In this article, we report a one-pot synthesis strategy to directly synthesize the hierarchical FeCu-ZSM-5 zeolite. Its physicochemical properties were studied by various characterization techniques and catalytic performance was tested in selective catalytic reduction (SCR) of NO with NH 3 as reductant. The characterization results show that: compared with three reference zeolites Fe/ZSM-5, Cu/ZSM-5, and Fe/Cu/ZSM-5 prepared through an incipient wetness impregnation method, the synthesized FeCu-ZSM-5 zeolite exhibits hierarchical micro-mesoporous structures, more Fe 3 + in zeolite framework, and larger isolated Cu 2 + species. Therefore, when used as a catalyst in NH 3 -SCR, the resulting hierarchical FeCu-ZSM-5 catalyst shows better catalytic performance (high NO conversion and N 2 selectivity) in a wide temperature window and higher hydrothermal stability than the three reference catalysts. Our work provides a simple and facile route to prepare the promising NH 3 -SCR catalyst for practical applications in controlling NO x emissions.[a] Dr.