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Nanocomposite films of polymethylmethacrylate PMMA with Sn0.75Fe0.25S2 nanoparticles (NPs) were fabricated by both thermolysis and casting techniques. Changes in PMMA/Sn0.75Fe0.25S2 nanocomposite (NCP) due to gamma irradiation have been measured. XRD results indicate that the gamma doses of 10–80 kGy cause intermolecular crosslinking that reduces the ordered portion in the NPs. Bonding between the NPs and the host PMMA was confirmed by FTIR. TGA results indicate an enhancement in thermal stability in the NCP films irradiated with doses 20–80 kGy. The optical band gap was reduced from 3.23 to 2.47 eV upon gamma irradiation up to 80 kGy due bonding between the NPs and PMMA which enhanced the amorphous part of the NPs. Finally, the color variation between the blank and irradiated films (ΔE) was determined. Color changes immensely when the PMMA/Sn0.75Fe0.25S2 NCP films are gamma irradiated. Values of ΔE were as much as 31.6 which is an acceptable match in commercial reproduction on printing presses.