Cu 0.5 Ni 0.5 Fe 2 O 4 nanoparticles have been synthesized in ethylene glycol solution and in deionised water. The glycothermal reaction was carried at 200 • C under gauge pressure of 100 psi. The hydrothermal treatment was done at 100 • C under zero pressure. Complete single-phase cubic spinel structure in the samples made by glycothermal (sample G) and hydrothermal (sample H) processes formed after annealing at 600 • C and 900 • C respectively. The coercive field of sample H increases from 72 Oe to 133 Oe after sintering at 700 • C and then decrease to 11 Oe on sintering at 1000 • C. This variation is attributed to surface effects and crossover from single to multidomain behavior due to increasing particle size.