The intricate link between water and energy has raised the need for a pragmatic approach towards absolving the cycle for sustainable clean water purification. Therefore, significant attention has been drawn towards advanced materials which harness solar energy for effective water purification, and are also able to manage pollutants including pathogens, organics and heavy metals.This thesis explores the feasibility of fabricating titanium dioxide (TiO2)-based materials and its derivatives through sustainable synthesis approaches for the simultaneous degradation of organics and heavy metal recovery.In a preliminary study, TiO2 hollow spheres were fabricated using carbonaceous spheres as templates to investigate the structural morphology and photocatalytic oxidation of organic pollutants as well as changes to flux performance with and without photoinduced superhydrophilicity. The study demonstrated the formation of 300 nm Hierarchical TiO2 Hollow Spheres (HTHS) composed of 13.79 nm nanoparticulates. The HTHS revealed increased UV-absorbance which suggest light scattering by the hollow morphology which resulted in enhanced organic degradation. The flux evaluation observed increased flux due to superhydrophilicity for both HTHS and P25 nanoparticulate. The P25 demonstrated higher magnitude of flux increment due to higher surface to fluid contact. However, the advantage of larger microstructures is the pragmatic recovery of material and prevention of release out of the treatment process.Subsequently, improvements were made to design a novel synthesis process as well as to modify the TiO2 based spheres. The synthesis method considered a green synthesis pathway which applied minimal additives and involved a 2-step process. Firstly, the highly-concentrated metal nitrate solution penetrated the pores of the carbonaceous spheres followed by a solvothermal treatment in Tiglycerolate during which Ion Exchange occurs. The morphology of the spheres includes micro spheres consisting of hierarchical, multi-shell hollow spheres assembled by nanoparticulates. throughout the Ph.D journey. His life philosophies, view-points and approaches aided me both in research and provocative thoughts on making life choices. I could not have imagined having a better advisor and mentor for my Ph.D study. Special thanks to my Co-Supervisor Dr. Bai Hongwei whom I have worked with since joining Prof. Darren's Research Group. His stories and life journey has always been inspiring and his advice, guidance, insights, and of course time and friendship in Ph.D journey.