Mesoscopic structures of SiC fibers produced from polycarbosilane by different methods were studied by diffraction and small-angle scattering of neutrons and x-rays. Microvoids of a size of 4–10 Å in diameter have been observed for the first time by neutron scattering in a medium momentum transfer range (Q = 0.1–1.0 Å−1). The size and the volume fraction of β–SiC particles were determined for fibers prepared at different heat-treatment temperatures. The results show that wide-angle neutron scattering measurements are especially useful for the study of the mesoscopic structure of multicomponent materials.