A boron-containing SiHfC(N,O) amorphous ceramic was synthesized upon pyrolysis of a single-source-precursor at 1000 °C in Ar atmosphere. The high-temperature microstructural evolution of the ceramic at high temperatures was studied using X-ray powder diffraction, Raman spectroscopy, solid-state nuclear magnetic resonance spectroscopy and transmission electron microscopy. The results show that the ceramic consists of an SiHfC(N,O)-based amorphous matrix and finely dispersed sp2-hybridized boron-containing carbon (i.e. ByC). High temperature annealing of ByC/SiHfC(N,O) leads to the precipitation of HfCxN1-x nanoparticles as well as to β-SiC crystallization. After annealing at temperatures beyond 1900 °C, HfB2 formation was observed. The incorporation of boron into SiHfC(N,O) leads to an increase of its sintering activity, consequently providing dense materials possessing improved mechanical properties as compared to those of boron-free SiC/HfC. Thus, hardness and elastic modulus values up to 25.7 ± 5.3 and 344.7 ± 43.0 GPa, respectively, were measured for the dense monolithic SiC/HfCxN1-x/HfB2/C ceramic nano/micro composite.