Superlattices are attracting extensive attention due to their unique properties. Nevertheless, the observations of superlattices are limited to those layered structures with weak interlayered interactions, and the effect of the superlattice in metal-based nanostructures on catalysis is unexplored yet. We here report a facile wet-chemical method for synthesizing two-dimensional Ru multilayered nanosheets (Ru MNSs) with a superlattice. Characterizations reveal that the superlattice is formed by stacking Ru layers with twisted angles from 2°to 30°. Owing to the strong synergy between the adjacent layers, Ru MNSs can serve as an efficient catalyst for the alkaline hydrogen evolution reaction (HER). Theoretical calculations reveal that the superlattice can induce the strain effect, which leads to lattice contraction and weak *H adsorption ability, as a result of improved HER performance. This work sheds new light on the utilization of the superlattice on enhancing catalysis in metal-based materials.

Electrochemical tip-enhanced Raman spectroscopy (EC-TERS) is a powerful technique for the in situ study of the physiochemical properties of the electrochemical solid/liquid interface at the nanoscale and molecular level. To further broaden the potential window of EC-TERS while extending its application to opaque samples, here, we develop a top-illumination atomic force microscopy (AFM) based EC-TERStechnique by using a water-immersion objective of a high numerical aperture to introduce the excitation laser and collect the signal. This technique not only extends the application of EC-TERS but also has a high detection sensitivity and experimental efficiency. We coat a SiO2 protection layer over the AFM-TERS tip to improve both the mechanical and chemical stability of the tip in a liquid TERS experiment. We investigate the influence of liquid on the tip–sample distance to obtain the highest TERS enhancement. We further evaluate the reliability of the as-developed EC-AFM-TERS technique by studying the electrochemical redox reaction of polyaniline. The top-illumination EC-AFM-TERS is promising for broadening the application of EC-TERS to more practical systems, including energy storage and (photo)­electrocatalysis.

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