The powder of Ni50Ti50 (at. %) was chosen for the preparation of NiTi shape memory alloys by the Spark Plasma Sintering (SPS) method through powder metallurgical routes.  The SPS method was carried out in the vacuum chamber using NiTi powder of 20-63 µm inside the graphite die. The sample was fabricated at the temperature of 1050 °C with 50 MPa of load for 10 min. Furthermore, the fabricated sample was undergone annealing at room temperature for 1100 °C for 48h for homogenization of the structure. The characterization of as-prepared and annealed samples was performed by X-ray diffractometer (XRD), SEM, and EBSD analysis. The microstructure of the samples was evaluated with phase identification related to the diffusion of particle-particle interaction during processing. The necking between two particles has been confirmed from the boundary layers of the EBSD investigation of samples. The NiTi sample fabricated by the SPS process is dominant in the austenite phase with some voids.  However, upon annealing the formation of precipitates of Ni4Ti3 and oxide phases Ni2Ti4O has been observed.