This work reports the synthesis and properties of a new membrane based on polyvinyl chloride (PVC) grafting with polyacrylic acid (PAA) using argon (Ar) plasma. The membranes of PVC were synthesized by solution-casting method, where PAA was deposited as an ultrathin film onto PVC using dielectric barrier discharge at atmospheric pressure with Ar gas. The surface characteristics and chemical composition of the modified membranes were analyzed by water contact angle, scanning electron microscopy, and Fourier transform infrared spectroscopy. Moreover, the electrochemical properties of the membrane were investigated via ion exchange capacity for the purpose of using it as a polyelectrolyte membrane.