Novel nanosized lamellar germanium phosphate, α-Ge (HPO4)2.1.84H2O(nGeP), with interlayer spacing (d001) = 7.71Ǻ, was prepared. Preparations of polystyrene/lamellar germanium phosphate nanocomposite membranes were carried out by mixing slurry tetrahydrofuran (THF) solution of (nGeP) , of different weight percentages (2.5, 5 and 15 wt %), with (THF) solution of 5% polystyrene (PS) in concentration at 45°C with stirring for 48 hours. The resultant mixtures were poured into flat surface containers, of desired thickness, respectively, and allowed to dry in air. The resulting fully dried composites were pealed from the glass containers. The composite membranes were transparent flexible thin films and were characterized by XRD, TGA, FT-IR, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Size particles of lamellar germanium phosphate calculated from XRD broadening method using the Scherrer,s equation, found to be 44.6 nm . TEM images of nanocomposites show that the (nGeP) in the nanometer scale, in the range 38-53 nm. The composite materials show to have mechanical and thermal stability properties superior to that of the original polymer, which a result of the enhancement of the thermal properties of PS/nGeP nanocomposites. The exchange capacities of the resultant composite membranes were investigated.