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Nitrogen-rich B–C–N materials have been prepared by the reaction between melamine and boron trichloride at different temperatures. The composition of the materials was dependent on the synthesis and annealing temperatures: C6N10.8–11H9.4B1.5–1.7 (for products synthesized and annealed at 673 K), C6N9.3–9.4H3.8–3.9B2.2–2.5 (for those synthesized at 673 K and annealed at 873 K) and C6N9.2H3.6B1.2–1.3 (for those synthesized and annealed at 873 K). Fourier transform infrared spectroscopy and 13C nuclear magnetic resonance showed that the s-triazine rings from the melamine molecules were preserved in materials synthesized and annealed at 673 and 873 K. The sample obtained at 873 K had a graphite-like structure as suggested by X-ray and electron diffraction studies. The s-triazine rings were decomposed in the materials synthesized or annealed at 1223 K and the main product obtained was turbostratic boron nitride.