Synthesis of stable CdS nanocrystals using experimental design: optimization of the emission

The optimization of the synthesis of CdS nanocrystals (CdS NCs) stabilized with 3-mercaptopropionic (MPA) acid was studied using chemometric tools. All factors (variables) involved in the CdS NC synthesis were optimized. The analysed factors were the CdCl 2 , Na 2 S and 3-mercaptiopropionic acid con...

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Bibliographic Details
Published in:New journal of chemistry 2019-08, Vol.43 (32), p.12836-12845
Main Authors: Di Tocco, Aylén, Porcal, Gabriela Valeria, Riberi, Walter Iván, Zon, María Alicia, Fernández, Héctor, Robledo, Sebastian Noel, Arévalo, Fernando Javier
Format: Article
Language:English
Subjects:
Cadmium chloride
Design of experiments
Design optimization
Factorial design
Fluorescence
Nanocrystals
Sodium sulfide
Synthesis
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Summary:The optimization of the synthesis of CdS nanocrystals (CdS NCs) stabilized with 3-mercaptopropionic (MPA) acid was studied using chemometric tools. All factors (variables) involved in the CdS NC synthesis were optimized. The analysed factors were the CdCl 2 , Na 2 S and 3-mercaptiopropionic acid concentrations, and the time and temperature of the reaction. First, a full factorial design was carried out to evaluate the effect of all factors and their interactions, where the analysed factors were the CdCl 2 , Na 2 S and 3-mecaptiopropionic acid concentrations, and the time and temperature of the reaction. Second, a central composite design was chosen for optimization of the factors. The optimization of the CdS NC synthesis was carried out using the fluorescence intensity of CdS NCs. The values of the factors that maximize the fluorescence intensity of the synthetized CdS NCs were a concentration range of CdCl 2 , Na 2 S and MPA of (7.96-8.49) × 10 −3 mol L −1 , (6.06-8.50) × 10 −3 mol L −1 and (47.58-71.85) × 10 −3 mol L −1 , respectively, and a temperature range of (20-74) °C. Under the best conditions, the relative error was 14%. The optimized CdS NCs were purified through size selective precipitation. A fluorescence quantum yield (QY) of 1.02% was obtained. On the other hand, the bulk band gap of the CdS NCs was 2.99 eV (close to 415 nm). The synthesis of the NCs studied was reproducible and they had good fluorescence. This work investigates CdS nanocrystal synthesis by applying chemometric tools. Very good reproducibility of nanocrystals of CdS was obtained.
ISSN:1144-0546
1369-9261
DOI:10.1039/c9nj02145k