Studies of formation of titanium nitride layer with laser gas alloying by multipulse laser irradiation of 5-ns duration are described. The nitridation process was observed by detecting the light emitted above the surface while it is irradiated. The nitrided surface was morphology-examined by an optical microscope and a scanning electron microscopy (SEM) and characterized by time of light mass spectrum (TOFMS) during laser ablation of the surface as well as by X-ray diffraction (XRD). The laser pulses melt the titanium surface and activate N2, which leads to nitridation of titanium in liquid phase. It is also found that the nitride layer grown is rich in Ti and consists of δ-TiN and α—Ti.