Crystal materials are an important pillar of advanced technology. Among them, the preparation of large-sized single crystal materials is of great importance for their practical application. Herein, we select the well-known nonlinear optical crystal KH[subscript 2]PO[subscript 4] and impressive deep-blue colored crystal CuSO[subscript 4]·5H[subscript 2]O to design an integrated experiment on the growth of large-size single crystals. This experiment, which aims to introduce the basic concepts and techniques of crystal growth and characterization, was designed for undergraduate majors in chemistry and materials science. To deepen the understanding of the complicated theoretical knowledge and cultivate their interests in crystal growth, students prepared large-scaled crystals and then characterized and investigated the structures, morphologies, and properties of KH[subscript 2]PO[subscript 4] and CuSO[subscript 4]·5H[subscript 2]O. The common analytical methods involved in this lab course will help students to enhance their practical ability and thinking ability as well as initially cultivate their scientific research thoughts in the crystal material field.