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A series of Bi1–xLaxFeO3 samples with 0.00 ≤ x ≤ 0.30 was synthesized by the sol–gel method. The effects of lanthanum concentration on the phase formation, microstructure and cycloidal spin ordering were studied using X-ray diffraction, scanning electron microscopy and Mössbauer spectroscopy. The crystal structure of the La-doped bismuth ferrite transformed from rhombohedral R3c (x ≤ 0.05) to a mixture of R3c and cubic Pm3m (0.07 ≤ x ≤ 0.15) and finally to a mixture of R3c, Pm3m and orthorhombic Pbam (0.20 ≤ x ≤ 0.30). The Pbam phase, with characteristic porous microstructure shown by microscopy images, was observed in Bi1–xLaxFeO3 compounds for the first time. Based on the Mössbauer spectroscopy, it was found that the cycloidal spin ordering started to disappear at x = 0.07. With increasing La concentration the share of the cycloid decreased from 100% at 0.00 ≤ x ≤ 0.05 to 0% at x = 0.30. At the beginning, for x ≤ 0.02, the anharmonicity parameter, m, of the cycloidal spin ordering was about 0.5, which is typical of a pure BiFeO3 compound. In the range 0.05 ≤ x ≤ 0.25, the m parameter was of the order of 0.1, which indicated the practically harmonic character of the cycloid. The structural transition at x = 0.07 was accompanied by a substantial increase in magnetization.
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