In the last decade, laser Ablation technique (Nd:YAG) has been considered as a perfect method for producing nanostructures with high purity. In the present study, Titanium diboride nanoparticles (TiB 2 NPs) have been deposited on Aluminum (Al) and their micromorphology and microstructural properties have been investigated. The synthesis of TiB 2 NPs has been carried out by the Laser Ablation technique (Nd:YAG) which has not been reported so far. Moreover, the effects of laser energy on improving the synthesis of TiB 2 NPs have been examined. In this regard, five samples of TiB 2 NPs were prepared by Laser Ablation method in different values of laser fluency in the range of 0.4-1.2 J/cm 2 . The structural properties of prepared nanoparticles were detected by grazing incidence X-ray diffraction, transmission electron microscopy, and energy dispersive X-ray spectroscopy. The morphology of samples was also investigated by field effect scanning electron microscopy. The results demonstrate the formation of spherical nanoparticles in all samples. Based on the results of the GIXRD patterns, pulsed laser energy is an effective parameter for the size of ablated nanoparticles. As can be seen, increasing the energy of laser beam decreases the average size of nanoparticles from 79.41 to 4 nm. As the next step, the as-prepared nanoparticles were deposited on Aluminum substrate with electrophoretic deposition technique at constant applied voltage (30 Volt) and constant deposition time (30 min). The X-ray diffraction pattern of TiB 2 NPs deposited onto Al substrate confirmed the formation of the TiB 2 thin films on all Al substrates. Also, the roughness and average particle size of deposited films were measured by atomic force microscopy images and MountainsMap ® Premium software. Increasing the fluency of laser beam made the surface more irregular and the maximum value of fractal dimension and hence, the most irregular topography has been observed in the sample produced by maximum laser fluency. Research Highlights• Titanium diboride nanoparticles have been synthesized by the laser ablation technique.• The effects of laser energy on improving the synthesis of TiB 2 NPs have been investigated.