The effect of different media, including cetyltrimethylammonium bromide (CTAB) and sodium borohydride (NaBH4), on the size, shape, optical absorption, and stability of titanium (Ti) and copper (Cu) nanoparticles (NPs) synthesized by laser ablation in liquid, was investigated. Ti and Cu NPs were fabricated by irradiating Ti and Cu targets using a Nd:YAG pulsed laser with a wavelength of 1064 nm, an energy of 500 mJ, repetition rate of 1 Hz, and a number of pulses of 1000. Results showed the direct effect of the type of surfactant on the size and size distribution of Ti and Cu NPs under the same laser ablation parameters. Morphological properties were described by field emission scanning electron microscope (FESEM) images, which revealed the formation of semispherical particles. The EDS results confirmed the spike-induced synthesis of Ti and Cu in CTAB and NaBH4 solutions. The transmission electron microscopy (TEM) images showed the nanostructures of Ti and Cu with spherical particles. The UV-vis absorption spectra showed that the absorption peak of Ti was almost constant at 289 nm, while the peak of Cu disappeared for both solutions. Zeta potential analysis showed that NPs prepared in CTAB solution were more stable than those in NaBH4 solution.