NiTi alloys containing more than 55%wt nickel undergo precipitation of Ni4Ti3, Ni3Ti2, and Ni3Ti phases during various heat treatments which could have a great effect on the chemical composition of the matrix and behavior of alloy. In this investigation, a NiTi alloy with Ti-57.5%wt nickel content, produced by vacuum induction melting in a graphite crucible, were subjected to the homogenization heat treatments in 1100oC and for various time periods (0.5, 1, 2, and 4 hours). The subsequent cooling was conducted in different cooling media (furnace and air) in order to examine the effect of cooling rate. Microstructural investigations show Ni4Ti3 particles with bimodal size distribution in furnace cooling. Differential scanning calorimetry demonstrates the correlation between homogenization time and transformation temperatures of the alloy.