In Situ Analysis of Growth Behaviors of Cu2O Nanocubes in Liquid Cell Transmission Electron Microscopy

• Published in: Analytical chemistry (Washington) Vol. 91; no. 15; pp. 9665 - 9672
• Main Authors: Lin, Ya-Hsuan, Chen, Jui-Yuan, Chen, Fu-Chun, Kuo, Ming-Yu, Hsu, Yung-Jung, Wu, Wen-Wei
• Format: Journal Article
• Language: English
• Published: Washington American Chemical Society 06.08.2019
• Subjects: Analytical chemistry; Catalysis; Chemical properties; Chemistry; Copper oxides; Electron beams; Electron radiation; Electronics industry; Kinetics; Liquid phases; Metal oxides; Metals; Morphology; Nucleation; Organic chemistry; Oxides; P-type semiconductors; Photovoltaic cells; Radiation; Reaction kinetics; Reducing agents; Solar cells; Transmission electron microscopy
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/acs.analchem.9b01192

Metal oxides have attracted substantial attention over the years and are commonly used in the semiconductor industry because of their excellent physical and chemical properties. Among the various metal oxides, cuprous oxide (Cu2O) is regarded as a promising material. It is inexpensive, earth-abundant, and nontoxic; therefore, it can be used in catalysis, sensors, solar cells, and p-type semiconductors. However, the redox reaction of Cu2O is still uncertain. The size, morphology, and structure of Cu2O strongly influence its properties. In this work, we developed a new synthesis method of Cu2O that involves reducing the precursor by an electron beam without reducing agent. The growth process of Cu2O nanocubes was observed via in situ liquid cell transmission electron microscopy (in situ LCTEM). The nucleation kinetics, oscillating growth behavior, and redox reaction of the Cu2O nanocubes in the liquid phase were systematically studied. Cu2O exhibited a round shape at the beginning and transformed into a cubic shape afterward. Interestingly, the Cu2O nanocubes grew clearly under long-term observation; however, their diameters increased and fluctuated during the short-term observation. The electron beam not only stimulated the solution to reduce the nanocubes but also caused electron radiation effect to the nanocubes. During the Cu2O growth and dissolution, the cubic shape evolved with specific planes in the {100} family. Our direct observation sheds light on the preparation of Cu2O by a reduction method, extending the study of reaction kinetics and providing a new way to synthesize metal oxides.