New Routes to Synthesizing an Ordered Perovskite CaCu3Fe2Sb2O12 and Its Magnetic Structure by Neutron Powder Diffraction.

A high-quality A,B-site-ordered double perovskite CaCu3Fe2Sb2O12 is prepared at ambient pressure by two routes, a wet-chemical procedure involving a mixture of CuO, Fe(NO3)3.9H2O, Ca(NO3)2, and Sb2O3 in citric acid and few HNO3 which is slowly evaporated and decomposed at 550 °C followed by a complex heating schedule (≈92% yield) and, secondly, by activating an oxide mixture of CuO, Fe2O3, Sb2O3, and CaCO3 by ball milling also followed by a complex heating schedule in which the amorphous material recrystallizes at < 820 °C (perovskite phase yield of 97%).