to avoid introduction of milling media during ball-milling process and ensure uniform distribution of sic and graphite in zrb2 matrix, ultrafine zrb2–sic–c composite powders were in-situ synthesized using inorganic–organic hybrid precursors of zr(opr)4, si(oc2h5)4, h3bo3, and excessive c6h14o6 as source of zirconium, silicon, boron, and carbon, respectively. to inhabit grain growth, the zrb2–sic–c composite powders were densified by spark plasma sintering (sps) at 1950°c for 10 min with the heating rate of 100°c/min. the precursor powders were investigated by thermogravimetric analysis–differential scanning calorimetry and fourier transform infrared spectroscopy. the ceramic powders were analyzed by x-ray diffraction, x-ray photoelectron spectroscopy, and scanning electron microscopy. the lamellar substance was found and determined as graphite nanosheet by scanning electron microscopy, raman spectrum, and x-ray diffraction. the sic grains and graphite nanosheets distributed in zrb2 matrix uniformly and the grain sizes of zrb2 and sic were about 5 lm and 2 lm, respectively. the carbon converted into graphite nanosheets under high temperature during the process of sps. the presence of graphite nanosheets alters the load-displacement curves in the fracture process of zrb2–sic–g composite. a novel way was explored to prepare zrb2–sic–g composite by sps of in-situ synthesized zrb2–sic–c composite powders.
due to the existence of metallic bond and covalent bond, zrb2 has high melting point, high hardness, superior thermal–electrical conductivity, and excellent corrosion resistance. 1 it has been shown that the uniform distribution of second phase led to higher strengths, moreover, smaller starting sic particle was helpful to improve densification and refine grain sizes.2,3 the addition of suitable content of sic into zrb2 had been proven beneficial for improving the oxidation resistance and mechanical property.4 the addition of graphite flakes or graphene increased the fracture toughness 5–7 and thermal shock resistance6,7 of zrb2–sic composite. the general method to prepare zrb2–sic–g composite was hot pressing of the mechanically mixed zrb2, sic powders, and graphite flakes. however, the sic or graphite flakes unevenly distributed in zrb2 matrix, in addition, the milling media may be introduced in the composite during the ballmilling process. due to the longer sintering time and lower heating rate, the significant growth of grain was found in zrb2–sic–g composite prepared by hot pressing.6 nevertheless, there was few report about spark plasma sintering (sps) of in-situ synthesized zrb2–sic–c composite powders to prepare zrb2–sic–g composite.