The ZrO 2 -embedded carboxy-functionalized h-BN composite, combined with graphene oxide (GO), formed a novel BN-COOH@ZrO 2 /GO composite. Structural characterization through IR, Raman spectroscopy, powder X-ray diffraction, and X-ray photoelectron spectroscopy supported the successful preparation of the composite, while scanning electron microscopy and transmission electron microscopy revealed its surface morphology and the presence of component materials. UV−vis spectroscopy (solid state) further supported these findings. Thermogravimetric analysis demonstrated enhanced thermal stability of the composite compared to GO. Electrical conductivity analysis showed that functionalization alone did not impart significant conductivity to insulating BN. However, integration with GO significantly enhanced conductivity. BN-COOH@ZrO 2 /GO exhibits electrochemical sensor activity for diclofenac sodium (DS) detection, achieving a low (limit of detection = 0.0146 μM) and high sensitivity (0.2464 μA μM −1 cm −2 ). The sensor showed high selectivity, reproducibility, and stability, effectively detecting DS in real samples with recovery rates ranging from 97.69% to 107.21%. This novel composite highlights its potential as an efficient material with enhanced thermal stability and electrical conductivity for detecting DS through cyclic voltammetry.