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The in situ exsolution technique of nanoparticles has brought new opportunities for the utilization of perovskite‐based catalysts in solid oxide cells. However, the lack of control over the structural evolution of host perovskites during the promotion of exsolution has restricted the architectural exploitation of exsolution‐facilitated perovskites. In this study, we strategically broke the long‐standing trade‐off phenomenon between promoted exsolution and suppressed phase transition via B‐site supplement, thus broadening the scope of exsolution‐facilitated perovskite materials. Using carbon dioxide electrolysis as an illustrative case study, we demonstrate that the catalytic activity and stability of perovskites with exsolved nanoparticles (P‐eNs) can be selectively enhanced by regulating the explicit phase of host perovskites, accentuating the critical role of the architectures of perovskite scaffold in catalytic reactions occurring on P‐eNs. The concept demonstrated could potentially pave the way for designing the advanced exsolution‐facilitated P‐eNs materials and unveiling a wide range of catalytic chemistry taking place on P‐eNs. [ABSTRACT FROM AUTHOR]

Ca 0.01 La 0.99− x Sm x NbO 4− δ ( x =0, 0.1, 0.2, 0.4, 0.6, 0.8, 0.99) is prepared by using a solid reaction route, and single phase is achieved. Structural and phase transformation of Ca 0.01 La 0.99− x Sm x NbO 4− δ have been characterized by high temperature X-ray diffraction. The lattice parameters a , b , c decrease and γ increases with increasing x , at both room and high temperature. The phase transformation temperature increases linearly with increasing x for Ca 0.01 La 0.99− x Sm x NbO 4− δ . The electrical conductivity of Ca 0.01 La 0.99− x Sm x NbO 4− δ is measured in wet air. A clear relationship between the structural, phase transformation and electrical conductivity of Ca 0.01 La 0.99− x Sm x NbO 4− δ is built, which will provide a guideline to tailor the electrical conductivity. [ABSTRACT FROM AUTHOR]