期刊
CHEMISTRY-A EUROPEAN JOURNAL
卷 17, 期 11, 页码 3213-3221出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.201002462
关键词
carbon nitrides; electron diffraction; intercalations; layered compounds; NMR spectroscopy
资金
- Deutsche Forschungsgemeinschaft (DFG) [SCHN 377/12, SE 1417/2]
- Fonds der Chemischen Industrie (FCI)
- Center for Nanoscience
- Cluster of excellence Nanosystems Initiative Munich (NIM)
Poly(triazine imide) with intercalation of lithium and chloride ions (PTI/Li+Cl-) was synthesized by temperature-induced condensation of dicyandiamide in a eutectic mixture of lithium chloride and potassium chloride as solvent. By using this ionothermal approach the well-known problem of insufficient crystallinity of carbon nitride (CN) condensation products could be overcome. The structural characterization of PTI/Li+Cl- resulted from a complementary approach using spectroscopic methods as well as different diffraction techniques. Due to the high crystallinity of PTI/Li+Cl- a structure solution from both powder X-ray and electron diffraction patterns using direct methods was possible; this yielded a triazine-based structure model, in contrast to the proposed fully condensed heptazine-based structure that has been reported recently. Further information from solid-state NMR and FTIR spectroscopy as well as high-resolution TEM investigations was used for Rietveld refinement with a goodness-of-fit (chi(2)) of 5.035 and wRp=0.05937. PTI/Li+Cl- (P6(3)cm (no. 185); a=846.82(10), c=675.02(9) pm) is a 2D network composed of essentially planar layers made up from imide-bridged triazine units. Voids in these layers are stacked upon each other forming channels running parallel to [ 001], filled with Li+ and Cl- ions. The presence of salt ions in the nanocrystallites as well as the existence of sp(2)-hybridized carbon and nitrogen atoms typical of graphitic structures was confirmed by electron energy-loss spectroscopy (EELS) measurements. Solid-state NMR spectroscopy investigations using N-15-labeled PTI/Li+Cl- proved the absence of heptazine building blocks and NH2 groups and corroborated the highly condensed, triazine-based structure model.
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