In this study, we present some results on the structure and properties of the solid solution of Bi0.5K0.5TiO3– BiFeCoO3 (BKT – BFCO) by Sol-gel method. Crystal structures of BKT – BFCO solid solutions were studies by XRD and Raman spectroscopy. The results were in good agreement with the previous reports of Bi0.5K0.5TiO3– BiFeO3 (BKT – BFO) and Bi0.5K0.5TiO3 – BiCoO3 (BKT – BCO) solid solutions. The magnetic properties were investigated via unsaturated M-H loop, which showed the competition of paramagnetic and antiferromagnetic ordering in BKT – BFCO. However, differing from the BKT – BFO and BKT – BCO solid solutions, the unclear values of saturated magnetism in BKT – BFCO raised the unexplained question, which needed further studies.