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In present work, agricultural residue Zea mays husk has been converted into cellulose using alkali and bleaching treatment. Further, the cellulose has been converted to nanocellulose through the acid hydrolysis method followed by ultrasonication. The Crystallinity and functional group analysis was studied using X‐ray diffraction (XRD) and Fourier‐transform infrared spectroscopy (FT‐IR), respectively. The surface morphological investigation of prepared Zea mays husk nanocellulose was carried out using scanning electron microscope (SEM) transmission electron microscope (TEM), and atomic force microscopy (AFM). The thermal stability was investigated using thermogravimetric and derivative thermal analysis (TGA/DTA). The obtained results revealed semi‐crystallinity nature, good thermal stability, and fibrous nanocellulose nature with agglomeration.

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