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It is always desirable to entirely understand the related electrochemical and electrocatalysis reactions of fuel cells, which is essential in order for scientists to engineer better materials and devices for energy conversion. In this chapter, readers will see how powerful the electrochemical NMR combination will be to provide insights into the processes occurring inside fuel cells. With solid NMR spectroscopy to probe surface states under electric potentials, nanocatalysts and adsorbed ligand substances have been investigated. With the merits of high-resolution liquid NMR spectroscopy, soluble intermediates and products in electrochemical and electrocatalysis reactions can be real-time monitored and identified. Unless stated otherwise, liquid NMR spectra are described in this chapter for the demonstration of recent advances in methodology and appliancation for in situ electrochemical NMR studies. Under in situ and even operando conditions, a series of characterization and diagnosis approaches for fuel cells have been developed, which will provide opportunities to explore the full cell devices and accordingly improve their performances.

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