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Engineering surface-active facets of metal cocatalysts is one of the most widely explored strategies to develop advanced photocatalysts and promote photocatalytic solar energy conversion. Here, the surface-active facets of Pd nanocrystals in Pd/g-C 3 N 4 photocatalyst was related to the injection flow rate of PdCl 2. When PdCl 2 was injected at a low flow rate of 7.5 mL/h (7.5-Pd/g-C 3 N 4), the Pd nanocrystals were uniformly dispersed onto the g-C 3 N 4 with exposed low-index {100} and {111} surface-active facets. However, increasing the injection flow rate to 150 mL/h (150-Pd/g-C 3 N 4) formed Pd nanocrystals where only the {100} surface-active facet was exposed. Under visible light irradiation, the 7.5-Pd/g-C 3 N 4 nanocomposite exhibited excellent water splitting activity for hydrogen production (7.61 mmol g−1 h−1), which was significantly better than with the 150-Pd/g-C 3 N 4 nanocomposite (3.3 mmol g−1 h−1). Theoretical calculations and experimental results confirm the importance of the {111} surface-active facets in the 7.5-Pd/g-C 3 N 4 nanocomposite for promoting photocatalytic activity. [Display omitted] • The Pd/g-C 3 N 4 photocatalyst was prepared in a simple one-pot synthesis method. • The surface-active facets of Pd nanocrystals in Pd/g-C 3 N 4 was controlled by the injection flow rate of PdCl 2. • 7.5-Pd/g-C 3 N 4 nanocomposite exhibited excellent photocatalytic activity for H 2 production. • 7.5-Pd/g-C 3 N 4 nanocomposite also shown good performance in varied photocatalytic reactions. [ABSTRACT FROM AUTHOR]

The construction of efficient and stable non-noble metal bifunctional electrocatalysts for the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER) presents a challenge in electrocatalytic water splitting. CoS 2 is a promising electrocatalyst that could replace precious metals. In this work, a series of Co-MOF precursors having average particle sizes ranging from the nanometer to the micron scale (86–1084 nm) were synthesized in an unprecedented attempt; Co/CoS 2 heterojunction embedded in nitrogen doped carbon framework (Co/CoS 2 @NC) was prepared through further carbonization and sulfurization. The samples were characterized and evaluated by X-ray powder diffractometer (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and electrochemical techniques. The results indicate that when the size of Co-MOF is less than 300 nm, the cubic structure framework easily collapses to form the spherical structure during the carbonization process. The catalytic activity of Co@NC is size-dependent; Co/CoS 2 @NC exhibited the best performance among the series, with an overpotential of 188 mV for HER and 349 mV for OER at a current density of 10 mA cm−2. This work provides experimental guidance for the design and synthesis of low-cost, efficient, and robust Co-based electrocatalysts. • With Co-MOF cubic nanoparticles as the precursor, Co/CoS 2 @NC was prepared through carbonization and sulfurization. • Co/CoS 2 @NC exhibited the best performance among the series. • The catalytic activity of Co@NC is size-dependent. • This work provides a guidance for the design and synthesis of low-cost, efficient, and robust Co-based electrocatalysts. [ABSTRACT FROM AUTHOR]

Nano-structuring and metal-support interactions are effective methods to improve the electrocatalytic activity of heterogeneous catalysis. In this study, we synthesized nitrogen-doped porous carbon substrates by using a SiO 2 -protected calcination strategy with ZIF-8 as a precursor. The experimental results revealed the prepared porous nitrogen-doped carbon (PNC) to have high dispersion, large specific surface area, and rich pore structure, allowing high exposure of active sites. The carbon support showed optimum characteristics to deposit precious metals with small particle sizes. X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) showed that the N groups on the PNC substrates served as coordination sites for Ru, allowing the formation of ultrafine nanoclusters. The Ru clusters showed good metal dispersion, exposing more active sites and improving the utilization of the precious metal. At a current density of 10 mA/cm2, Ru/PNC showed a minimum overpotential of 40 mV. This work provided a simple and effective method for the preparation of excellent carbon substrates and the synthesis of metal clusters with small particle sizes. N-doped porous carbon (PNC) was synthesized by a SiO 2 -protected calcination strategy by using ZIF-8 as precursor. Compared with Ru/NC, the HER catalytic performance of Ru/PNC catalysts with Ru clusters has been significantly improved. [Display omitted] • Ru nanoclusters was prepared by the EG microwave-assisted method. • N-doped porous carbon was synthesized by a SiO 2 -protected calcination strategy. • Ru/PNC catalyst showed excellent HER-catalytic performance in acidic media. [ABSTRACT FROM AUTHOR]