Benzene thermal synthesis and characterization of crystalline carbon nitride
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A new solvothermal route has been successfully used to prepare crystalline carbon nitride powder from 1,3,5-trichlorotriazine (C3N3Cl3) and lithium nitride (Li3N) in benzene at 360 °C and 6–7 MPa. The as-prepared sample was brown and was analyzed by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectroscopy (FTIR). The results show that the powder mainly consists of α-C3N4, β-C3N4 and some unidentified carbon-nitrogen crystalline phases. The experimental lattice constants of α-C3N4 (a=6.48 Å,c=4.72 Å) and β-C3N4 (a=6.43 Å,c=2.47 Å) match the latest ab-initio calculations (a=6.47 Å and c=4.72 Å for α-C3N4, a=6.40 Å and c=2.40 Å for β-C3N4) quite well. The relative nitrogen-to-carbon composition ratio is 0.76. Only C–N and C=N bonds were demonstrated by XPS and FTIR. The feasibility of this synthetic method is discussed and this approach may provide a possible and very effective way to realize the growth of pure crystalline carbon nitride materials, which is quite different from the conventional solid-state reactions (SSR).
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