New approach to the synthesis of nanocrystalline boron carbide

The use of nanoparticles in ceramic matrix composites provides lower sintering temperatures and higher densities at a given temperature than common coarse-grained materials. Nanocrystalline B4C was synthesized by an inexpensive carbothermal reduction method using carbon black and B2O3 as precursor. Full conversion was achieved at 1623 K for annealing times of 480 minutes or with a large excess of B2O3 and oxidation of the remaining carbon after 30 minutes of annealing. The average particle size of the synthesized B4C powder was 260 nm, which was reduced to 70 nm after separation of the small particle fraction from the larger particles by sedimentation. A mixture of the as-prepared powder and commercial coarse-grained B4C yielded an increase of the density of low temperature hot pressed samples by 25% in comparison to pure commercial B4C. Possible chemical reactions and mechanisms in the synthesis of B4C were examined with the Gibbs free energies of reactions. The most likely reaction was the reduction of B2O3 vapor at the surfaces of the carbon particles after its vapor transport from the liquid B2O3. An observed reduction of B4C yield above 1623 K was probably caused by loss of B2O3 vapor from the reaction mixture.