We report the green synthesis of novel ZrO2-Glycine nanocomposite referred to as ZrO2-Gly NC followed by its characterization using X-ray diffraction (XRD), Fourier transforms infrared (FT-IR) spectroscopy, SEM/EDX, and transmission electron microscopy (TEM) techniques. Further, the inhibition effect of the varying concentration of ZrO2-Gly NC on the corrosion of mild steel (MS) in 1 M HCl was investigated by weight loss and electrochemical measurements at 40–80 °C. The percentage inhibition efficacy of NC increased with the increase of concentration and temperature and reached about 81.01% at 500 ppm at 70 °C which decreased at 80 °C and exhibited 73.5% inhibition efficiencies. According to the polarization measurements, the investigated ZrO2-Gly NC works as a mixed-type inhibitor with predominantly inhibiting cathodic reaction. Also, the adsorption isotherm analysis indicated that the adsorption was spontaneous and followed the Langmuir adsorption isotherm. Furthermore, the contact angle measurement revealed the water-repelling property of the investigated inhibitor. The surface morphological study via SEM–EDS micrograph affirmed the appearance of a smooth surface in presence of inhibited media suggesting the formation of protective film by the adsorption of ZrO2-Gly NC on the surface of the MS even at higher temperature.