In the present study, the precipitation method was used to synthesize microcrystalline Nd-doped CaSO phosphor. Structural and morphological analysis of the phosphor samples were performed by using X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods. In addition, luminescent properties of the samples were characterized by thermoluminescence (TL) and optically stimulated luminescence (OSL) methods. The results of XRD analysis and SEM images showed that the prepared CaSO:Nd powder samples have an orthorhombic crystal structure and almost spherical in size with an average between 3 and 17 μm. In the light of the luminescence analysis, the optimum preheat temperature required to evacuate the low temperature electron traps was determined as 170 °C. It was also presented that CaSO:Nd samples have the potential to be used as a dosimetric material with a linear dose sensitivity between 1 and 20 Gy (as TL dosimeter), and 1 and 10 Gy (as an OSL dosimeter) when they are exposed to beta irradiation. In addition, the full width at the half maximum (FWHM) values of the main TL peaks presented no independence of HR.