Key Laboratory of Novel Thin Film Solar Cells, Institute of Applied Technology, Hefei Institutes of Physical Science, Chinese Academy of Sciences, Hefei, 230031, P. R. China.
Nanoscale. 2016 May 21;8(19):10021-5. doi: 10.1039/c6nr02505f. Epub 2016 May 3.
Phosphine-free synthesis of CISe quantum dots (QDs) is highly desirable, yet it has been challenging. The main difficulty lies in achieving phosphine-free Se precursors. Most reported protocols for the synthesis of size-confined CISe QDs highly depend on the use of air-sensitive, toxic, and expensive alkylphosphines to prepare reactive Se precursors and to confine particle growth. Herein, we present a new amine/thiol combination-based route to Se precursors that may enable a general synthesis of phosphine-free selenide QDs. What's more, instead of the traditional "hot-injection" method, we also report the first one-pot noninjection synthesis of high quality CISe QDs enabled by our strategy. A very high chemical yield of ∼95% is demonstrated, as well as the facile gram-scale production of monodisperse CISe QDs. By simply adjusting the amount of 1-dodecanethiol used in the synthesis, we are able to produce CISe QDs with continuous tunability of the particle size from ∼2 nm to ∼10 nm, and hence their intrinsic optical properties.
无膦合成 CISe 量子点(QD)是非常需要的,但一直具有挑战性。主要的困难在于实现无膦硒前体。大多数报道的用于合成尺寸受限的 CISe QD 的方案高度依赖于使用空气敏感、有毒和昂贵的烷基膦来制备反应性硒前体并限制颗粒生长。在此,我们提出了一种新的基于胺/硫醇的硒前体合成路线,可能能够实现一般的无膦硒化物 QD 的合成。更重要的是,我们还报告了首次通过我们的策略实现的高质量 CISe QD 的一锅无注入合成。证明了高达约 95%的化学产率,以及易于进行克级规模的单分散 CISe QD 的生产。通过简单地调整 1-十二硫醇在合成中的用量,我们能够生产出具有从约 2nm 到约 10nm 连续可调的粒径的 CISe QD,从而实现其本征光学性质。