The precipitation phenomenon of Ni3Cr phase in Ni-10 at% Cr alloy was studied through the isothermal annealing at different high temperatures. It was found that a metastable microstructure is formed during isothermal annealing at 850 ºC. The precipitation of ordered Ni3Cr phase was obtained during isothermal annealing at 950 and 975 ºC. Both processes increase the microstress in the matrix and consequently seemed to impose a heavily pinning action on the magnetic domain walls. The precipitation process was found to be controlled by a second order reaction, activated by an energy of 1.3 eV.