In this project, the preparation and application of highly effective nanocatalysts toward CO2 reduction and formic acid oxidation reactions will be investigated. In these carbon-based energy cycles, if energy from renewable energy can be used to synthesize fuels from captured CO2, the storage of these energy sources is chemical energy based with higher energy density and ease of use within existing infrastructures when compared with electricity in batteries or hydrogen energy. Therefore, we will explore the CO2 reduction catalysts systematically. In the first year, we will use the reverse reaction of CO2 reduction, formic acid oxidation reaction, to screen the catalysts and the electrochemical analyzer will be used. In the second year, the Au-based nanocatalysts will be prepared and gas chromatography will be constructed to analyze the gaseous product such as CO and CH4 during CO2 reduction. In the third year, the Pd-based nanocatalysts will be prepared and high performance liquid chromatography will be constructed to analyze the liquid product such as formic acid during CO2 reduction. It has been reported that the faradaic efficiency of electrode materials such as Pt, Pd, Au, and Ag for CO2 reduction is highly related to their structures (alloy or core/shell), morphology (size, aspect ratio, and thickness of the shell), supports (carbon black and carbon nanotubes) and electrolytes. We will combine the synthesis of materials with two advanced in-situ technologies, including X-ray absorption spectroscopy (XAS) and scanning transmission electron microscopy (STEM), to elucidate the electronic states, atomic arrangements, and morphological and structural evolution during heating under specific atmospheres. The in-situ XAS will be performed in National Synchrotron Radiation Research Center in Taiwan while the in-situ STEM will be conducted in Department of Chemical Engineering and Materials Science, University of California.The combination of experimental, spectroscopic and microscopic results will open new insights into the design of highly effective and stable catalysts toward CO2 electrochemical reduction.