采用热压烧结工艺制备β-LiAlSiO4/Cu复合材料。对复合材料进行多次热循环过程中的热膨胀行为测试,对烧结态复合材料进行原位高温XRD分析,对热循环前后复合材料的微观组织进行观察。结果表明:经过2次以上热循环处理后,β-LiAlSiO4/Cu复合材料获得稳定的热膨胀系数。在热循环过程中复合材料残余应力得到松弛和释放,可以显著降低复合材料的热膨胀系数。复合材料中的残余应力引起β-LiAlSiO4颗粒中的Li+从有序到无序的非可逆性的相转变。在热循环过程中复合材料残余应力的释放引起基体孪晶变形。 Preparation of β-LiAlSiO4 / Cu Composites by Hot Press Sintering Process. The thermal expansion behavior of the composites during several thermal cycles was tested. The in-situ high temperature XRD analysis of the sintered composites was carried out, and the microstructure of the composites before and after thermal cycling was observed. The results show that the β-LiAlSiO4 / Cu composite has a stable coefficient of thermal expansion after more than two thermal cycles. During thermal cycling, the residual stress of composites is relaxed and released, which can significantly reduce the thermal expansion coefficient of the composites. Residual stresses in the composite lead to an irreversible phase transition of Li + in the β-LiAlSiO4 particles from ordered to disorder. During the thermal cycling, the residual stress of composite material caused the twins deformation of the matrix.