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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]