A multiple zirconium dioxide interphase for SiC/SiC f composites was developed using the sol–gel approach. The morphology, elemental composition, topography, and tensile strength of ZrO 2 coated Nicalon™ CG fibers were examined using scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS), atomic force microscopy (AFM), and single filament tensile strength analysis as a function of the number of coats. The interfacial frictional stress values of the SiC/SiC f and SiC/(ZrO 2 ) n /SiC f minicomposites were evaluated using micro indentation tests.It was shown that the presence of multiple ZrO 2 coating on Nicalon™ CG promotes decoupling of the fibers from the matrix and frictional pullout, with the fiber sliding pressure decreases as a number of coats increase. Due to strong bonding at the fiber/coating and the matrix/coating boundaries, on the one hand, and weak bonding between interfacial layers, on the other hand, debonding and sliding occur within the interphase.Thus, the fiber/matrix decoupling in SiC/(ZrO 2 ) n /SiC f minicomposites can be regulated by designing the multiple ZrO 2 interphase.