Magnesium metavanadate dihydrate (MgV2O6·2H2O) was synthesized as a nanophosphor by a water-assisted solid-state reaction (WASSR) method, and its crystal structure and luminescence properties were investigated in detail. MgV2O6·2H2O has an orthorhombic structure with space group Pnma. In the crystal structure, the MgO6 octahedra and VO4 tetrahedra formed a layered structure in the direction of the b axis, and the VO4 tetrahedra formed a chain structure along the a axis. The nanophosphor showed broad and strong optical absorption in the near-ultraviolet region and exhibited a broad yellow emission peak at 563 nm.
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