The micro-level magnetic alignments of zinc ferrite nanoparticles synthesized by sol–gel method were investigated using magnetization study, neutron diffraction and Mo¨ssbauer spectroscopy. Magnetization behavior of the sample clearly indicates the presence of superparamagnetism. The neutron diffraction was performed at seven different temperatures between 6 K and 300 K. The cation distribution is found to have a variation from the from normal spinel structure. Both A and B site magnetic moment values found to vary with temperature which is found to correlates with variations in bond lengths and lattice constants. The Mo¨ ssbauer spectrum at room temperature shows typical doublet while the spectrum 5 K shows well defined sextet. The two sub-spectra in the sextet resolves well by the application of 5 T magnetic field and the noncollinear nature of magnetic alignment with in the tetrahedral and octahedral sites of zinc ferrite are deduced.