With the continuous expansion of the semiconductor industry, the number of discarded light-emitting diodes (LEDs) is rapidly increasing. LEDs contain a variety of valuable metals, particularly gallium (Ga), which mainly exists in the form of GaN within the light-emitting chips. As a rare and dispersed metal, gallium has been listed as a strategic resource in many countries. However, its current recycling rate remains low, and the supply security is relatively weak. Therefore, the efficient recovery of gallium from waste LEDs not only could alleviate the pressure on the resource supply but could also help reduce the potential environmental impact of electronic waste.

On the other hand, gallium oxide (Ga₂O₃), as a wide-bandgap semiconductor material, possesses excellent electrical, optical, and catalytic properties. Especially at the nanoscale, it exhibits a high specific surface area, enhanced interfacial activity, and superior electron transport characteristics, making it highly promising for applications in ultraviolet photodetectors, high-temperature electronic devices, gas sensors, and photocatalysis. Accordingly, synthesizing nanostructured Ga₂O₃ materials from recovered gallium represents a cutting-edge approach to combining resource recycling with the development of advanced functional materials.

This study proposes a resource recovery process centered on pyrolysis–ball milling–nitric acid leaching–precipitation synthesis, using nitric acid as the leaching agent to achieve selective and efficient gallium extraction from waste LEDs. Through an orthogonal experimental design, the leaching parameters are optimized to enhance the recovery performance. Furthermore, a controlled precipitation and thermal treatment strategy is employed to synthesize nanostructured Ga₂O₃ materials, providing both theoretical support and technical pathways for the resource utilization and functional reuse of electronic waste.