Hydrogen is an eco-friendly and efficient alternative to renewable energy. The electrolytic splitting of water for the production of hydrogen has undergone tremendous development in recent years, corresponding to the growing need for clean energy. Electrocatalysts play a crucial role in hydrogen evolution reaction (HER) electrolysis owing to their diminishing overpotential. On the other hand, oxygen evolution reaction (OER) has slow kinetics that limit its electrochemical activity, requiring the generation of alkaline water oxidation electrocatalysts. While noble metal electrocatalysts possess better activity in OER and HER, their availability and high cost render them unattainable. Transitional metal-based electrocatalysts have shown promise in addressing these drawbacks. Prussian blue analogues (PBAs) are open-framework metal-organic frameworks (MOFs) with transition metal content, allowing for tailored physicochemical properties and potential water splitting applications. However, their limited surface area and inferior electrical conductivity minimize their activity in water-splitting processes, which inevitably diminishes their overall efficiency. Interestingly, the carbon-based electrocatalysts, especially zero-dimensional graphene quantum dot (GQD), have gain attentions due to their nanosized, capable of providing uniform coverage of the intended substance. By considering this, incorporating GQD into electrocatalysts, the electrical conductivity can be improved, leading to enhanced kinetic transport properties and providing excellent stability of catalysts. Heretofore, in this thesis, we aimed to establish tandem surface engineering for high-efficiency PBAs as noble metal-free electrocatalysts for water splitting, as the PBA still suffers from the lack of low surface area and electronic conductivity.

In Chapter 4, tandem surface engineering via graphene quantum dots-assisted fluorinated NiFe Prussian blue analogue for OER was proposed: the first strategy involved surface reconstruction through the facile hydrothermal process of fluorination on NiFe PBA surfaces. The second strategy involved F-NiFe PBA modification by introducing GQD. The F- ions may participate in the change of the electronic structure without changing the framework structure of NiFe PBA, while the GQD will leading to enhance the catalytic activity. GQD/F-NiFe PBA has exhibited an overpotential of 318 mV at 50 mA cm-2 for OER and remains stable under a high current density. It is interesting to bring up that the F doping that will reconstruct the surface of NiFe-PBA and could support the GQD would alter the surfaces chemistry of F-NiFe PBA, which is favorable to increasing the electrical conductivity and electrocatalytic OER performance. The synergistic interactions of both surface reconstruction from F- ions and higher surface oxidation of GQD bring about a tremendously stable structure, boosting the performance of NiFe PBA.

Furthermore, in Chapter 5, we propose to enhance the GQD decorated CoFe PBA by activating the surface engineering process through mild oxidation of UV/ozone treatment for HER. By incorporating GQD to provide an abundant lattice mismatch in the CoFe PBA electronic structures to facilitate faster kinetic and electron transport performance. X-ray absorption spectroscopy (XAS) revealed the role of UV/ozone activation, which effectively induced the electron density of Co atoms and confirmed that the transition metal Co elements are the most asymmetrically connected to oxygen atoms. The optimized as-assembled CoFe PBA/GQD-UV shows remarkable electrocatalytic performance toward HER, with a low overpotential of 77 mV for reaching a current density of 10 mA cm-2 with excellent durable current retention of 99.8% for 12 h under an extremely high current density of 500 mA cm-2 in an acidic solution.

This research is crucial because it provides a new perspective on the surface engineering strategy of effective catalysts for water splitting, leading to the establishment of an affordable and sustainable preparation strategy for water splitting catalyst materials.

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