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Diamond particles have great potential to enhance the mechanical, optical, and thermal properties of diamond-polymer composites. However, the improved properties of diamond-polymer composites depend on the size, dispersibility, and concentration of diamond particles. In the present study, diamond-polymer composites were prepared by adding the microdiamond particles (MDPs) with different concentrations (0.2-1 wt.%) into polymers (acrylate resins) and then subjected to a photocuring process. The surface morphology and topography of the MDPs-polymer composites demonstrated a uniform high-density distribution of MDPs for one wt.% MPDs. Thermogravimetric analysis was employed to investigate the thermal stability of the MDPs-polymer composites. The addition of MDPs has significantly influenced the polymers' thermal degradation. Absorption and emission spectra of thin layers were recorded through UV/Vis spectrophotometry and spectrofluorimetry. The obtained results revealed a significant increase in the fluorescence intensity of MDPs-polymer composites (at 1 wt.% of MDPs, a 1.5×, 2×, and 5× increase in fluorescence was observed for MDPs-green, MDPs-amber daylight, and MDPs-red resin, respectively) compared with the reference polymer resins. The obtained results of this work show the new pathways in producing effective and active 3D-printed optical elements.