High-Throughput Workflow for the Synthesis of CdSe Nanocrystals Using a Sonochemical Materials Acceleration Platform

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Abstract
We present a complete open-hardware and software Materials Acceleration Platform (MAP) for sonochemical synthesis of nanocrystals using a versatile tool-changing platform (Jubilee) configured for automated ultrasound application, a liquid-handling robot (Opentrons OT2) and a well-plate spectrometer. An automated high-throughput protocol was developed demonstrating the synthesis of CdSe nanocrystals using sonochemistry and different combinations of sample conditions, including precursor and ligand compositions and concentrations. Cavitation caused by ultrasound fields cause local and transient increases in temperature and pressure sufficient to drive the decomposition of organometalic precursors to drive the chemical reaction leading to nanocrystal formation. A total of 625 unique sample conditions were prepared and analyzed in triplicate with an individual sample volume of as little as 0.5 mL, which drastically reduced chemical waste and experimental times. The rapid onset of cavitation and quick dissipation of energy results in fast nucleation with little nanocrystal growth leading to the formation of small nanocrystals or magic-size clusters (MSCs) depending on composition. Using the effective mass approximation, the calculated QDs diameters obtained in all our experimental conditions ranged between 1.3 and 2.1 nm, which was also validated with small angle xray scattering (SAXS). Polydispersity, QD shape and optical properties largely varied depending on the concentration of ligands present in solution. Statistical analysis of the spectroscopic data corroborates the qualitative relationships observed from the optical characterization of the samples with the model-agnostic SHAP analysis. The complete workflow relies on relatively low-cost and open-source systems (<$15k for both robotic platforms). Automation and the reduced volumes also allows for cost-efficient experimentation, increasing the accessibility of this MAP. The high-throughput capabilities of the automated sonication platform, the extensible nature of the Jubilee system, and the modular nature of the protocol, make the workflow adaptable to a variety of future studies, including other nanocrystal design spaces, emulsification processes, and nanoparticle re-dispersion or exfoliation.
Funding Information
  • National Science Foundation (1917340)
  • National Science Foundation (1633216)

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