Over the last few decades, nanotechnology has gained huge interest due to its extensive application in various fields including catalysis, electronics, optics, energy, and environment. The design and controlled synthesis of advanced nanomaterials with unique properties make them highly attractive in these fields. Nanomaterials can be classified into one-, two-, and three-dimensional materials. The main characteristic of nanostructured materials is their surface reactivity due to their active surface functional groups. The control of the size, shape, and nature of nanoparticles is strongly influenced by the synthetic route applied during the preparation step (i.e. hydrothermal, solvothermal, combustion, sol-gel). The Special Issue of Nanomaterials, entitled, "Tuning the physicochemical properties of nanostructured materials through advanced preparation methods," contains the contribution of research groups from different fields and discuss the recent developments in nanomaterials with regard to the preparation method used.