Impact of microwave irradiation on cyclo-octeno-1,2,3-selenadiazole: formation of selenium nanoparticles and their polymorphs

Abstract

In this work a one-pot microwave assisted synthesis of selenium nanoparticles and their different forms, by decomposition of cyclo-octeno-1,2,3-selenadiazole is described first ever time.

Microwave-Assisted Green Synthesis and Antioxidant Activity of Selenium Nanoparticles Using Theobroma cacao L. Bean Shell Extract

“…Moreover, it was observed that higher amounts of sodium selenite increased the crystalline size of SeNPs, at a fixed concentration of CBSE. This behaviour could be explained by considering that high amounts of the metal precursor involve a large number of selenium nuclei that could agglomerate during the growth step, giving rise to nanoparticles with larger size [23]. These results agree with those reported by other authors who evaluated the influence of using reducing and capping agents during the synthesis of SeNPs [31,32], obtaining larger nanoparticles when the concentration of these agents was lower than the concentration of the metal precursor.…”

“…This pattern could be indexed according to the trigonal phase of SeNPs (crystalline t-SeNPs), in agreement with results obtained by Raman spectroscopy. The presence of this structure could be due to the partial conversion of amorphous nanoparticles to their most stable crystalline form [23]. The prepared SeNPs calculated crystalline size was 41.5 nm using Debye–Scherrer’s equation, which was lower than the reported value of 58 nm by Alagesan et al [8] using a leaf extract of Withania somnifera .…”

“…Microwave radiation can be absorbed easily by the mixture solution containing the ions salt and reducing agents. Consequently, localized superheating occurs resulting in fast and efficient heating, completing reactions in minutes or even seconds using less energy [22,23]. Green synthesized NPs under microwave irradiation have been reported to have minimum particle size and particle size distributions, and maximum stability [19].…”

Synthesis of a one-dimensional atomic crystal of vanadium selenide (V2Se9)

“…Furthermore, Se, which is observed at all temperatures, is dispersed in several places in the form of particles; Se can be removed by heat treatment at its sublimation temperature (>221 C). 38 The remaining Se particles can be removed by sublimation (heat treatment in a tube furnace at 250 C under Ar atmosphere for 24 h). It is evident from the XRD pattern ( Fig.…”

Inorganic Molecular Chain Nb2Se9: Synthesis of Bulk Crystal and One‐Atom‐Thick Level Exfoliation

“…The sublimation of residual Se in Nb 2 Se 9 can be confirmed by thermogravimetric characterization using differential thermal analysis (DTA) and thermogravimetric analysis (TGA). Before the Se sublimation process (Figure c), the mass decreased near 280 °C owing to sublimation of Se . In addition, mass reduction was observed at 500 °C owing to decomposition of Nb 2 Se 9 (Nb 2 Se 9 [s] → 2NbSe 2 [s] + 5Se [g], an endothermic reaction with negative DTA values in a wide temperature range).…”