In the present work, pure nanocrystalline monoclinic Zirconia (ZrO2) has been successfully synthesized and optimized by the modified co-precipitation method. The concentration of raw material has been optimized with the fixed amount of precipitation agent (Potassium hydroxide
KOH). The thermal history of the precursor has been examined through TG/DTA analysis. All the samples are subjected to study the structure, fingerprints of the molecular vibrations, and morphology analyses. The representative sample has been analyzed through Transmission Electron Microscope
(TEM) and X-ray Photo Electron Spectroscopy (XPS) analyses. The as-prepared sample exhibits the better crystallinity and surface morphology with lesser particle size (190 nm) when the raw material concentration is 0.2 M. The as-prepared ZrO2 filler (0, 3, 6, 9, and 12 wt.%) is spread
through the enhanced polymer electrolyte P(S-MMA) (27 Wt.%)-LiClO4 (8 wt.%)-EC + PC (1;1 of 65 wt.%) complex system via solution casting method. The as-synthesized electrolyte films are examined via complex impedance analysis. P(S-MMA) (27 wt.%)-LiCIO4 (8 wt.%)-EC + PC
(1 ;1 of 65 wt.%)-6 wt.% of ZrO2 shows the high ionic conductivity 2.35 × 10–3 Scm–1. Temperature-dependent ionic conductivity studies obey the non-linear behavior. The enhanced ZrO2 has been expected to enhance the other electrochemical
properties of the lithium secondary battery.