In this paper we report the magnetic properties of nanosized intermetallic FeAl particles, prepared by a two-step chemical synthesis route and characterized using X-ray diffraction, conventional and high-resolution transmission electron microscopy (HRTEM), and energy dispersive X-ray spectroscopy (EDX) techniques. The nanoparticles have the same crystal structure (B2) as bulk FeAl. Atomic fringes of the FeAl nanocrystals were observed by using HRTEM. The particles were rectangular in shape with an average length of 20−23 nm. The prepared nanoparticles are found to show magnetization with superparamagnetic behavior arising from the core as well as the surface of these particles. A wide distribution of blocking temperature is evident for these superparamagnetic particles.