Combustion synthesis experiments in a fluidized bed have been conducted using nitrogen as the fluidizing gas for the formation of transition-metal nitrides that are potential replacements for traditional hydrodenitrogenation and hydrodesulfurization catalysts. The microwave-assisted ignition of reaction has been investigated for its potential to produce nitride overlayers on two different sizes of tantalum particle substrates. Various characterization techniques-X-ray diffractometry, energy dispersive spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy-have been used to study the presence of nitride overlayers. The results indicate that microwave assistance can permit controlled formation of tantalum nitride (Ta2N) overlayers.