Prepared by a Chemical Approach. -The title nanocomposite particles are prepared by addition of silica spheres to a dispersion of Fe(NO3)3, CoCl2, and Ga(NO3)3 in MeOH followed by sonication for 1 h and annealing at 850°C for 5 h under flowing H2. The samples are characterized by powder XRD, XAFS, TEM, 57 Fe Moessbauer spectroscopy, and magnetic measurements. The size of Co 2 FeGa particles is tuned by varying the amount of silica supports. The superparamagnetic critical size of the Co2FeGa nanoparticles is about 17 nm. -(FELSER*, C.; et al.; Chem. Mater. 22 (2010) 24, 6575-6582, http://dx.