Hollow NiCo‐LDH Nanocage Derived From ZIF‐67 as an Efficient Catalyst for the Thermal Decomposition of Ammonium Perchlorate

Heterogeneous catalysis achieves efficient thermal decomposition of ammonium perchlorate (AP) by creating abundant catalytically active sites and optimizing mass transfer and diffusion processes. Based on this, hollow nickel–cobalt‐layered double hydroxide (H‐NiCo‐LDH) nanocages derived from metal–organic frameworks (MOFs) were successfully synthesized using an etching‐deposition‐growth strategy. The hollow structure and surface mesopores of H‐NiCo‐LDH not only expose more abundant catalytically active sites but also enhance the mass transfer and diffusion efficiency of gas‐phase intermediate products. The bimetallic synergy between Ni and Co effectively modulates the electronic structure, facilitating electron transfer during the catalytic reaction and promoting the deep oxidation of NH 3 to higher‐valence nitrogen oxides. Performance tests demonstrate that adding 5% H‐NiCo‐LDH significantly advances the high‐temperature thermal decomposition temperature of AP by 109.7°C and markedly increases the content of higher‐valence nitrogen oxides in the decomposition products. Furthermore, incorporating H‐NiCo‐LDH shortens the overall combustion time of AP while enhancing the flame brightness. This work not only demonstrates exceptional performance of H‐NiCo‐LDH in catalyzing AP thermal decomposition but also provides novel insights for developing efficient AP thermal decomposition catalysts through structural design and composition regulation.