Methane (CH₄) emissions significantly contribute to global warming and represent an untapped carbon resource. Cu-SSZ-13 zeolites are known for their high catalytic efficiency in CH₄-to-methanol (CH₃OH) conversion, but challenges such as over-oxidation and high activation temperatures persist. Our previous studies demonstrated that Fe incorporation enhances Cu-SSZ-13 performance by promoting the formation of active [Cu(trans-μ-1,2-O₂)Cu]²⁺ species, yet the structural dynamics of these sites remain unclear. This proposal aims to employ operando XAFS to elucidate the evolution of Cu and Fe species in Fe-Cu-SSZ-13 during CH₄ oxidation with N₂O. By correlating synthesis parameters, structural changes, and catalytic performance, we seek to establish design principles for efficient bimetallic zeolite catalysts for selective CH₄-to-CH₃OH conversion. conversion.