Nanocomposites were prepared by a very simple route from preformed platinum particles and a nickel layered hydroxide salt (LHS), these compounds being first synthesized separately by the polyol process. The nanoparticles were treated with mercaptoacetate before being brought into contact with the lamellar compound. XPS and IR spectroscopies give clear evidence for interactions between the platinum nanoparticles and the mercaptoacetate species. XRD, TEM and magnetic characterizations show that the structure of the nickel hydroxide layers is retained and that some of the LHS sheets contain incorporated nanoparticles. (C) 2009 Elsevier Ltd. All rights reserved.