Nickel Aluminium ferrite with general formula NiAlxFe2-xO4for ‘x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0’ were synthesized by High Energy Ball milling. Fourier Transform Infrared Spectra (FTIR) and Dielectric characteristics were measured at room temperature as a function of frequency for synthesized ferrite. Infrared spectra exhibit two vibrational bands; high frequency band v_1 observed for the samples in the range of 603 〖cm〗^(-1)to 632 〖cm〗^(-1)assigned by stretching vibrations of tetrahedral metal oxygen bond and low frequency band v_2 observed in range 418 〖cm〗^(-1)to 489 〖cm〗^(-1)assigned due to metal oxygen vibrations in octahedral B sites. The dielectric investigation of Nickel Aluminium ferrite shows that the value of dielectric constant, dielectric loss and dielectric loss tangent are high at low frequency and become frequency independent at high frequencies.
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