Zinc sulfide (ZnS)–poly (arylene ether ketone) (PAEK) nanocomposites (NCs) were synthesized in dimethylformamide solution by carboxylic-functionalized hyperbranched PAEK (ACA-HPAEK) as surface modifier without ligand exchange. The changes in the photoluminescence (PL) of ZnS-PAEK NCs with different reaction times, zinc ion (Zn2+)/thiourea ratios, and ZnS/ACA-HPAEK ratios were investigated, aiming at producing the novel NC with distinct luminescence properties. Fourier transform infrared spectroscopy and high-resolution analytical transmission electron microscopy were used to confirm the formation of ZnS quantum dots with small particle size. Ultraviolet–visible spectroscopy and PL spectroscopy were used to characterize the luminescence properties of NCs. The results of differential scanning calorimetry and thermogravimetric analysis showed that the NCs exhibited excellent heat resistance. At last, the novel ZnS-PAEK NCs with distinct luminescence properties and excellent heat resistance were obtained.
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