Synthesis of colloidal PbSe nanoparticles using a microwave-assisted segmented flow reactor

Hostetler, Eric B.; Kim, Ki Joong; Oleksak, Richard P.; Fitzmorris, Robert C.; Peterson, Daniel A.; Padmavathi, C.; Chang, Chih-Hung; Paul, Brian K.; Schut, David M.; Herman, Gregory S.

doi:10.1016/j.matlet.2014.04.089

Cited by 32 publications

(28 citation statements)

References 33 publications

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“…By heating the solution directly and uniformly using microwaves, rather than by conduction through the tubing, the nucleation of colloidal QDs is promoted over the deposition of QDs on the walls of the tubing. Experiments comparing single phase and segmented flow showed that segmenting the solution flow by introducing argon gas also reduced sidewall deposition by increasing circulation as previously described (Hostetler et al 2014;Kim et al 2014a). Segmented flow also leads to a narrow distribution of residence times (Trachsel et al 2005) for the QDs, something that is critical for achieving a narrow size distributions (Marre et al 2008;Yen et al 2003).…”

Section: Reactor Designsupporting

confidence: 59%

“…The most important advantage of the CFMW reactor is the ability to optimize the synthesis using very small volumes, and then allowing scale up with the same equipment and without developing a completely new process. This reactor design can be applied to many different QD and nanoparticle systems (Hostetler et al 2014;Kim et al 2014).…”

Section: Reactor Designmentioning

confidence: 99%

“…MWCFRs have been investigated extensively for the synthesis of organic molecules and have shown to be highly versatile, scalable, and provide high production rates (Bergamelli et al 2010;Glasnov and Kappe 2007). MWCFRs have recently been used to synthesize PbSe (Hostetler et al 2014) and CuInSe 2 nanoparticles with good control over particle size distributions (Kim et al 2014).…”

Section: Introductionmentioning

confidence: 99%

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Structural and optical characterization of CuInS2 quantum dots synthesized by microwave-assisted continuous flow methods

et al. 2015

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Semiconductor quantum dots (QDs) have recently been incorporated into consumer displays and lighting technologies. Now that these materials are being produced on industrial scales, it is important to investigate scalable synthetic methods and less toxic materials and chemistries. To achieve these goals, we have synthesized cadmium-free, visible light-emitting QDs using a microwave-assisted continuous flow reactor. After synthesis, the CuInS 2 QD cores underwent a near-complete Zn cation exchange reaction in a batch reactor, followed by the growth of a ZnS shell. Analysis of X-ray diffraction, transmission electron microscopy, and Raman spectroscopy data indicate that the crystal structure changes from CuInS 2 (chalcopyrite) to ZnS (zincblende) during the cation exchange reaction. Compositional analysis indicated that the core/shell QDs were *98 % ZnS, with Cu and In present at much lower concentrations. The photoluminescence (PL) peak position was blue shifted for longer cation exchange reactions, and it was found that the ZnS shell was necessary for improved PL stability.The synthesized QDs have a PL down conversion efficiency of *65 % when using a blue LED source.

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Section: Reactor Designsupporting

confidence: 59%

Section: Reactor Designmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Structural and optical characterization of CuInS2 quantum dots synthesized by microwave-assisted continuous flow methods

et al. 2015

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“…SMFRs with inner recirculation are applicable solutions of the sparkling issue in single-phase microfluidic reactors coupled with the microwave because this issue is caused by the in-situ deposition of the nanomaterials on the inner channel wall at the microwave zone. Chalcogenide binary PbSe NPs [ 101 ] and ternary CuInSe 2 NPs [ 102 ] have been synthesized using microwave-assisted SMFRs. Chang’s group employed microwave-assisted SMFRs to develop the route for the separation of crystal nucleation and growth stages and achieved precise control over the reaction by fine-tuning of the parameters and stage separation ( Figure 9 a) [ 102 ].…”

Section: Nanomaterials Synthesis By Segmented Flowmentioning

confidence: 99%

Segmented Microfluidic Flow Reactors for Nanomaterial Synthesis

Kim

Chang

2020

Nanomaterials

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Microfluidic reactors have remarkably promoted the synthesis and investigation of advanced nanomaterials due to their continuous mode and accelerated heat/mass transfer. Notably, segmented microfluidic flow reactors (SMFRs) are an important class of microfluidic reactors that have been developed to accurately manipulate nanomaterial synthesis by further improvement of the residence time distributions and unique flow behaviors. This review provided a survey of the nanomaterial synthesis in SMFRs for the aspects of fluid dynamics, flow patterns, and mass transfer among and within distinct phases and provided examples of the synthesis of versatile nanomaterials via the use of different flow patterns.

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“…Nanomaterial synthesis in a micro-reactor with precisely controlled reaction conditions (i.e., minimize heat/mass transfer by instantaneous mixing) has become a versatile approach in modern synthetic chemistry [ 15 , 16 ] and been developed for producing metals (Au, Ag) [ 17 , 18 , 19 , 20 , 21 ], metal oxides (ZnO, TiO 2 , Fe 3 O 4 , SiO 2 ) [ 22 , 23 , 24 , 25 ], chalcogenides (CdSe, PbSe, CuInSe 2 ) [ 26 , 27 , 28 ], and core-shell (Fe 2 O 3 /SiO 2 , CdSe/ZnS) NPs [ 29 , 30 ]. These methods should be amenable to developing an industrially-relevant large-scale synthesis method by arraying many micro-reactors in parallel (hundreds to millions) [ 31 ].…”

Section: Introductionmentioning

confidence: 99%

Characterization of Cotton Ball-like Au/ZnO Photocatalyst Synthesized in a Micro-Reactor

et al. 2018

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Noble metal/metal oxide nanostructures are an efficient system in photocatalysis. Continuous and scalable production of advanced particle systems will be a requirement for commercial-scale deployment for many applications, including photocatalysis. In this work, Au/ZnO structures were synthesized in a continuous flow micro-reactor at room temperature and the detailed characteristics of the product indicate a specific cotton ball-like core-shell microstructure that showcases specific advantages compared to traditional batch synthesis methods. The formation pathway of the core-shell Au/ZnO structures is discussed with the pH-dependent speciation diagram, and photocatalytic activity was assessed under simulated sunlight, demonstrating the enhanced performance of the cotton ball-like Au/ZnO microstructures in photocatalytic dye degradation. This work describes the application of microreaction technology in the continuous production of metal/metal oxide photocatalysts.

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Synthesis of colloidal PbSe nanoparticles using a microwave-assisted segmented flow reactor

Cited by 32 publications

References 33 publications

Structural and optical characterization of CuInS2 quantum dots synthesized by microwave-assisted continuous flow methods

Structural and optical characterization of CuInS2 quantum dots synthesized by microwave-assisted continuous flow methods

Segmented Microfluidic Flow Reactors for Nanomaterial Synthesis

Characterization of Cotton Ball-like Au/ZnO Photocatalyst Synthesized in a Micro-Reactor

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