Wang Fudong, Tang Rui, Buhro William E
Department of Chemistry and Center for Materials Innovation, Washington University, Saint Louis, Missouri 63130-4899, USA.
Nano Lett. 2008 Oct;8(10):3521-4. doi: 10.1021/nl801692g. Epub 2008 Aug 29.
Tri-n-octylphosphine oxide (TOPO) is a commonly used solvent for nanocrystal synthesis. Commercial TOPO samples contain varying amounts of phosphorus-containing impurities, some of which significantly influence nanocrystal growth. Consequently, nanocrystal syntheses often give irreproducible results with different batches of TOPO solvent. In this study, we identify TOPO impurities by (31)P NMR, and correlate their presence with the outcomes of CdSe nanocrystal syntheses. We subsequently add the active impurity species, one by one, to purified TOPO to confirm their influence on nanocrystal syntheses. In this manner, di-n-octylphosphine oxide (DOPO) is shown to assist CdSe quantum-dot growth; di-n-octylphosphinic acid (DOPA) and mono-n-octylphosphinic acid (MOPA) are shown to assist CdSe quantum-rod growth, and DOPA is shown to assist CdSe quantum-wire growth. (The TOPO impurity n-octylphosphonic acid, OPA, has been previously shown to assist quantum-rod growth.) The beneficial impurities are prepared on multigram scales and can be added to recrystallized TOPO to provide reproducible synthetic results.
三辛基氧化膦(TOPO)是一种常用于纳米晶体合成的溶剂。市售的TOPO样品含有不同量的含磷杂质,其中一些杂质会显著影响纳米晶体的生长。因此,使用不同批次的TOPO溶剂进行纳米晶体合成时,常常会得到不可重复的结果。在本研究中,我们通过³¹P核磁共振(NMR)鉴定TOPO中的杂质,并将它们的存在与CdSe纳米晶体合成的结果相关联。随后,我们将活性杂质逐一添加到纯化的TOPO中,以确认它们对纳米晶体合成的影响。通过这种方式,我们发现二辛基氧化膦(DOPO)有助于CdSe量子点的生长;二辛基次膦酸(DOPA)和单辛基次膦酸(MOPA)有助于CdSe量子棒的生长,并且DOPA有助于CdSe量子线的生长。(之前已经证明TOPO杂质正辛基膦酸(OPA)有助于量子棒的生长。)这些有益杂质可以大量制备,并添加到重结晶的TOPO中,以提供可重复的合成结果。