Photocatalysts based on TiO2 have been intensively investigated in order to achieve better photocatalytic efficiency for different applications such as decomposition of various organic pollutants. Recently, studies on the doping of transition metals (Fe, Ag, Au) and non-metal (N) ions into TiO2 have become attractive in the area of photocatalysis [1, 2]. Many approaches to improve the photocatalytic activity of TiO2 have been tested, and many researchers have pointed out that the photocatalytic activity of TiO2 generally depends on its morphology, crystal composition, crystallinity, and surface area. Of these synthetic approaches, hydrothermal treatment is one of the most widely used methods for increasing the crystallinity of TiO2 [3]. Hydrothermal treatment can also be used to change the morphology, microstructure, and phase composition of materials by varying the reaction parameters. Our previous work reports the synthesis of nanocrystalline TiO2 involving hydrothermal and ultrasonic treatments and also hydrothermal synthesis in microwave field with immersed sonotrode in the reaction environment [4]. Microwave irradiation, which energy is delivered to the reactants through molecular interaction with the electromagnetic field, is a new method that may resolve the problems rising from the conventional synthesis methods. It can reduce reaction time significantly due to its different reaction mechanism and has the advantage of uniform, rapid and volumetric heating [5]. In this paper, undoped and doped with Fe and N ions TiO2 nanocrystals were synthesized by microwaveassisted hydrothermal method. The novelty and originality of our research is given by the use of the hydrothermal synthesis in microwave field in different synthesis conditions. Like synthesis precursors we used titanium isopropoxide, urea and iron nitrate. The doping concentration was established at 2 and 3% from Ti composition. The materials were structural and morphological characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRUV-VIS), scanning electron microscopy (SEM) coupled with energy dispersive X-rays analysis (EDAX). Also the surface area was determined by BET method. The results reveal that the dominant crystal phase of undoped and Fe-doped TiO2 / N-doped TiO2 is anatase as spherical form. Also the elemental analysis confirmed the doping elements presence in TiO2 structure.