We report the synthesis of sodium zinc diphosphate (Na2ZnP2O7) using a domestic microwave oven (2.45 GHz) and metal ion doped sodium zinc diphosphate (Na1.88Gd0.04ZnP2O7/Na1.92M0.04ZnP2O7 (M=Mn and Cu)) by a solid state metathesis reaction. All the materials were characterized by powder X-ray diffraction (XRD) and infrared spectroscopy (IR). These metal doped diphosphates were crystallized in a tetragonal lattice with space group . The IR spectra of all the samples were characterized by bands due to the group. The powder electron spin resonance (ESR) spectrum of Na1.88Gd0.04ZnP2O7 gave a characteristic 鈥淯鈥?type spectrum. The powder ESR spectrum of Na1.92Mn0.04ZnP2O7 consists of six lines while Na1.92Cu0.04ZnP2O7 gave a broad profile. All the doped metal ions occupy the Na+ site in the diphosphate lattice. The broad emission band at 614 nm (red band) observed for Na1.92Mn0.04ZnP2O7 is assigned to an electronic transition of Mn2+ in distorted octahedral coordination.