In order to improve the poor surface hardness and the wear resistance, titanium has been nitrided with plasma (ion) nitriding which is one of the methods to treat surface properties of titanium alloys. The increment at surface hardness and so the wear resistance of nitrided titanium alloys has been provided by means of compound layer (ε-Ti2N+δ-TiN) and diffusion zone (α-Ti) occurred by plasma ion nitriding. The goal of the present paper is to investigate effects of nitriding temperature and nitriding time on the microstructure and hardness value of nitrided surface layers. A systematic study was undertaken with specimens of commercial pure Ti and Ti-6Al-4V alloy. As treatment parameters, we have used; nitriding time (from 2 to 9 hour), nitriding atmosphere (H2-80%N2), total pressure (1 kPa) and cathode temperature (from 600 to 800 oC). The Vickers indenter was used for analysis of the micro hardness measurements. The thin hardened layer at the nitrided surface was characterized by glancing-angle X-ray difractometer. X-ray diffraction analysis has confirmed the formation of ε-Ti2N and δ-TiN phases on the nitrided specimens. Experimental details and characterization of plasma (ion) nitrided titanium have reported and discussed.