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Ca 12 Al 14 O 32 F 2 :Eu 3+ red phosphors were prepared by the sol-gel method with CF 3 COOH as the fluorine source. X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectra, and photoluminescence spectra, as well as thermogravimetric and differential thermal analysis were utilized to characterize the samples. All the samples were single phase with a cubic structure. The as-obtained Ca 12 Al 14 O 32 F 2 :Eu 3+ red phosphors consisted of nanoparticles with sizes of approximately 40–100 nm. Under the excitation of UV light, Ca 12 Al 14 O 32 F 2 :Eu 3+ exhibited the characteristic emissions of Eu 3+ , and the effect of annealing temperature, annealing time, and CF 3 COOH and Eu 3+ concentrations on the luminescence intensity were discussed in detail.