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CH4‐CO2 chemical looping is proposed for separate H2 and CO production using nanostructured Fe‐Ni looping materials. The product streams are obtained by first feeding CH4, which decomposes to H2 and carbon. The latter acts as reductant for the subsequent CO2 feed, which together with Fe re‐oxidation yields CO. After 25 CH4‐CO2 cycles, 10Fe5Ni@Zr has a higher H2 space–time yield than 10Fe0Ni@Zr (...