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Effect of Fe3O4 segregation at grain boundaries on the electrical transport and magnetic properties of La0.67Ca0.33MnO3 is investigated. The experimental results show that the Fe3O4 segregation not only shifts the paramagnetic-ferromagnetic transition temperature of La0.67Ca0.33MnO3 to a lower temperature region but also induces a new transition in a lower temperature region. Meanwhile, the transition processes observed in both the resistivity and magnetization curves are obviously widened. Compared to pure La0.67Ca0.33MnO3, we assume that the Fe3O4 segregation level at the grain boundaries can modify the electrical transport and magnetic properties of La0.67Ca0.33MnO3.