This work studied the effect of plasma treatment on the wettability of composite materials constituted of polyethylene glycol (PEG) and polyhydroxybutyrate (PHB) processed through the spin-coating and electrospinning techniques. For this purpose different polymeric solutions of PEG:PHB with proportions of 100:0, 80:20, 50:50, 20:80, and 0:100 were prepared. It found that the hydrophobicity of the as-prepared composite films processed by electrospinning was higher than those processed by spin-coating, using the same proportions of PEG:PHB. The electrospun samples with higher content of PHB (20:80 and 0:100) showed a surface morphology constituted by fibers of 1.7-1.9 μm in size. On the other hand, the electrospun samples processed with a lower content of PHB (100:0, 80:20, 50:50) did not form fibers and exhibited a rough surface. The subsequent plasma treatment with argon plasma of the electrospun samples produced a decrease in the contact angle, even in the samples with surface roughness. These contact angle values were similar to those obtained by spin-coating, or even lower, as in the case of the sample with PEG:PHB content of 20:80 in which the dip-coated film, the as-prepared membrane, and the plasma-treated membrane showed contact angles of 49°, 77.4°, and 0° (superhydrophilic) respectively.