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The demand of small-angle x-ray scattering (SAXS) windows for in-situ characterization of materials nano-structures in a heated vacuum environment has been increased dramatically. High-quality diamond prepared by chemical vapor deposition (CVD) has become the preferred window material due to its excellent optical and mechanical properties. However, impurities and defects in diamonds may lead to the strong X-ray scattering especially in the heating process, affecting the testing accuracy of the object. In this work, single-crystal diamond (SCD) and polycrystalline diamond (PCD) films with different quality were prepared, and their SAXS properties were investigated at room temperature and heating under vacuum. The results show that the scattering intensity of the undoped high-quality SCD is small and uniform, while that of the SCD window doped with a small amount of nitrogen increases, mainly due to the nitrogen atoms and vacancy clusters scattering. While for the PCDs, the grain boundaries and the dark features lead to strong scattering background. As the temperature rises from room temperature to 280 °C, although the phonon vibration of diamonds exhibits the obvious temperature dependence, the coherent scattering of diamonds with X-ray hardly changes, indicating no new scatterers with the changed gyration radius were generated in the heating process. SCD and PCD windows were successfully applied in an in-situ heating SAXS cell. [ABSTRACT FROM AUTHOR]