A novel organothermal reduction process for producing nanocrystalline Ni 2 P with a circular-shaped flake morphology
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A novel organothermal reduction process for producing nanocrystalline Ni2 P with a circular-shaped flake morphology Shu-Hong Yua) Structure Research Laboratory and Department of Chemistry, University of Science and Technology of China, Hefei, 230026, People’s Republic of China
Jian Yang, Yong-Sheng Wu, Zhao-Hui Han, Lei Shu, and Yi Xie Department of Chemistry, University of Science and Technology of China, Hefei, 230026, People’s Republic of China
Yi-Tai Qiana) Structure Research Laboratory and Department of Chemistry, University of Science and Technology of China, Hefei, 230026, People’s Republic of China (Received 4 March 1998; accepted 8 July 1998)
An organothermal reduction process has been successfully developed for synthesis of nanocrystalline Ni2 P in benzene at 140 ±C. An x-ray powder diffraction pattern (XRD) indicated that the product was pure hexagonal Ni2 P phase with a cell constants a 0.5866 and c 0.3377 nm. Transmission electron microscopy (TEM) showed that the average particle size of the powders was 40 nm with a circular-shaped flake morphology.
Metal phosphides and arsenides are technologically important as semiconductors, phosphorescence devices, and electronic components.1 As one kind of nickel phosphides, dinickel phosphide (Ni2 P) is very resistant to corrosions2 and oxidation.3 Conventionally, dinickel phosphide is made by direct combination of elements,4 by the reaction of highly toxic phosphine with metal or metal hydride5 in a metal-organic chemical vapor deposition process or via self-propagating high-temperature synthesis.6 These methods typically require high temperatures (1000 ±C) and long annealing periods to produce the crystalline materials. Recently, Fitzmaurice et al.7 reported that light grinding of a mixture of Na3 E (E As or P) and MCln (M metal) in an agate pestle and mortar initiates a solid-state metathesis (SSM) reaction to prepare metal phosphides and arsenides. However, the main product Mx E is contained in a fused black mass, which shows a smooth morphology and the presence of metal, pnictide, and to a lesser extent sodium and chlorine. Prior to our work, Motojima et al.2 reported a method to prepare dinickel phosphide by reacting a gas mixture of NiCl2 , PCl3 , H2 , and Ar at high temperature (.950 ±C). In addition, dinickel phosphide was also prepared by the reduction of nickel phosphate with hydrogen at high temperature.8 Recently, our group has successfully synthesized GaN,9 b –In2 S3 nanocrystalline,10 and Bi2 S3 nanorods11 in organic media via the solvent thermal process. Here, we report on a new
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Address all correspondence to these authors. J. Mater. Res., Vol. 13, No. 12, Dec 1998
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low temperature route to nanocrystalline Ni2 P via an organothermal reduction process in benzene. In a typical reaction, 0.005 mol analytical grade NiCl2 and 5 ml PCl3 were mixed with benzene in a Teflon-lined autoclave of 100 ml capacity, which was filled with benzene u
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