title: Continuous-flow synthesis of CdSe quantum dots: a size-tunable and scalable approach.
abstract: In recent years, continuous-flow/microreactor processing for the preparation of colloidal nanocrystals has received considerable attention. The intrinsic advantages of microfluidic reactors have opened new opportunities for the size-controlled synthesis of nanocrystals either in the laboratory or on a large scale. Herein, an experimentally simple protocol for the size-tunable continuous-flow synthesis of rather monodisperse CdSe quantum dots (QDs) is presented. CdSe QDs are manufactured by using cadmium oleate as cadmium source, selenium dioxide as selenium precursor, and 1-octadecene as solvent. Exploiting selenium dioxide as selenium source and 1-octadecene as solvent allows execution of the complete process in open air without any requirement for air-free manipulations using a glove box or Schlenk line. Continuous-flow processing is performed with a stainless steel coil of 1.0 mm inner diameter pumping the combined precursor solution through the reactor by applying a standard HPLC pump. The effect of different reaction parameters, such as temperature, residence time, and flow rate, on the properties of the resulting CdSe QDs was investigated. A temperature increase from 240 to 260 °C or an extension of the residence time from 2 to 20 min affords larger nanocrystals (range 3-6 nm) whereas the size distribution does not change significantly. Longer reaction times and higher temperatures result in QDs with lower quantum yields (range 11-28 %). The quality of the synthesized CdSe QDs was confirmed by UV/Vis and photoluminescence spectroscopy, small-angle X-ray scattering, and high-resolution transmission electron microscopy. Finally, the potential of this protocol for large-scale manufacturing was evaluated and by operating the continuous-flow process for 87 min it was possible to produce 167 mg of CdSe QDs (with a mean diameter of 4 nm) with a quantum yield of 28 %.
authors.affiliation: Christian Doppler Laboratory for Microwave Chemistry (CDLMC) and Karl Franzens University Graz, Heinrichstrasse 28, 8010 Graz, Austria.
authors.forename: Mojtaba
authors.initials: M
authors.lastname: Mirhosseini Moghaddam
authors.forename: Mostafa
authors.initials: M
authors.lastname: Baghbanzadeh
authors.forename: Amin
authors.initials: A
authors.lastname: Sadeghpour
authors.forename: Otto
authors.initials: O
authors.lastname: Glatter
authors.forename: C Oliver
authors.initials: CO
authors.lastname: Kappe
keywords: continuous flow; high-temperature chemistry; microreactors; nanocrystals; quantum dots