Poly(ether ether ketone) (PEEK) was synthesized with a good yield, by nucleophilic substitution reaction of 4,4'-difluorobenzophenone (DFBP) with hydroquinone (HQ) in the presence of anhydrous potassium carbonate (K2CO3) under microwave (MW) irradiation. The highest yield of 96.1% was obtained using sulfolane as the solvent and with a reaction time of only 55 min. The reaction time was reduced greatly compared with conventional heating. The product was characterised by infrared spectroscopy (IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The polymer, having inherent viscosities of 0.71 dlg(-1), has excellent thermal stability as shown by 10% weight loss in nitrogen at about 563 degrees C. The XRD pattern confirmed the semicrystalline character of PEEK synthesized.