The synthesis of inorganic materials of a specific size and shape is a key aspect in modern powder technology. During the past two decades, solution-based precipitation reactions have been explored for controlled particle formation. A wide variety of particle shapes, sizes, and compositions has been demonstrated. However, several questions, especially concerning particle nucleation, remain. Some of these questions are currently addressed by investigating precipitate (ex situ) at different reaction stages by means of powder x-ray diffraction (PXRD), scanning (SEM) and transmission electron microscopy (TEM).