Bulk quantity Boron Carbonitride (BCN) microspheres were successfully synthesized via an organic precursor pyrolysis approach. The organic precursor was synthesized at 90 degrees C by the polymerization reaction of boron trichloride, aniline and ethylenediamine with a molar ratio of 1:1:1. All particles presented uniform spherical structure with the size of 2 mu m. The products have oxidation starting temperature at 624 degrees C much higher than graphene (404 degrees C). (C) 2017 Elsevier B.V. All rights reserved.