Porous boron nitride (BN) powder was prepared through a facile template-free synthesis route through the pyrolysis of controlled polymerized ammonia borane (AB) at 1300 °C. The prepared products were characterized using different techniques such as X-ray diffraction analysis, X-ray photoelectron spectroscopy, scanning transmission electron microscopy, transmission electron microscopy and N2 sorption analysis. We investigated the effect of AB polymerization temperature and time on the micropores formation and surface areas of the obtained products. Lower heating temperatures of AB before pyrolysis resulted in higher surface area and micropore volume. The highest surface area was obtained from isothermal heating of AB at 70 °C and 32 h before being subjected to pyrolysis at 1300 °C.
