Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals

<p>Abstract</p> <p>We address two aspects of general interest for the chemical synthesis of colloidal semiconductor nanocrystals: (1) the rational design of the synthesis protocol aiming at the optimization of the reaction parameters in a minimum number of experiments; (2) the tran...

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Main Authors: Renard Olivier, Proti&#232;re Myriam, Nerambourg Nicolas, Reiss Peter
Format: Article
Language:English
Published: SpringerOpen 2011-01-01
Series:Nanoscale Research Letters
Subjects:
Online Access:http://www.nanoscalereslett.com/content/6/1/472
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author Renard Olivier
Proti&#232;re Myriam
Nerambourg Nicolas
Reiss Peter
author_facet Renard Olivier
Proti&#232;re Myriam
Nerambourg Nicolas
Reiss Peter
author_sort Renard Olivier
collection DOAJ
description <p>Abstract</p> <p>We address two aspects of general interest for the chemical synthesis of colloidal semiconductor nanocrystals: (1) the rational design of the synthesis protocol aiming at the optimization of the reaction parameters in a minimum number of experiments; (2) the transfer of the procedure to the gram scale, while maintaining a low size distribution and maximizing the reaction yield. Concerning the first point, the design-of-experiment (DOE) method has been applied to the synthesis of colloidal CdSe nanocrystals. We demonstrate that 16 experiments, analyzed by means of a Taguchi L<sub>16 </sub>table, are sufficient to optimize the reaction parameters for controlling the mean size of the nanocrystals in a large range while keeping the size distribution narrow (5-10%). The DOE method strongly reduces the number of experiments necessary for the optimization as compared to trial-and-error approaches. Furthermore, the Taguchi table analysis reveals the degree of influence of each reaction parameter investigated (e.g., the nature and concentration of reagents, the solvent, the reaction temperature) and indicates the interactions between them. On the basis of these results, the synthesis has been scaled up by a factor of 20. Using a 2-L batch reactor combined with a high-throughput peristaltic pump, different-sized samples of CdSe nanocrystals with yields of 2-3 g per synthesis have been produced without sacrificing the narrow size distribution. In a similar setup, the gram-scale synthesis of CdSe/CdS/ZnS core/shell/shell nanocrystals exhibiting a fluorescence quantum yield of 81% and excellent resistance of the photoluminescence in presence of a fluorescent quencher (aromatic thiol) has been achieved.</p> <p> <b>PACS: </b>81.20.Ka, 81.07.Bc, 78.67.Bf</p>
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spelling doaj.art-38b6de3cf337473aa93623baef064b472023-09-02T16:16:47ZengSpringerOpenNanoscale Research Letters1931-75731556-276X2011-01-0161472Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystalsRenard OlivierProti&#232;re MyriamNerambourg NicolasReiss Peter<p>Abstract</p> <p>We address two aspects of general interest for the chemical synthesis of colloidal semiconductor nanocrystals: (1) the rational design of the synthesis protocol aiming at the optimization of the reaction parameters in a minimum number of experiments; (2) the transfer of the procedure to the gram scale, while maintaining a low size distribution and maximizing the reaction yield. Concerning the first point, the design-of-experiment (DOE) method has been applied to the synthesis of colloidal CdSe nanocrystals. We demonstrate that 16 experiments, analyzed by means of a Taguchi L<sub>16 </sub>table, are sufficient to optimize the reaction parameters for controlling the mean size of the nanocrystals in a large range while keeping the size distribution narrow (5-10%). The DOE method strongly reduces the number of experiments necessary for the optimization as compared to trial-and-error approaches. Furthermore, the Taguchi table analysis reveals the degree of influence of each reaction parameter investigated (e.g., the nature and concentration of reagents, the solvent, the reaction temperature) and indicates the interactions between them. On the basis of these results, the synthesis has been scaled up by a factor of 20. Using a 2-L batch reactor combined with a high-throughput peristaltic pump, different-sized samples of CdSe nanocrystals with yields of 2-3 g per synthesis have been produced without sacrificing the narrow size distribution. In a similar setup, the gram-scale synthesis of CdSe/CdS/ZnS core/shell/shell nanocrystals exhibiting a fluorescence quantum yield of 81% and excellent resistance of the photoluminescence in presence of a fluorescent quencher (aromatic thiol) has been achieved.</p> <p> <b>PACS: </b>81.20.Ka, 81.07.Bc, 78.67.Bf</p>http://www.nanoscalereslett.com/content/6/1/472semiconductor nanocrystalsquantum dotssynthesisexperimental planfluorescencescale-upcolloids
spellingShingle Renard Olivier
Proti&#232;re Myriam
Nerambourg Nicolas
Reiss Peter
Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
Nanoscale Research Letters
semiconductor nanocrystals
quantum dots
synthesis
experimental plan
fluorescence
scale-up
colloids
title Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
title_full Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
title_fullStr Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
title_full_unstemmed Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
title_short Rational design of the gram-scale synthesis of nearly monodisperse semiconductor nanocrystals
title_sort rational design of the gram scale synthesis of nearly monodisperse semiconductor nanocrystals
topic semiconductor nanocrystals
quantum dots
synthesis
experimental plan
fluorescence
scale-up
colloids
url http://www.nanoscalereslett.com/content/6/1/472
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AT proti232remyriam rationaldesignofthegramscalesynthesisofnearlymonodispersesemiconductornanocrystals
AT nerambourgnicolas rationaldesignofthegramscalesynthesisofnearlymonodispersesemiconductornanocrystals
AT reisspeter rationaldesignofthegramscalesynthesisofnearlymonodispersesemiconductornanocrystals