We describe the development of a high-throughput, automated method for conducting TEM characterization of materials, to remove this bottleneck from the discovery process. We propose this approach will be of particular utility within the broad field of block copolymer amphiphile assembly, where researchers wish to rapidly formulate for phases of interest including vesicles in drug delivery, fragrance and cosmetic formulation. A vesicle phase is not immediately accessible, without screening block sizes and conditions, and is difficult to converge on using DLS for example, but rather often requires analysis by TEM combined with more sophisticated scattering experiments.<br/><br/>In this presentation, we will describe the very rapid generation (hours of work as opposed to months) of phase diagrams for block copolymer amphiphiles. We demonstrate the high-throughput approach for two separate types of amphiphilic block copolymers. One type, consisting of poly(ethylene glycol)-block-poly(hydroxypropyl methacrylate), the other consisting of poly(2-(dimethylamino)ethyl methacrylate)-block-poly(hydroxypropyl methacrylate), were each prepared by systematically varying the degree of polymerization of the hydrophobic block. These were each synthesized in 96-well plates to rapidly generate a range of morphologies in aqueous solution. In this manner, 45 different assembled polymer samples were prepared at a time. These samples were sampled by automated picoliter volume liquid handling (piezoelectric robotic dispenser) and analyzed by automated transmission electron microscopy (TEM by SerialEM) and automated image analysis to rapidly generate phase diagrams. Moreover, we will describe approaches for conducting polymerization and assembly of nanomaterials in situ, in a liquid TEM cell. Linking the process of reaction development and discovery directly to the process of imaging materials.

High throughput and solution phase TEM for discovery of new pisa reaction manifolds

2019 Fall National Meeting

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