In this paper, a new practical training project was designed and implemented for a Bi-based semiconductor. It is convenient to investigate the structures and properties of semiconductors for undergraduate materials chemistry. Bi-based semiconductors are getting recognition for promising sunlight-driven properties. Among them, Bi[subscript 2]Ti[subscript 2]O[subscript 7] is a novel semiconductor, and there are few related studies. Herein, Bi[subscript 2]Ti[subscript 2]O[subscript 7] was prepared by a mild and convenient hydrothermal method. Then, the structures and properties of the as-prepared sample were characterized by XRD, SEM, and photocatalytic degradation experiments. The practical training project provides an excellent opportunity for students to deeply explore the structure-activity relationship between the microstructure and the semiconductive properties. Specifically, the microstructures and properties were studied with Materials Studios software. Key features of this training project include the following: (1) A new practical project of elective course was successfully implemented by combining experimental design and theory analysis. It provides students with practical opportunities to understand research methods of semiconductor materials. (2) This practical training approach can provide students with necessary theoretical knowledge and technical ability, such as first-principles, sample preparation, and characterization methods for semiconductor materials. (3) It can enhance novel semiconductor design capabilities and characterization skills. It also can foster the development of students majoring in material-related fields and promote the cultivation of their research interests.