Facile synthesis of PbSe hollow nanostructure assemblies via a solid/liquid-phase chemical route and their electrogenerated chemiluminescence properties

Spherical PbSe hollow nanostructure assemblies (HNSAs) were synthesized by a simple one-pot solid/liquid-phase reaction in which solid KPbI ₃·2 H₂O and SeO₂ are heated in oleic acid/dodecylamine/1-octadecene at 250 °C for 30 min. XRD analysis shows that the obtained product is cubic-phase PbSe and well crystallized. FESEM and TEM images reveal that the obtained spherical PbSe assemblies are made up of small, irregular, and fused hollow nanostructure building blocks. On the basis of temperature- and time-dependent investigations as well as control experiments, molten-salt corrosion of solid PbSe nanocrystal aggregates formed in situ during the high-temperature ripening stage is suggested to explain the formation of such novel assemblies. Moreover, when the reaction temperature is further increased to 280 or 320 °C with other conditions unchanged, cubic and orthorhombic mixed-phase PbSe HNSAs is generated. The obtained PbSe HNSAs exhibit excellent electrogenerated chemiluminescence (ECL) performance. Two strong and stable emission peaks at about -1.4 and +1.5 V (vs. Ag/AgCl) are observed. In particular, the ECL intensity is influenced by the crystal phase of PbSe.