Towards Data-Rich Experimental Workflows for Nanomaterial Synthesis Through Modular Automated Reactor and Purification Platforms

Automated workflows increasingly are implemented towards nanomaterial synthesis for optoelectronic and catalytic applications. One application of these automated platforms and workflows is to investigate the effect of synthesis parameters on nanoparticle synthesis outcomes to generate hypotheses for nanoparticle nucleation and growth mechanisms and thus to guide future synthesis. Such automated platform-based investigation requires thorough characterization of reaction product streams to determine size distribution, shape, and phase of synthesized nanoparticles.<br/><br/>Presently, however, most automated nanoparticle synthesis platforms rely on optical characterization due to its availability and ease of integration. This limits the types of materials that can be explored with automated workflows. While interfacing automated platforms with powerful structural characterization tools such as TEM imaging of X-Ray beamline-based methods is theoretically possible, in practice this is difficult due to the complexity of most automated platforms, in terms of portability and set-up. Furthermore, for structural characterization such as TEM imaging requires purification of synthesized nanoparticles. Addressing this issue requires the development of modular, <i>portable</i> synthesis and purification platforms that can be seamlessly interfaced with powerful platforms in specialized materials characterization facilities.<br/><br/>This talk will report on a modular, portable purification platform that enables downstream <i>in-situ</i> TEM imaging for automated nanoparticle synthesis workflows. Using commercial off-the-shelf hardware and silica media, we fabricated a versatile, automated size-exclusion chromatography system for efficient separation of CdSe quantum dots (QDs) from crude organic-phase reaction mixtures. These purified nanoparticles can then be rapidly characterized using liquid-phase TEM or characterized in batches at a higher resolution using grid TEM. Integrating this automated nanoparticle purification platform with downstream TEM platforms and upstream portable automated synthesis platforms, enables data-rich automated synthesis and structural characterization workflows that facilitate investigation into the mechanisms of nanoparticle formation for different systems.