Jiangsu Key Laboratory of Biofunctional Materials, College of Chemistry and Materials Science, Nanjing Normal University, Nanjing 210097, PR China.
Chemistry. 2011 Mar 21;17(13):3739-45. doi: 10.1002/chem.201002066. Epub 2011 Feb 23.
Spherical PbSe hollow nanostructure assemblies (HNSAs) were synthesized by a simple one-pot solid/liquid-phase reaction in which solid KPbI(3)⋅2 H(2)O and SeO(2) 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.
球形 PbSe 空心纳米结构组装体 (HNSAs) 是通过一种简单的固/液单相反应合成的,其中固体 KPbI(3)⋅2H(2)O 和 SeO(2) 在油酸/十二胺/1-十八烯中于 250°C 加热 30 分钟。XRD 分析表明,所得到的产物为立方相 PbSe,结晶良好。FESEM 和 TEM 图像显示,所得到的球形 PbSe 组装体由小的、不规则的、熔融的空心纳米结构构建块组成。基于温度和时间依赖性研究以及对照实验,提出了在高温成熟阶段原位形成的固态 PbSe 纳米晶聚集体的熔融盐腐蚀来解释这种新型组装体的形成。此外,当反应温度进一步升高至 280 或 320°C 而其他条件不变时,生成立方相和正交相混合相 PbSe HNSAs。所得到的 PbSe HNSAs 表现出优异的电致化学发光 (ECL) 性能。在约-1.4 和 +1.5V(相对于 Ag/AgCl)处观察到两个强而稳定的发射峰。特别是,ECL 强度受 PbSe 的晶体相影响。