Using 2 M HCl as a catalyst, the copolymer was synthesized by condensation of sulphanilic acid (SA), thiourea (T), and formaldehyde (F) in a 1:1:2 monomer ratio. Metal complexes were synthesized by employing this terpolymer as a ligand with two transition metal ions, Cu(II) and Ni(II), in a 2:1 molar ratio. The reaction was run for three hours at 60 °C with effective reflux. UV-visible spectroscopy, NMR, FTIR, SEM, and XRD were used to analyze the resulting metal complexes. The elemental composition of the SATF-I-M copolymeric metal complexes was examined using elemental analysis. The thermal durability of the terpolymer ligand metal complexes was assessed using thermogravimetric analysis (TGA), and the activation energy was calculated using the Freeman–Carroll and Sharp–Wentworth techniques based on TGA data. The RF-501 (PC) S CE (LVD) MODEL PL spectrometer was used to measure the spectra of complexes containing the two transition metal ions in order to study the photoluminescence characteristics of the newly generated copolymeric metal complexes. The main goal of this study is to create new polymeric metal complexes and investigate their photoluminescent properties, while recognizing the important contributions of current researchers in the area.