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A new perovskite oxide, (Sr0.67Sm0.33)(Mn0.33Ti0.67)O3, was synthesized at 1573 K in an Ar flow. The structure of the oxide was determined to be orthorhombic with the space group of Pnma using X‐ray diffraction and electron diffraction. High‐resolution transmission electron microscope (HRTEM) images of the oxide revealed that nano‐domain structures were formed by twinning due to a phase transition. This is the first time that phase transition of the oxide has been observed in situ using a heating stage in a TEM. The high‐temperature phase possessed an orthorhombic structure with the space group of Imma, which appeared above 723 K.