The invention relates to a material with
negative thermal expansion performance and a preparation method thereof. The method is characterized by comprising the steps that 1, PbO, TiO2, Bi2O3 and Co3O4samples are mixed and blended uniformly according to a preset ratio, and pre-
processing is conducted; 2, the mixed samples are added to a tube
crucible, an
antioxidant is added, and the tube cruciblecontaining the mixed samples is placed into a sealed mold; 3, the sealed mold is placed in high-pressure synthesis equipment,
temperature and pressure are increased, heat and pressure preserving areconducted, and the temperature and the pressure are reduced to a
room temperature and normal pressure; 4, the processed samples are taken out and demolded, the processed samples are washed, the samples are dried, and the novel material (1-x)PbTiO3-xBiCoO3 with the
negative thermal expansion performance is obtained, wherein 0.0<=x<=1.0. Compared with a traditional material with the negative thermalexpansion performance, the material, with the
negative thermal expansion performance, prepared through the method has high purity, high
repeatability, significantly enhanced negative
thermal expansion performance and broadened negative expansion temperature zone, and therefore the material has wide scientific researching and practical value.