Park Nayon, Monahan Madison, Ritchhart Andrew, Friedfeld Max R, Cossairt Brandi M
Department of Chemistry, University of Washington.
Department of Chemistry, University of Washington;
J Vis Exp. 2019 May 7(147). doi: 10.3791/59425.
This text presents a method for the synthesis of In37P20(O2C14H27)51 clusters and their conversion to indium phosphide quantum dots. The In37P20(O2CR)51 clusters have been observed as intermediates in the synthesis of InP quantum dots from molecular precursors (In(O2CR)3, HO2CR, and P(SiMe3)3) and may be isolated as a pure reagent for subsequent study and use as a single-source precursor. These clusters readily convert to crystalline and relatively monodisperse samples of quasi-spherical InP quantum dots when subjected to thermolysis conditions in the absence of additional precursors above 200 °C. The optical properties, morphology, and structure of both the clusters and quantum dots are confirmed using UV-Vis spectroscopy, photoluminescence spectroscopy, transmission electron microscopy, and powder X-ray diffraction. The molecular symmetry of the clusters is additionally confirmed by solution-phase P NMR spectroscopy. This protocol demonstrates the preparation and isolation of atomically-precise InP clusters, and their reliable and scalable conversion to InP QDs.
本文介绍了一种合成In37P20(O2C14H27)51团簇及其转化为磷化铟量子点的方法。In37P20(O2CR)51团簇已被观察到是由分子前驱体(In(O2CR)3、HO2CR和P(SiMe3)3)合成InP量子点过程中的中间体,并且可以作为纯试剂分离出来,用于后续研究以及用作单源前驱体。当在200℃以上不存在额外前驱体的情况下进行热解时,这些团簇很容易转化为准球形InP量子点的晶体且相对单分散的样品。使用紫外可见光谱、光致发光光谱、透射电子显微镜和粉末X射线衍射来确认团簇和量子点的光学性质、形态和结构。通过溶液相31P核磁共振光谱进一步确认了团簇的分子对称性。该方案展示了原子精确的InP团簇的制备和分离,以及它们可靠且可扩展地转化为InP量子点的过程。