AbstractThis study focuses on developing and characterizing polymer‐based materials for high‐performance applications as proppants in oil and gas wells. We use styrene‐divinylbenzene (Sty‐DVB) copolymers as the base, incorporating additives such as polybutadiene (PB) and polyphenylene oxide (PPO). Materials were synthesized via batch polymerization, enabling the production of multiple formulations in a single step, which accelerates data analysis and reduces experimental workload. Key properties such as glass transition temperature (Tg), fracture toughness, and deformation resistance were evaluated. The optimal DVB content (10–12 wt.%) balanced crosslinking density and mechanical performance. PB enhanced fracture toughness by up to 100% at concentrations below 19 wt.%, but lowered Tg. PPO, fully dissolved in the Sty‐DVB matrix, increased Tg above 130°C and significantly improved ultimate stress and strain (up to 400%) and also fracture toughness (up to 100%). This study lays the groundwork for developing lightweight, high‐performance polymeric materials for demanding applications.