In the middle of the Neolithic Age, Chinese ancestors applied pottery-making techniques to the technology of construction and invented a series of building materials, made of burnt clay, that had significantly better strength and water resistance, which greatly improved the living conditions of ancient humans. In the middle and lower reaches of the Yangtze River, the process of evolution of Neolithic building construction is much more obvious, with burnt clay-made materials widely used. In our study, XRD, XRF, magnetic susceptibility measurements and colorimetry were used to comprehensively analyze the burnt clay samples of different cultural stages unearthed at Qixingdun site in Huarong, Hunan Province. The results show that the six burnt clay samples were probably building materials made from local soil, mixed with plant remains such as rice husk and rice straw and then baked. The equivalent firing temperature range of these burnt clay samples is 550~700 ℃.