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The preparation of La0.9Na0.1CrO3 (LNCO), Ni0.5Cu0.5Fe2O4 (NCFO) and their composites of the type (1−x) La0.9Na0.1CrO3 (LNCO) + (x) Ni0.5Cu0.5Fe2O4 (NCFO) (x=0.25, 0.50) through solid state route is reported. From X-ray diffraction data analysis, the parent La0.9Na0.1CrO3 was found to crystallize in orthorhombic structure (Pnma) while Ni0.5Cu0.5Fe2O4 has crystallized into the cubic structure (Fd3m) further verified via Retvield refinement. The morphology and compositional studies were carried out using field emission scanning electron microscopy (FESEM) and energy dispersive analysis of X-rays (EDAX), respectively. Lattice structure was confirmed via Raman characterization for the prepared samples. The sample formation was further verified through Fourier transform Infra-Red (FTIR) spectroscopy. The dielectric studies reveal the La0.9Na0.1CrO3(13*104) and Ni0.5Cu0.5Fe2O4(1.83*104) exhibit high dielectric constant. However, their composites show abrupt drop in dielectric constant. The electric modulus study confirmed that the samples exhibit non-Debye character with spread of relaxation time constants.