One-Step Synthesis of Copper and Cupric Oxide Particles from the Liquid Phase by X-Ray Radiolysis Using Synchrotron Radiation

Abstract

The deposition of copper (Cu) and cupric oxide (Cu4O3, Cu2O, and CuO) particles in an aqueous copper sulfate (CuSO4) solution with additive alcohol such as methanol, ethanol, 2-propanol, and ethylene glycol has been studied by X-ray exposure from synchrotron radiation. An attenuated X-ray radiation time of 5 min allows for the synthesis of Cu, Cu4O3, Cu2O, and CuO nano/microscale particles and their aggregation into clusters. The morphology and composition of the synthesized Cu/cupric oxide particle clusters were characterized by scanning electron microscopy, scanning transmission electron microscopy, and high-resolution transmission electron microscopy with energy dispersive X-ray spectroscopy. Micro-Raman spectroscopy revealed that the clusters comprised cupric oxide core particles covered with Cu particles. Neither Cu/cupric oxide particles nor their clusters were formed without any alcohol additives. The effect of alcohol additives is attributed to the following sequential steps: photochemical reaction due to X-ray irradiation induces nucleation of the particles accompanying redox reaction and forms a cluster or aggregates by LaMer process and DLVO interactions. The procedure offers a novel route to synthesize the Cu/cupric oxide particles and aggregates. It also provides a novel additive manufacturing process or lithography of composite materials such as metal, oxide, and resin.