Polysulfone is a widely used polymer for hemodialysis membranes. Improving polysulfone membrane hemocompatibility and removing toxins are highly desirable for the quality of life of the dialysis patient. The main objective of this work is the investigation of a novel dual post treatment approach comprising the effect of microwave treatment on hydrogen peroxide-treated polysulfone hollow fiber (PS HF) membranes. Microwave treatment of fibers impregnated with magnesium chloride was adopted. The morphology, structure, and surface properties of the membranes were comprehensively characterized using scanning electron microscopy, Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, contact angle and zeta potential measurements. The mechanical properties of the treated fibers were also investigated. The performance of the studied membranes was evaluated in terms of pure water permeability and sieving coefficients of urea and creatinine. Results indicated that membrane mechanical properties and hydrophilicity could be enhanced using microwave treatment while maintaining a stable chemical structure. The hollow fiber membrane mean pore size decreased by (4.5-66%) for both microwave and combined treatments, while no significant change was observed on membrane average porosity. After fibers were subjected to MW treatment (3-7% MgCl2), there was a slight variation in the urea and creatinine sieving coefficients and a considerable alteration in permeability. Microwave post-treatment in wet conditions could be applied as a useful technique for tuning hemodialysis PS HF membranes.