Gd 2 (SO 4 ) 3 ·8H 2 O , Gd 2 O 2 SO 4 , and Gd 2 O 2 SO 4 :Eu 3+ nanoparticles have been synthesized in the presence of Gd 3+ ion and sodium dodecyl sulphate (SDS) by the simple complexationthermal decomposition (CTD) method. The structural analysis, growth mechanism and optical properties of the Gd 2 (SO 4 ) 3 ·8H 2 O, and Gd 2 O 2 SO 4 is described by diffraction pattern, functional group analysis, Raman, morphology, elemental analysis, and absorbance spectra. The most intriguing future was that the Gd 2 O 2 SO 4 nanoplates are in the range of 42-50 nm without adding any external stabilizer. The study results revealed that the Gd 2 O 2 SO 4 nanoparticles with orthorhombic structure are having a band gap of 3.12 eV. Furthermore, Gd 2 O 2 SO 4 shows an intense red photoluminescence associated with the 5 D 0 → 7 F 2 transition in the presence of Eu 3+ .The results suggest that the Gd 2 O 2 SO 4 :Eu 3+ nanophosphors, may have a beneficial approach in the field of biomedical application as luminescent probe/labels.