In the domain of incremental nanotechnology, surface mechanical attrition treatment is a technique which can transform superficial structure of a material to nanocrystalline without changing the chemical composition. This study is a part of the development and implementation of the technique by using ultrasonic vibrations. The material used is pure titanium in rolled and annealed condition. The nanocrystalline structure is characterized using X-ray diffraction (XRD), and transmission electron microscopy (TEM). The measured grain size is in the order of 5~60 nm. A correlation in the results of XRD and TEM is also discussed.