In this paper, we report a simple but novel aqueous solution based 'one-pot' method for preparation of (NiFe2O4)x -(SrFe12O19)1-x nanocomposites consist of hard ferrite-soft ferrite phases. A physical mixing method has also been employed to prepare nanocomposites having same compositions. The effects of synthetic methodologies on the microstructures of the nanocomposites as well as their magnetic and microwave absorption properties have been evaluated. Crystal structures and microstructures of these composites have been investigated by using X-ray diffraction, transmission electron microscope and scanning electron microscope.In the nanocomposites, prepared by both methods, presence of nanocrystalline NiFe2O4 and SrFe12O19 phases was detected. However, nanocomposites, prepared by one-pot method, possessed better homogeneous distribution of hard and soft ferrite phases than the nanocomposites, prepared by physical mixing method. Nanocomposites, prepared by one-pot method, demonstrated significant spring exchange coupling interaction between hard and soft ferrite phases and exhibited magnetically single phase behaviour. The spring exchange coupling interaction enhanced the magnetic properties (high saturation magnetization and coercivity) and microwave absorption properties of the nanocomposites, prepared by one-pot method, in comparison with the nanocomposites prepared by physical mixing method as well as pure NiFe2O4 and SrFe12 O19 nanoparticles. Minimum reflection loss of the composite was ∼-17 dB (i.e., 98% absorption) at 8.2 GHz for an absorber thickness of 3.2 mm. © 2015 American Scientific Publishers. All rights reserved.