The main objective of this work was to develop an interrupted wet-spinning process for the elaboration of hollow and multi-membrane chitosane fibers. The knowledge of the specific role of the processing parameters (extrusion rate and coagulation time) and physico-chemical parameters of coagulation (chitosane dope concentration, nature and concentration of the coagulant agent) allow us to elaborate hollow fibers from a liquid macrofiber of chitosane by interrupting the coagulation step through water washing. This approach was generalized for the elaboration of multi-membrane hollow fibers by alternating coagulation baths and water washing baths in a sequenced coagulation process. By modifying the dope viscosity and the nature and concentration of the coagulant agent, the microstructure of chitosan hydrogels was studied by specific scattering and microscopy techniques. Depending on the coagulation conditions, it was possible to process hydrogels with different microstructure consisting of aggregates assembled into micrometric clusters or capillary gels with more organized structures of periodic parallel micro-channels. This work opens the way to elaboration of a wide range of chitosan physical hydrogels based on the concept of “decoy of biological media” with tuneable biological properties for tissue engineering: hollow tubes and multi-membrane tubes as blood vessel substitutes or nerve guides
