Abstract : Polyelectrolyte microcapsules prepared by the Layer-by-Layer deposition technique have attracted a great deal of interest for their potential applications in various fields such as drug delivery and biotechnology. The aim of this work was to develop new LbL microcapsules made from hyaluronic acid (HA) - biocompatible, biodegradable and non-toxic polysaccharide. First, optimization of conditions for preparing microcapsules from HA and poly(allylamine) (PAH) was carried out. In the second step, synthetic PAH was replaced by biocompatible cationic polymers: a polypeptide, poly(L-lysine (PLL) or a quaternized derivative of chitosan (QCH) from polysaccharide family. The influence of the polycationic partner on the morphology, stability, permeability properties and enzymatic degradation of microscapsules was analyzed. Those properties were then tuned by shell cross-linking. The encapsulation of dextran release as a model drug was demonstrated.