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Nanocellulose is a renewable and biocompatible nanomaterial that evokes much interest because of its versatility in various applications. This study reports the production of nanocellulose from Agave gigantea (AG) fiber using the chemical-ultrafine grinding treatment. Chemical treatment (alkalization and bleaching) removed non-cellulose components (hemicellulose and lignin), while ultrafine grinding reduced the size of cellulose microfibrils into nanocellulose. From the observation of Transmission Electron Microscopy, the average diameter of nanocellulose was 4.07 nm. The effect of chemical-ultrafine grinding on the morphology and properties of AG fiber was identified using chemical composition, Scanning Electron Microscopy, X-ray Diffraction, Fourier Transform Infrared, and Thermogravimetric Analysis. The bleaching treatment increased the crystal index by 48.3% compared to raw AG fiber, along with an …