Electric power system applications demand for high‐temperature dielectric materials. The improved performance of polymer nanocomposites requires improvement in their thermal conductivity & stability, dielectric stability and processing technique. However, they often lose their dielectric properties with a rise in temperature. Here, we offer a solution by incorporating electrically conducting material (MXene) and semiconducting inorganic nanoparticles (ZnO NPs) into an insulating PMMA polymer matrix to maintain high dielectric constant, both at the room and high temperature. Therefore, to achieve desirable thermal and dielectric properties is the main objective of the present study based on the homogeneous distribution of the nanofillers by in‐situ bulk polymerization assisted by strong sonication in the corresponding polymer. The introduction of MXene and ZnO NPs into the PMMA not only acquires a substantial increment in the dielectric constant, to attain a value 437, with minimum energy loss of 0.36 at 25 Hz, but also improves the thermal conductivity of PMMA up to 14 times by causing the reduction of thermal resistance, which is actually responsible for the poor thermal conductivity of amorphous pure PMMA polymer. More importantly, hybrid PMMA/4:2 wt% MXene:ZnO nanocomposite leads to an excellent thermal stability. Moreover, further characterization of the synthesized nanocomposites by FTIR, SEM and XRD leads to the evaluation of strong interaction of ternary components with PMMA matrix.
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