We report here the growth and characterization of iron oxide nanoparticles by polyionic multilayersassembled by electrostatic layer-by-layer adsorption. The polyions poly(diallyldimethylammonium) chloride(PDDA) and polystyrenesulfonate (PSS) were used for the layer-by-layer assembly of the polyions.Nanoparticle nucleation was achieved by a cyclic repetition of Fe oxidative hydrolysis under an inertatmosphere. We employed UV-vis analysis for both monitoring the multilayer assembly process andascertaining the influence of the Fe oxidative hydrolysis process on the integrity of the polymer film. Nodegradation of the multilayers due to the particle growth procedure was observed. The nucleation andgrowth of needle-shaped nanoparticles with a length of about 100 nm and a width of about 10 nm weredetected by transmission electron microscopy (TEM). The void volume of the polymer
matrix provided anupper limit to the particle size. As shown by selective area electron diffraction (SAED), the polycrystallineparticles were identified as
mages/gifchars/beta2.gif" BORDER=0 ALIGN="middle">-FeOOH (akaganéite), a result confirmed by reflection-absorption IRspectroscopy.