Carbon-carbon composites are deemed as candidate materials for application in very high temperature reactors. In a very high temperature reactor, carbon-carbon composite materials would experience severe environmental impacts from high temperatures. As a result, we applied non-destructive ex-situ diffraction experiments to investigate the microstructure changes of the carbon-carbon composite materials experiencing different temperatures. In this study, the samples were prepared in a format of a three-dimensional pitch-based carbon-carbon composite. The samples were heated to 500 (°C), 700 (°C), and 900 (°C) for 2 minutes, respectively. In order to understand the temperature effect on carbon-carbon composite, we facilitated the high penetration of the synchrotron X-ray diffraction at National Synchrotron Radiation Research Center to examine the evolution of microstructures subjected to heat treatment. The results show that the lattice parameters of a-axis and c-axis evolve upon heating. The molecular dynamics simulation results suggest that the early-stage rearrangement is originated from the release of the defects.