Abstract：The hyperfine red phosphors, Eu3＋ doped AgGd(WO4)2, with various shapes have been prepared by a simply hydrothermal synthesis procedure. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy were used to characterize the products. A series of controlled experiments indicate that the shape and size of as-prepared architectures can be tuned effectively by controlling the reaction conditions, such as pH values of the initial solution and different kinds of surfactants. The results of XRD indicated that all of the synthesized samples were monocline phase. The pH value of the starting solution and the surfactant played a key role in the formation of products with different morphologies. Spherical, rod-like and hollow spherical particles could be obtained with different particle size by adjusting the reaction condition. AgGd0.9Eu0.1(WO4)2 emission spectrum showed the characteristic emission of Eu3＋. The luminescence intensity of the synthesized samples can be influenced by the morphology and the size of particles.