Large-scale synthesis of amorphous phosphorus nitride imide nanotubes with high luminescent properties
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i Zhu and Chengqi Yi Department of Chemistry, University of Science & Technology of China, Hefei, Anhui 230026, People’s Republic of China
Yi Xiea) Nano-materials and Nano-chemistry, Hefei National Laboratory for Physical Sciences at Microscale, University of Science & Technology of China, Hefei, Anhui 230026, People’s Republic of China; and Department of Chemistry, University of Science & Technology of China, Hefei, Anhui 230026, People’s Republic of China (Received 15 June 2004; accepted 15 September 2004)
A facile solvothermal approach was successfully developed for the large-scale synthesis of amorphous phosphorus nitride imide (H3xP3N5+x) nanotubes with high luminescent properties by the reaction of 1,3,5-hexachlorotriphosphazene (P3N3Cl6) with sodium amide (NaNH2) at low temperatures. Transmission electron microscope images showed that the inner diameter of nanotubes is 120 ± 20 nm, wall thickness is 40 ± 10 nm, and length ranges from several to ten micrometers. Scanning electron microscope images revealed that the proportion of the nanotubes exceeds 90%. X-ray photoelectron spectroscopy spectra indicated that the binding energies of P2p and N1s are 133.30 and 398.40 eV, respectively, and the atomic ratio of P:N is 3:5.13. The infrared spectra of the sample are comparable to those of the reported HPN2 and HP4N7. Thermogravimetric analysis revealed that the product is very robust in a nonoxidizing atmosphere. The structure and the optical properties of the product and the annealed samples were investigated by x-ray diffraction and photoluminescence measurements, respectively.
I. INTRODUCTION
In the past three decades, much attention has been focused on the nonmetal nitrides (such as BN, Si3N4, and predicted C3N4), which can be used as high-performance materials because of their outstanding thermal, mechanical, and chemical stability, coupled with their low density.1,2 For reasons of analogy, P3N5 should have a structure and properties similar to those of the above mentioned nonmetal nitrides. Reliable spectroscopic, crystallographic, and structural data of P3N5 had not been obtained until the successful synthesis of pure, stoichiometry, hydrogen-free, and crystalline phosphorus nitride P3N5 by Schnick’s group.3 Recently, phosphorus nitride P3N5 was structurally characterized after considerable effort.4–6 At the same time, significant advances
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Address all correspondence to this author. e-mail: [email protected] DOI: 10.1557/JMR.2005.0041 J. Mater. Res., Vol. 20, No. 2, Feb 2005
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are gained in the studies of ternary phosphorus nitrides, such as HPN2,7 HP4N7,8,9 and XP4N7 (X ⳱ Na, K, Ru, Cs).10 Both binary and ternary phosphorus nitrides all have the potential for various ceramic applications.3 In the solid-state form, HPN 2 contains a threedimensional framework of corner-sharing PN 4 tetrahedra, and the hydrogen atoms are covalently bonded to half of the nitrogen atoms.7 In HP4N7, there are PN4-tetrahedra as characteristic structural motifs, which
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