In this chapter, results of our recent investigations on the structural, microstructural and magnetic properties of Cu-based Heusler alloys and MFe2O4 (M = Mn, Fe, Co, Ni, Cu, Zn) nanostructures will be discussed. The chapter is divided into two parts, the first part describes growth and different characterizations of Heusler alloys while in the second part magnetic properties of nano-ferrites are discussed. The Cu50Mn25Al25-xGax (x = 0, 2, 4, 8 and 10 at %) alloys have been synthesized in the form of ribbons. The alloys with x ≤ 8 show the formation of Heusler single phase of the Cu2MnAl structure. Further increase of Ga content gives rise to the formation of γ-Cu9Al4 type phase together with Cu2MnAl Heusler phase. The alloys are ferromagnetically ordered and the saturation magnetization (Ms) decreases slightly with increasing Ga concentration. Annealing of the ribbons significantly changes the magnetic properties of Cu50Mn25Al25-xGax alloys. The splitting in the zero field cooled (ZFC) and field cooled (FC) magnetization curves at low temperature has been observed for alloys. Another important class of material is Nanoferrites. The structural and magnetization behaviour of spinel MFe2O4 nanoferrites are quite different from that of bulk ferrites. X-ray diffraction study revealed spinel structure of MFe2O4 nanoparticles. The observed ferromagnetic behaviour of MFe2O4 depends on the nanostructural shape as well as ferrite inversion degree. The magnetic interactions in Ce doped CoFe2O4 are antiferromagnetic that was confirmed by zero field/field cooling measurements at 100 Oe. Log R (Ω) response measurement of MgFe2O4 thin film was taken for 10–90% relative humidity (% RH) change at 300 K.