Identification of Volume Fractions of Components in a Polymer Composition Using Dielectric Spectroscopy

Insufficient reproducibility of physical and technical properties limits the wider application of polymer composites with dispersed particles. This issue arises from “parasitic” components in the polymer composition introduced during production and their mutual arrangement within the composition. This paper proposes a method for quantifying the proportion of parasitic components, accounting for their spatial arrangement, by combining dielectric spectroscopy, photosedimentation, electron microscopy, and mechanical testing. Polymer films of polymethyl methacrylate (PMMA) with zinc oxide particles were prepared using an in situ approach: zinc hydroxide particles were synthesized in mini‐reactors within a PMMA/toluene solution, followed by explosive destruction and dispersion of the particles. Subsequent heating at 130°C ± 1°C converted the hydroxide to zinc oxide directly in the films. The proposed method revealed that vacuoles accounted for 10%–20% of the sample volume, exceeding the critical pore fraction that significantly affects mechanical performance. In contrast, the volume fraction of the particles themselves was negligible, not exceeding 0.1%. This analytical approach enables identification of the internal structure of polymer composite products and provides a basis for predicting their mechanical properties.