A Au colloid was prepared in a 5 mM HAuCl4 solution through irradiation with a focused infrared femtosecond laser at 800 nm. The Au colloid was characterized by absorption spectra, transmission electron microscopy, and x-ray diffraction analysis. The appearance of absorption peak around 526 nm in the absorption spectra and the wine-red color of sample solution HAuCl4 under focused laser irradiation verified the formation of Au colloid. The solution color changed in the order of yellow → orange → wine-red due to the local formation of Au nanoparticles near the focus. The pulse energy, focus position of laser beam, and solvent composite play important roles in formation, grain size, and stability of the Au colloid. A mechanism for the precipitate of Au nanoparticles was proposed, and a multiphoton process of femtosecond laser was involved.