The layered nanocrystalline sodium manganese phosphate was synthesized by low-heating solid state reaction using MnSO 4 •H 2 O and Na 3 PO 4 •12H 2 O as raw materials. The resulting sodium manganese phosphate and its calcined products were characterized using element analysis, thermogravimetry and differential thermal analyses (TG/DTA), Fourier transform IR (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), ultraviolet-visible (UV-Vis) absorption spectroscopy, and magnetic susceptibility. The results showed that the product obtained at 70 ℃ for 3 h, NaMnPO 4 •3H 2 O, was a layered compound, and its crystallite size and interlayer distance were 27 nm and 1.124 nm, respectively. The thermal process of NaMnPO 4 •3H 2 O between room temperature and 700 ℃ experienced three steps, the dehydration of the one adsorption water at first, and then dehydration of the two crystal waters, at last crystallization of NaMnPO 4 . Magnetic susceptibility measurements of NaMnPO 4 • 3H 2 O from room temperature to 2.5 K point to ferrimagnetic ordering at T N -35 K.