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The effect of a crosslinking agent on the formation of porous solids by polymerizing microemulsions formulated with monomers was investigated. Phenomenological studies were carried out to evaluate the possibility of controlling the morphology of the porous polymeric materials by using precursor microemulsions having a distinct microstructure. A microemulsion system, containing methyl methacrylate (MMA), acrylic acid (AA), the crosslinking agent ethyleneglycol dimethacrylate (EGDMA), water, and sodium dodecylsulfate (SDS) as surfactant, was studied. An identical surfactant‐free system, formed using the same monomers, crosslinking agent, and water, but without surfactant, was also studied. Microemulsion samples from both these systems, having a water in oil droplet microstructure and also samples exhibiting bicontinuous microstructural characteristics, were used as precursor systems for polymerization …