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A series of Eu3+-doped C12H18Ca3O18 phosphors were synthesized through a facile hydrothermal method and the properties of as-prepared phosphors were explored by X-ray diffractometer (XRD), scanning electron microscope (SEM), and photoluminescence (PL) spectrometer. The exploration results indicated that the C12H18Ca3O18:Eu3+ had been successfully synthesized. The morphology of C12H18Ca3O18:Eu3+ was a strip with the size of 100–4000 nm × 50–400 nm × 50–200 nm and the ratio of length to width of 2–80. The strongest emission peak of C12H18Ca3O18:Eu3+ around 620 nm was ascribed to 5Do→7F2 transition of Eu3+, and the peaks centered at 590, 653 and 694 nm respectively corresponded to 5Do →7F1, 7F3, and 7F4 transitions. C12H18Ca3O18: Eu3+ gave the red light emission, as indicated by color coordinate analysis. The photoluminescence intensity of the phosphors prepared under the Eu3+ concentration of 6% was the highest. The crystal structure of C12H18Ca3O18:Eu3+ was changed after europium ions occupied the lattice position of calcium ions. Europium ion could displace calcium arbitrarily. As a new kind of matrix, calcium citrate possesses the properties of both organic and inorganic compounds and the luminescent C12H18Ca3O18: x Eu3+ particles may be applied in biological fluorescent tags and luminescent materials.