We report high-temperature synchrotron X-ray diffraction (SXRD), magnetization, and current-voltage (I-V) characteristics for the samples of Co2.75Fe0.25O4 ferrite. The material was prepared by chemical reaction of the Fe and Co nitrate solutions at pH similar to 11 and subsequent thermal annealing. Physical properties of the samples were measured by cycling the temperature from 300 K to high temperature (warming mode) and returning back to 300 K (cooling mode). The lattice structure showed sensitivity to high measurement temperatures. Magnetization curves showed a defect-induced ferromagnetic phase at higher temperatures and superparamagnetic blocking of the ferrimagnetic particles near to 300 K or below. Electrical conductivity exhibited a thermal hysteresis loop at higher measurement temperatures. The samples exhibited new form (not studied so far) of surface magnetism in Co rich spinel oxides and irreversibility phenomena in the lattice structure, magnetization, and conductivity on cycling the measurement temperatures.