Synthesis of Boron Nitride from Triammoniadecaborane and Ammonia

YOGO Toshinobu, MATSUO Shigeru, NAKA Shigeharu

doi:10.2109/jcersj1950.95.104

Highly pure boron nitride of low crystallinity could be synthesized from triammoniadecaborane and ammonia below 800°C under atmospheric pressure. Triammoniadecaborane reacted with ammonia at temperatures between 300° and 450°C, and formed an amorphous solid containing BN, NH and BH bonds. According to the data of IR spectrum, the BH absorption band at 2500cm^-1 decreased in intensity with increasing temperature, and disappeared at 800°C. The 800cm^-1 band assigned to the BNB bonding increased in intensity from 700° to 800°C. The degree of alignment of the B₃N₃ hexagonal layer increased as the reaction time increased from 2h to 10h at 800°C. The X-ray diffraction profiles of the product formed at 800°C for 10h showed the broad diffractions centered at 2θ=25.5° and 42.0° (Cu Kα). The crystallization of boron nitride synthesized at 800°C for 10h proceeded above 1180°C. The 100 reflection of hexagonal boron nitride was separated from the broad 10 diffraction of the specimen heated at 1550°C for 2h. The lattice constant (c⁰) and size of crystallite (L^c) of the specimen were 6.735 and 220Å, respectively, after heating at 1550°C under atmospheric pressure for 2h. The size of crystallite increased from 320 to 830Å as the temperature increased from 1100°C to 1500°C under 2.0GPa for 10min heating. Boron nitride synthesized by heating at 800°C for 10h crystallized to hexagonal boron nitride when heated at 1500°C and 2.0GPa for 10min.

Synthesis of Boron Nitride from Triammoniadecaborane and Ammonia

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