Engineering Nanoscale Zn ₁₀ In ₂ S ₁₃ (ZIS) Based Electrocatalysts via Micro Bubble Lithography (MBL) for Efficient Bifunctional Oxygen Electrocatalysis

Abstract Achieving a climate‐neutral energy future requires efficient, selective, and durable electrocatalysts for key reactions such as the oxygen evolution reaction (OER) and the 4e − oxygen reduction reaction (ORR), which predominantly produces hydroxide ions (OH − ), essential for metal–air batteries. This work presents a novel Microbubble Lithography (MBL)‐assisted microfabrication strategy to create highly ordered, nanostructured Zn₁₀In 2 S₁ 3 (ZIS)‐based metal chalcogenide architectures with precisely engineered surface topographies and electronic structures. The bottom‐up, template‐free lithographic method enables spatially controlled patterning and nanoscale tuning of active site exposure, allowing precise regulation of catalytic activity and selectivity. The MBL‐patterned ZIS demonstrates bifunctionality, achieving a highly selective 4e − ORR pathway favouring OH − production with an onset potential of −0.103 V vs. Ag/AgCl and stability beyond 15 h. It also delivers excellent OER performance with overpotentials of 100 mV at 10 mA cm − 2 and 600 mV at 50 mA cm − 2 , a Tafel slope of 120 mV dec −1 , and durability over 5000 CV cycles. This study highlights that microbubble‐ induced nanoarchitecture engineering synergistically enhances active site utilization and intrinsic electronic properties, guiding the design of next‐generation bifunctional electrocatalysts for sustainable energy conversion and durable metal‐air batteries.