This study dealt with both the strengthening of matrix and the suppression of interfacial reaction for the development of high toughness Nb/MoSi2 laminate composites. The impact values of Nb/MoSi2, Nb/MoSi2-SiC, Nb/MoSi2-ZrO2 laminate composites were investigated at the room temperature. The flexural strength of MoSi2 based composites containing SiC or ZrO2 particles were also evaluated at elevated temperatures. The reduction of reaction layer by the addition of ZrO2 particles led to the sufficient improvement in the impact value of Nb/MoSi2 laminate composites. The flexural strength of MoSi2-SiC and MoSi2-ZrO2 materials decreased at temperatures higher than 800 °C.