Chitin is the second most abundant polysaccharide in nature. This chapter provides information related to the preparation of chitin and chitosan whiskers. It represents the various methods of preparation of chitin and chitosan whiskers including steam explosion, acid hydrolysis, alkali treatment, grinding, and mixing. They were subjected to various chemical treatments to analyze their binding and extensive application of products. During the preparation of chitin and chitosan whiskers, their influence on time, temperature, and pressure was evaluated. Various spectroscopic techniques, like SEM, TEM, and AFM, were used to study the morphology, particle size, and surface topography of the prepared chitin and chitosan whiskers. In addition to their relatively easy availability, nontoxicity, biodegradability, and affordability of structural adaptation, the chitin and chitosan whiskers differ in morphology, which has led to their widespread applications in the biomedical and industrial fields.