This chapter covers different routes of preparation of hierarchical nanostructures (HNS) of titanium dioxide. Keeping the interest in developing modern and sustainable methods of materials chemistry, this chapter focuses on synthesis routes for TiO 2 HNSs reported by researchers from all over the world. The chapter includes the details of chemical reactions taking place during the synthesis and the effects of various process parameters like: type of surfactants, organic/inorganic titanium salts, temperature and pressure on products. The obtained TiO 2 HNSs from different synthesis routes are subsequently compared in terms of their morphology, crystallite size, surface area, particle size and phase. The merits and demerits of all synthesis techniques are also added for comprehensive information. At the end, various applications of HNSs are discussed and their performance is analyzed with respect to the morphologies obtained from different synthesis techniques.

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