Grogan, Joseph M
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Publication The Nanoaquarium: A Nanofluidic Platform for in SiTu Transmission Electron Microscopy in Liquid Media(2011-12-21) Grogan, Joseph MThere are many scientifically interesting and technologically relevant nanoscale phenomena that take place in liquid media. Examples include aggregation and assembly of nanoparticles; colloidal crystal formation; liquid phase growth of structures such as nanowires; electrochemical deposition and etching for fabrication processes and battery applications; interfacial phenomena; boiling and cavitation; and biological interactions. Understanding of these fields would benefit greatly from real-time, in situ transmission electron microscope (TEM) imaging with nanoscale resolution. Most liquids cannot be imaged by traditional TEM due to evaporation in the high vacuum environment and the requirement that samples be very thin. Liquid-cell in situ TEM has emerged as an exciting new experimental technique that hermetically seals a thin slice of liquid between two electron transparent membranes to enable TEM imaging of liquid-based processes. This work presents details of the fabrication of a custom-made liquid-cell in situ TEM device, dubbed the nanoaquarium. The nanoaquarium’s highlights include an exceptionally thin sample cross section (10s to 100s of nm); wafer scale processing that enables high-yield mass production; robust hermetic sealing that provides leak-free operation without use of glue, epoxy, or any polymers; compatibility with lab-on-chip technology; and on-chip integrated electrodes for sensing and actuation. The fabrication process is described, with an emphasis on direct wafer bonding. Experimental results involving direct observation of colloid aggregation using an aqueous solution of gold nanoparticles are presented. Quantitative analysis of the growth process agrees with prior results and theory, indicating that the experimental technique does not radically alter the observed phenomenon. For the first time, in situ observations of nanoparticles at a contact line and in an evaporating thin film of liquid are reported, with applications for techniques such as dip-coating and drop-casting, commonly used for depositing nanoparticles on a surface via convective-capillary assembly. Theoretical analysis suggests that the observed particle motion and aggregation are caused by gradients in surface tension and disjoining pressure in the thin liquid film.Publication In Situ Liquid-Cell Electron Microscopy of Colloid Aggregation and Growth Dynamics(2011-06-16) Grogan, Joseph M.; Bau, Haim; Rotkina, LolitaWe report on real-time observations of the aggregation of gold nanoparticles using a custom-made liquid cell that allows for in situ electron microscopy. Process kinetics and fractal dimension of the aggregates are consistent with three-dimensional cluster-cluster diffusion-limited aggregation, even for large aggregates, for which confinement effects are expected. This apparent paradox was resolved through in situ observations of the interactions between individual particles as well as clusters at various stages of the aggregation process that yielded the large aggregates. The liquid cell described herein facilitates real-time observations of various processes in liquid media with the high resolution of the electron microscope.Publication Bubble and Pattern Formation in Liquid Induced by an Electron Beam(2013-12-08) Grogan, Joseph M; Schneider, Nicholas M; Bau, Haim H; Ross, Frances MLiquid cell electron microscopy has emerged as a powerful technique for in situ studies of nanoscale processes in liquids. An accurate understanding of the interactions between the electron beam and the liquid medium is essential to account for, suppress, and exploit beam effects. We quantify the interactions of high energy electrons with water, finding that radiolysis plays an important role, while heating is typically insignificant. For typical imaging conditions, we find that radiolysis products such as hydrogen and hydrated electrons achieve equilibrium concentrations within seconds. At sufficiently high dose-rate, the gaseous products form bubbles. We image bubble nucleation, growth, and migration. We develop a simplified reaction-diffusion model for the temporally and spatially varying concentrations of radiolysis species and predict the conditions for bubble formation by . We discuss the conditions under which hydrated electrons cause precipitation of cations from solution, and show that the electron beam can be used to “write” structures directly, such as nanowires and other complex patterns, without the need for a mask.