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For the first time, hafnia (HfO2) nanoparticles have been produced by photochemical synthesis. The photochemical route has been proven to be scalable, affordable, and straightforward to create monoclinic HfO2 nanoparticles with a size of tens of nanometers. The exploitation of this route offers a chance to create large amounts of dense nanoparticles with reduced costs and time of production for future creation of large area composite scintillators for fast timing techniques. Specific annealing treatments from 450 °C to 1000 °C have been targeted to tune the structural and morphological properties and optimize the luminescence of the nanoparticles. Hafnia nanoparticles annealed at low temperature display an amorphous structure. After thermal treatment at 1000 °C, HfO2 nanoparticles crystallize into a monoclinic phase, as evidenced by thermal analyses and X-ray diffraction. Radioluminescence and photoluminescence of HfO2 have been investigated at room temperature and 77 K. The emission band of hafnia covers a range from 300 to 600 nm and it can be attributed to defects within the matrix. In particular, the highest radioluminescence intensity appears in the crystalline sample annealed at 1000 °C, thanks to the higher crystallinity degree and the reduction of non-radiative channels and quenching defects. Photoluminescence and scintillation decay have evidenced the presence of the fast decay in the nanosecond time range. Thus, due to their size, density, and spectroscopic and timing features, monoclinic hafnia nanoparticles obtained by photochemical synthesis are attractive for potential creation of large area scintillating composites. [ABSTRACT FROM AUTHOR]