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While heterogeneous photocatalysis holds great promise for solar energy conversion, increasing photocatalytic efficiency remains a challenge due to the complexity of underlying mechanisms. Time-resolved spectroscopic techniques provide valuable insights into photocatalytic processes. This chapter reviews recent applications of these techniques to both well-established photocatalysts and to emerging energy materials, including hybrid perovskites and covalent organic frameworks. We describe applications of transient absorption spectroscopy and time-resolved terahertz spectroscopy to reveal intermediates, charge carrier transfer and recombination dynamics, and photophysical processes. Moreover, we provide an overview of the emerging technique of two-dimensional electronic spectroscopy, which has recently offered unprecedented insights into ultrafast dynamics and quantum coherent phenomena in photocatalytic materials. This chapter thus intends to inspire researchers on how time-resolved spectroscopies could help understand the underlying mechanisms, which will be the key to achieving sustainable sunlight conversion technologies based on photocatalysis.

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