Synthesis And Electrochemical Analysis Of One-dimensional Se Nanomaterials By Microwave-heating Method

T-Se nanowire bundles with length up to tens of micrometers and diameters of 30-50 run were prepared by microwave-heating reduction of selenium dioxide (SeO₂) with glucose at 100°C in 20 min without stirring, employing ammonia (concentration 15%) as solvent. Products were characterized by XRD, TEM, FESEM. Some experiments were taken to observe the effects of ammonia and PVP .It is found that the growth mechanism of Se nanomaterials is different from the familiar sphere-wire process. A novel flake-cracking mechanism is proposed.Furthermore, hammer-shape t-Se nanorod bundles with length up to 20μm and diameters of 100-120 nm were first prepared by microwave-heating reduction of selenium dioxide (SeO₂) with glucose at 120℃C in 30 min under stirring, employing ammonia (concentration 25%) as solvent. It was found stirring and ammonia play an important rule in formation of hammer-shape t-Se nanorod bundles. On the basis of TEM of intermediates, a novel flake cracking-reaction mechanism is proposed.Powders of t-Se nanowire bundles synthesized by microwave-heating and t-Se in bulk were prepared for working electrode. The 0.2 M NaOH solution was degassed with ultrapure N₂ prior to experiment. Three- electrode was used to carry out Liner Sweep Voltammetry(LSV) experiment. The result suggests that the t-Se nanowire bundles were oxidized more easily than t-Se in bulk, t-Se in bulk was reduced more easily than t-Se nanowire bundles. The discharge behavior of t-Se nanowire bundles is excellent compared with t-Se in bulk, t-Se nanowire bundles can used as material for hydrogen storage.