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Films and fibers of PMMA/ZnO nanocomposites (100/0, 99/01, 97/03, 95/05, 90/10, and 85/15wt.%) were produced by casting and electrospinning, respectively. Their structural, thermal, and optical properties were investigated by XRD, SEM, TGA, PAS, and PL. The incorporation of ZnO NPs reduced the diameter of PMMA fibers and the presence of beads. The surfaces of the fibers exhibited greater hydrophobicity,...