Microbead and nanophase carbon materials attract many researchers due to their unique applications, [1] which include high-density and high-strength carbon artifacts, [2] super-active carbon beads of high surface area, [3] lithium storage, [4a] lithium battery anodes, [4b-d] spherical packing materials for HPLC, [5] hydrogen storage applications, [6] and catalysis. [7] Much attention has focused on the preparation (precursors and methods) and properties of these carbon materials, because their applications significantly depend on the shape and size of the particles.Carbon nitrides are of current interest due to their novel mechanical, optical, and tribological properties, including low density, extreme hardness, surface roughness, wear resistance, chemical inertness, and biocompatibility.[8] These superhard diamondlike materials promise a variety of technological and biological applications. For example, they are used as biocompatible coatings on biomedical implants, [8][9] battery electrodes, [10] catalytic supports, [11] gas separation systems, [12] electronic materials, [13] and humidity and gas sensors.[14]Unlike carbon-based materials, applications of carbon nitrides are not only governed by the texture and size of the particles [13] but also by the relative nitrogen content. As a consequence, an extensive effort has focused on the discovery of precursors along with the appropriate methods to increase the nitrogen content in carbon nitrides.There is very little literature on the preparation of carbon nanospheres and nitrogen-rich carbon nitrides (> 60 wt % N). Gillan reported preparations of carbon nitrides C 3 N 4 (60.9 wt % N) and C 3 N 5 (66.0 wt % N) and graphitic carbon using high-nitrogen 2,4,6-tri(azido)-1,3,5-triazine as the pre-
