We present a combined theoretical and experimental study on the morphological, structural, and optical properties of β-Ag₂MoO₄ microcrystals. β-Ag₂MoO₄ samples were prepared by a co-precipitation method. The nucleation and formation of Ag nanoparticles on β-Ag₂MoO₄ during electron beam irradiation were also analyzed as a function of electron beam dose. These events were directly monitored in real-time using in situ field emission scanning electron microscopy (FE-SEM). The thermodynamic equilibrium shape of the β-Ag₂MoO₄ crystals was built with low-index surfaces (001), (011), and (111) through a Wulff construction. This shape suggests that the (011) face is the dominating surface in the ideal morphology. A significant increase in the values of the surface energy for the (011) face versus those of the other surfaces was observed, which allowed us to find agreement between the experimental and theoretical morphologies. Our investigation of the different morphologies and structures of the β-Ag₂MoO₄ crystals provided insight into how the crystal morphology can be controlled so that the surface chemistry of β-Ag₂MoO₄ can be tuned for specific applications. The presence of structural disorder in the tetrahedral [MoO₄] and octahedral [AgO₆] clusters, the building blocks of β-Ag₂MoO₄, was used to explain the experimentally measured optical properties.

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