SUMMARY

Electrodeposition is a widely used manufacturing technology in industry due to its simplicity, low-cost and scalability for practical applications. In electrodeposition, the composition and morphology of yielded materials can be tuned by adjusting electrochemical parameters and electrolyte compositions. To reveal the insights of electrodeposition and develop rational design strategies, we designed a series of in situ XRD tools for electrodeposition, which allows for systematic investigation to reveal how deposition conditions impact the chemical/phase composition and morphology. Several model materials were studied. Cu-Zn alloy was first electrodeposited under different conditions to obtain desired compositions and morphology. Then Zn is electrochemically etched from Cu-Zn alloy to form 3D Cu as current collectors for Li-metal batteries. A quantification method for electrochemical deposition is developed with using Cu deposition as the model system, which quantitatively characterize the growth rate and texture formation. A high throughput in situ X-ray diffraction characterization platform is also developed to provide capability for the design and screening of complex metals and alloys under different electrochemical deposition/ dealloying conditions. To explore its potential applications in energy storage, we utilized this platform to investigate the plating process of Zn metal anodes because of its higher X-ray diffraction intensity compared to lithium. Zn electrodeposition under different current densities and a current density-texture relationship was found. The tools developed and insights gained in this dissertation have not only enhanced the design and performance of metal anodes for energy storage applications but also paved the way for the rational design and screening of new materials synthesis.