The book deals with novel aspects and perspectives in metal oxide and hybrid material fabrication. The contributions are mainly focused on the search for a new group of advanced materials with designed physicochemical properties, especially an expanded porous structure and defined surface activity. The proposed technological procedures result in an enhanced activity of the synthesized hybrid materials, which is of great importance when considering their potential fields of application. The use of such materials in different technological disciplines, including aspects associated with environmental protection, allows for the verification of the proposed synthesis method. Thus, it can be stated that those aspects are of interdisciplinary character and may be located at the interface of three scientific disciplines—chemistry, materials science, and engineering—as well as environmental protection. Furthermore, the presented scientific scope is in some way an answer to the continuous demand for such types of materials and opens new perspectives for their practical use