Toray T300 PAN-based carbon fibers were surface oxidized in air at 300, 400 and 500 °C. The composition of surface was determined by X-ray photoelectron spectrometry (XPS), and the monofilaments of original carbon fiber and surface oxidized carbon fibers were tensile tested at room temperature. Three-dimensional carbon fiber reinforced BN-Si3N4 matrix composites were prepared by precursor infiltration and pyrolysis using a hybrid precursor mixed by borazine and perhydropolysilazane. With the increase of the oxidation temperature, the content of size on the surface of fiber reduces, and the tensile strength of carbon fiber declines. Carbon fiber oxidized at 400 °C has a 93% residual strength and the fiber oxidized at 500 °C is seriously decayed. The composite reinforced by original carbon fibers exhibits excellent mechanical properties, including high flexural strength (182.3 MPa) and good toughness; while the composite reinforced by 400 °C oxidized carbon fibers is weak (only 102.4 MPa) and brittle. The distinct difference of mechanical properties between the two composite is attributed to the change of the interfaces between carbon fibers and nitride matrices.