High-energy synchrotron radiation has proven to be a powerful technique for investigating fundamental deformation processes for various materials, particularly metals and alloys. In this study, high-energy synchrotron X-ray diffraction (XRD) was used to evaluate Alloy 617 and Alloy 230, both of which are top candidate structural materials for the very-high-temperature reactor (VHTR). Uniaxial tensile experiments using in-situ high-energy X-ray exposure showed the substantial advantages of this synchrotron technique. First, the small volume fractions of carbides, e.g., ∼6% of M6C in Alloy 230, which are difficult to observe using laboratory-based X-ray machines or neutron scattering facilities, were successfully examined using high-energy X-ray diffraction. Second, the loading processes of the austenitic matrix and carbides were separately studied by analyzing their respective lattice strain evolutions. In the present study, the focus was placed on Alloy 230. Although the Bragg reflections from the γ matrix behave differently, the lattice strain measured from these reflections responds linearly to external applied stress. In contrast, the lattice strain evolution for carbides is more complicated. During the transition from the elastic to the plastic regime, carbide particles experience a dramatic loading process, and their internal stress rapidly reaches the maximum value that can be withstood. The internal stress for the particles then decreases slowly with increasing applied stress. This indicates a continued particle fracture process during plastic deformations of the γ matrix. The study showed that high-energy synchrotron X-ray radiation, as a nondestructive technique for in-situ measurement, can be applied to ongoing material research for nuclear applications.