Abstract: SrAl₂O₄: Eu²⁺,Dy³⁺ are commercial materials with green persistent luminescence, which have shown actual applications in many fields. The SrAl₂O₄: Eu²⁺,Dy³⁺ phosphors were synthesized by the the sol-gel method. We guided the students with the control variate method to analyze the influences of the key factors such as aluminum/strontium adding ratio, aluminum/urea adding ratio and calcining ambience on the luminescence and redox properties of SrAl₂O₄: Eu²⁺,Dy³⁺ phosphors. The optimum preparation conditions of SrAl₂O₄: Eu²⁺,Dy³⁺ materials played important roles on the chemical production. This work is helpful to train students’ scientific research and experimental operation abilities, and provides an important referring example for the optimization of samples quality and luminescence properties of SrAl₂O₄: Eu²⁺,Dy³⁺ materials.