Preparation of carbon-nitride bulk samples in the presence of seed carbon-nitride films

A procedure was developed for preparing bulk carbon-nitride crystals from polymeric α-C3N4.2 at high pressure and high temperature in the presence of seeds of crystalline carbon-nitride films prepared by using a high-voltage discharge plasma combined with pulsed laser ablation of a graphite target. The samples were evaluated by using X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, Auger electron spectroscopy (AES), secondary-ion mass spectrometry (SIMS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Notably, XPS studies of the film composition before and after thermobaric treatments demonstrated that the nitrogen composition in the α-C3N4.2 material, which initially contained more than 58 % nitrogen, decreased during the annealing process and reached a common, stable composition of ∼ 45 %. The thermobaric experiments were performed at 10 - 77 kbar and 350 - 1200 .deg. C.