Precipitation of silver ions simultaneously with chloride and bromide ions in ethylene glycol at a mild temperature (e.g., 60 1C) has been successfully demonstrated for the synthesis of silver chlorobromide (AgCl x Br 1Àx , 0 o x o 1) nanoparticles, which is realized by injecting a AgNO 3 solution into a solution containing both halogen ions. The injection rate of the AgNO 3 solution has been determined to be critical for controlling the uniformity of AgCl x Br 1Àx nanoparticles. Time-resolved in situ high-energy synchrotron X-ray diffraction has been applied, for the first time, to quantitatively monitor the reaction kinetics of nanocrystal formation. The real-time results shed light on the fact that the injection rate of AgNO 3 solution significantly influences the nucleation and growth processes, and thus the quality of resulting AgCl x Br 1Àx nanoparticles. Specifically, fast injection enables the complete addition of AgNO 3 solution to the reaction solution before the nucleation process starts, leading to a good separation of nucleation and growth and thus the formation of uniform AgCl x Br 1Àx nanocubes with well-defined composition and narrow size distribution. By contrast, slow injection results in a continuous addition of AgNO 3 solution to the reaction solution even after nucleation starts, leading to continuous multiple nucleation/growth processes and thus the formation of AgCl x Br 1Àx nanoparticles with broad dimensional and morphological distributions.