Synthèse organométallique et Réactivité (UMR 7565 CNRS)Université Henri Poincaré Nancy I, BP 239, 54506 Vandoeuvre les Nancy Cedex, France P. Willmann Centre National d’Etudes Spatiales, 18 Avenue Edouard Belin, 31401 Toulouse Cedex 9, France J. Olivier-Fourcade : J.-C. Jumas Laboratoire des Agrégats Moléculaires et Matériaux Inorganiques (UMR 5072 CNRS)( Université Montpellier II, Place Eugène Bataillon, 34095 Montpellier Cedex 5, France