This master thesis presents a new fabrication method to prepare hydrogels with fully interconnected and tunable macropore networks prepared with co-continuous polymer blends. The main contributions are: (1) a hydrogel fabrication process providing a high control over the average pore size diameter, their volume fraction and their interconnectivity; (2) the microstructural characterization of porous hydrogels with new techniques such as X-ray microtomography and (3) the preparation of porous gels with industrial equipment such as extruders and injection molding presses. The development and improvement of methods and techniques to prepare porous polymers and porous gels have been intensive areas of research in materials science over the past 20 years because of their potential use in fields as diverse as high performance membranes and filtration devices, supports for catalysis and biochemical reactions, encapsulating devices for drug release, and scaffolds for cells seeding and proliferation. For this last application, in tissue engineering, some typical parameters related to porosity must be rigorously controlled: (1) the average pore size diameter; (2) the pore volume fraction; (3) the pore interconnectivity. Porous hydrogels are excellent candidates due to their similarities with the extracellular matrix (composition, mechanical properties and diffusion properties). A certain number of methods and techniques have been developed and studied to prepare gels comprising microstructured 3-D networks of (more or less) interconnected pores (also called sometimes microfluidic gels or (macro)porous gels). Poly(L-lactide) (PLA) porous materials were realized from immiscible and co-continuous binary blends of polystyrene/poly(L-lactide) (PS/PLA) at 50/50 %vol prepared by different methods : (1) internal mixer (cubic samples with 0.8 mm sides) and (2) extrusion followed by injection molding which allows the fabrication of bars with superior dimensions (0.95 cm x 1.25 cm x 6.3 cm). Quiescent annealing of the binary blends was performed at 190 °C to tune the characteristic dimensions of the co-continuous morphology: (1) 0, 10, 30, 60 and 90 min for cubic samples and (2) 0, 10, 20 and 30 min for bars. Afterwards, the PLA phase has been isolated by a specific solvent extraction of the PS phase to obtain porous PLA molds. Gravimetric analysis have demonstrated a co-continuity superior to 95% for cubic samples and superior to 85% for the bars. This morphology was analyzed by scanning electron microscopy (SEM) for each annealing time (for the cubic samples). Image analysis performed on the SEM micrographs have demonstrated that the average pore diameter can range from 3 mum to over 400 mum and that the specific interfacial area ranges from 5800 cm-1 to 45 cm-1, for annealing times going from 0 min to 90 min). The porosity of the bars was observed by X-ray microtomography and shows that the average pore diameter ranges from 10 mum to 500 mum (annealing from 10 min to 30 min). Solutions of agar or alginate were subsequently injected into the PLA porous molds by using a manual injection system, followed by an in situ gelification. Visual inspections and optical microscope observations show a complete injection for molds with average pore sizes over 20 mum (cubic samples) and over 300 mum (for bars). These assumptions are also supported by the gels morphology characterization. The second polymer phase (PLA) was subsequently dissolved using a second selective solvent, leaving only the porous gel structures. X-ray microtomography analysis, which provide 2-D and 3-D images, have demonstrated that the morphologies of the porous gels are similar to the PLA molds microstructures. For example, porous gels prepared with cubic PLA molds annealed during 60 min, show an average pore size of about 285 mum (as compared to 200 mum for the PLA molds) and a specific interfacial area of 70 cm -1 (as compared to 100 cm-1 for the PLA molds). Similar results were obtained for the porous gels prepared with the porous PLA bars (qualitative observation). The effectiveness of two sterilization methods has been proven on nutrient agar (NA) and "Brain Heart Infusion" (BHI) with no bacterial colonies apparition. The first method is the freeze-drying followed by an oven treatment at 120 °C in a sterile environment. The porous gel morphology was characterized by X-ray microtomography before and after freeze-drying, and after rehydration, demonstrating the conservation of the macroscopic dimensions of the gels, of their morphologies and porosities. The second method is the successive baths in an ethanol solution. Finally mechanical compression tests have shown that porous gels, as can be expected, have a lower compressive resistance as compared to non-porous hydrogels. (Abstract shortened by UMI.).
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- Engineering, Chemical;Engineering, Biomedical;Engineering, Materials Science