Harnessing High‐Energy Ionizing Radiations for the Synthesis of Photoluminescent Nanomaterials

ABSTRACT Nanomaterials (NMs), especially the photoluminescent ones, have emerged as a vital class of functional materials, which underpin applications in energy, healthcare, and the environment. However, conventional synthetic methods often rely on toxic reagents and harsh conditions, limiting scalability and reproducibility. In this context, radiation‐assisted synthesis employing high‐energy (keV–MeV range) radiations, such as γ‐rays, electron beams (EBs), and ion beams, has gained prominence as a clean, controllable, and green approach for generating photoluminescent NMs. This review critically compiles and evaluates the progress made in radiolytic synthesis of photoluminescent NMs, highlighting how radiation‐generated reactive species govern nucleation, growth, and defect formation. Reported studies reveal that absorbed doses typically range from a few grays (Gy) to hundreds of kilograys (kGy), producing nanostructures from ultrasmall clusters to quantum dots (QDs) (< 10 nm), with photoluminescence (PL) QEs up to ∼70% in some core–shell and hybrid systems. The review also outlines current challenges and provides an outlook on emerging opportunities for defect engineering and hybrid nanocomposite design. Further, this report provides a single source of such information for the nanoscience fraternity. Overall, the article positions the radiation chemical approach as a versatile, promising strategy for the green and sustainable controlled production of a variety of photoluminescent NMs.