Synthesis and characterization of polyether structure carbon nitride

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Carbon nitride powder with an atomic N/C ratio of 1 has been prepared by reaction of cyanuric chloride with sodium metal. X-ray diffraction, Fourier transform infrared spectra, and x-ray photoelectron spectroscopic data provide substantial evidence for a graphite-like sp2-bonded structure composed of building blocks of s-triazine rings bridged by carbon-carbon atoms in the bulk carbon nitride. The electron-microscopy results reveal that the material is spherical particles with an average diameter of 50 nm. The optical properties and thermal stability are also characterized. Based on the experimental results, it is deduced that the structure of as-prepared material carbon nitride has polyether structure.

I. INTRODUCTION

Carbon nitride and related materials have attracted much interest in the past decade. They have been regarded as superhard materials.1 For example, firstprinciples calculations have suggested that the hardness of beta-C3N4 may exceed that of diamond.2,3 Therefore, this kind material may be used in many fields, such as catalyst supports or semiconductor or conductor materials due to their special properties. Some methods including plasma,4 sputtering,5 laser ablation,6 chemical vapor deposition,7 and high-pressure pyrolysis8 have been applied to synthesize such compounds. Wang provided a review about such materials.9 Synthesis of carbon nitrides using chemical method has also been reported. For instance, Khabashesku et al. prepared carbon nitride power by solid-state reactions between cyanuric chloride or its fluoro analog and lithium nitride.10 Carbon nitride spheres were prepared by template-directed solid-state or solution reaction of cyanuric chloride or fluoride with lithium nitride.11 Nitrogen-rich carbon nitrides were fabricated as amorphous, bulk solids from the slow thermal decomposition of 2,4,6,-triazido-1,3,5-triazine [(C3N3)(N3)] by Gillan.12 Miller et al. obtained nitrogenrich carbon nitride power via the facile low-temperature decomposition of trichloromelamine (C3N3)(NHCl)3.13 C3N4 materials have been synthesized via high-pressure and relatively low-temperature procedure that involved a

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Address all correspondence to this author. e-mail: [email protected] DOI: 10.1557/JMR.2004.0249

chemical reaction of hexachlorobenzene (HCB) and sodium azide (NaN3) in the presence of a sodium flux.14 In the literature, Wurtz-like reactions have been used to synthesize diamond and carbon nanotubes.15–18 For example, Qian’s group15 reported the synthesis of diamond powder from the reaction of carbon tetrachloride with sodium. Subsequently, they prepared multiwall carbon nanotubes by reduction of HCB using metallic potassium.16 Lee et al. synthesized carbon materials with graphitic structure through HCB and sodium.17 Bao and co-workers synthesized carbon nanotube bundle with mesoporous structure18 and hollow carbon spheres (50–100 nm)19 by a self-assembly approach using HCB and Na. In this article, we report the one-step synthesis of polyether structure20,21 carbon nitride using Wurtz-like reactio

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