John Henry J. Scott

Methodology for imaging nano-to-microscale water condensation dynamics on complex nanostructures.

A better understanding of the role that nanoscale surface chemical heterogeneities and topographical features play in water droplet formation is necessary to improve design and robustness of nanostructured superhydrophobic surfaces as to make them fit for industrial applications. Lack of an imaging method capable of capturing the water condensation process on complex nanostructures with required magnification has thus far hindered experimental progress in this area. In this work, we demonstrate that by transferring a small part of a macroscale sample to a novel thermally insulated sample platform we are able to mitigate flooding and electron heating problems typically associated with environmental scanning electron microscopy of water condensation. We image condensation dynamics on individual complex particles and a superhydrophobic network of nanostructures fabricated from low thermal conductivity materials with an unobstructed 90° perspective of the surface-to-water interface with field of view as small as 1 μm(2). We clearly observe the three-stage drop growth process and demonstrate that even during late stages of the droplet growth the nearly spherical drop remains in a partially wetting Wenzel state.

Electron beam heating effects during environmental scanning electron microscopy imaging of water condensation on superhydrophobic surfaces

Superhydrophobic surfaces (SHSs) show promise as promoters of dropwise condensation. Droplets with diameters below ∼10 μm account for the majority of the heat transferred during dropwise condensation but their growth dynamics on SHS have not been systematically studied. Due to the complex topography of the surface environmental scanning electron microscopy is the preferred method for observing the growth dynamics of droplets in this size regime. By studying electron beam heating effects on condensed water droplets we establish a magnification limit below which the heating effects are negligible and use this insight to study the mechanism of individual drop growth.

Dropwise Condensation of Low Surface Tension Fluids on Omniphobic Surfaces

Compared to the significant body of work devoted to surface engineering for promoting dropwise condensation heat transfer of steam, much less attention has been dedicated to fluids with lower interfacial tension. A vast array of low-surface tension fluids such as hydrocarbons, cryogens, and fluorinated refrigerants are used in a number of industrial applications, and the development of passive means for increasing their condensation heat transfer coefficients has potential for significant efficiency enhancements. Here we investigate condensation behavior of a variety of liquids with surface tensions in the range of 12 to 28 mN/m on three types of omniphobic surfaces: smooth oleophobic, re-entrant superomniphobic, and lubricant-impregnated surfaces. We demonstrate that although smooth oleophobic and lubricant-impregnated surfaces can promote dropwise condensation of the majority of these fluids, re-entrant omniphobic surfaces became flooded and reverted to filmwise condensation. We also demonstrate that on the lubricant-impregnated surfaces, the choice of lubricant and underlying surface texture play a crucial role in stabilizing the lubricant and reducing pinning of the condensate. With properly engineered surfaces to promote dropwise condensation of low-surface tension fluids, we demonstrate a four to eight-fold improvement in the heat transfer coefficient.

Guided Three-Dimensional Catalyst Folding during Metal-Assisted Chemical Etching of Silicon

In recent years metal-assisted chemical etching (MaCE) of silicon, in which etching is confined to a small region surrounding metal catalyst templates, has emerged as a promising low cost alternative to commonly used three-dimensional (3D) fabrication techniques. We report a new methodology for controllable folding of 2D metal catalyst films into 3D structures using MaCE. This method takes advantage of selective patterning of the catalyst layer into regions with mismatched characteristic dimensions, resulting in uneven etching rates along the notched boundary lines that produce hinged 2D templates for 3D folding. We explore the dynamics of the folding process of the hinged templates, demonstrating that the folding action combines rotational and translational motion of the catalyst template, which yields topologically complex 3D nanostructures with intimately integrated metal and silicon features.

Direct Imaging of Complex Nano- to Microscale Interfaces Involving Solid, Liquid, and Gas Phases

Surfaces with special wetting properties not only can efficiently repel or attract liquids such as water and oils but also can prevent formation of biofilms, ice, and clathrate hydrates. Predicting the wetting properties of these special surfaces requires detailed knowledge of the composition and geometry of the interfacial region between the droplet and the underlying substrate. In this work we introduce a 3D quantitative method for direct nanoscale visualization of such interfaces. Specifically, we demonstrate direct nano- to microscale imaging of complex fluidic interfaces using cryostabilization in combination with cryogenic focused ion beam milling and SEM imaging. We show that application of this method yields quantitative information about the interfacial geometry of water condensate on superhydrophilic, superhydrophobic, and lubricant-impregnated surfaces with previously unattainable nanoscale resolution. This type of information is crucial to a fundamental understanding as well as the design of surfaces with special wetting properties.

Three dimensional aspects of droplet coalescence during dropwise condensation on superhydrophobic surfaces

We report formation of nano-to-microscale satellite droplets in the geometrical shadow of high contact angle primary drops during dropwise water condensation on a nanostructured superhydrophobic surface (SHS). The primary drops contribute to the heat transfer process by sweeping up satellite droplets without covering their nucleation site and thus allow for rapid condensation of multiple droplets from the same site.

Dynamics of nanoparticle self-assembly into superhydrophobic liquid marbles during water condensation.

Nanoparticles adsorbed onto the surface of a drop can fully encapsulate the liquid, creating a robust and durable soft solid with superhydrophobic characteristics referred to as a liquid marble. Artificially created liquid marbles have been studied for about a decade but are already utilized in some hair and skin care products and have numerous other potential applications. These soft solids are usually formed in small quantity by depositing and rolling a drop of liquid on a layer of hydrophobic particles but can also be made in larger quantities in an industrial mixer. In this work, we demonstrate that microscale liquid marbles can also form through self-assembly during water condensation on a superhydrophobic surface covered with a loose layer of hydrophobic nanoparticles. Using in situ environmental scanning electron microscopy and optical microscopy, we study the dynamics of liquid marble formation and evaporation as well as their interaction with condensing water droplets. We demonstrate that the self-assembly of nanoparticle films into three-dimensional liquid marbles is driven by multiple coalescence events between partially covered droplets and is aided by surface flows causing rapid nanoparticle film redistribution. We also show that droplet and liquid marble coalescence can occur due to liquid-to-liquid contact or squeezing of the two objects into each other as a result of compressive forces from surrounding droplets and marbles. Irrelevant of the mechanism, coalescence of marbles and drops can cause their rapid movement across and rolling off the edge of the surface. We also demonstrate that the liquid marbles randomly moving across the surface can be captured and immobilized by hydrophilic surface patterns.

Neutron Powder Diffraction of Carbon-Coated FeCo Alloy Nanoparticles

Neutron powder diffraction is used to study the order–disorder transformation in carbon-coated FexCo1−x nanoparticles produced using a radio frequency plasma torch. The nanoparticles, nominally Fe50Co50, are produced from alloy powder and acetylene precursors by gas-phase nucleation from the plasma. The resulting nanoparticles undergo an order–disorder transformation near 730 °C, passing from an ordered B2 (CsCl) structure to a disordered A1 (body-centered-cubic) structure upon heating, similar to the transformation seen in bulk equiatomic FeCo. Although it is very difficult to quench the disordered state in bulk samples, the extreme cooling rates present in the plasma reactor produce metastable disordered nanoparticles. Neutron powder diffractograms acquired during a heating–cooling cycle at 27, 500, 710, 800, 710, and 400 °C indicate the particles relax to their equilibrium ordered state upon heating first, disorder as they pass through the transformation temperature, and reorder upon cooling.

Directed 2D‐to‐3D Pattern Transfer Method for Controlled Fabrication of Topologically Complex 3D Features in Silicon

A process that allows control over the 3D motion of catalyst nanostructures during metal-assisted chemical etching by their local pinning prior to etching is demonstrated. The pinning material acts as a fulcrum for rotation of the catalyst structures resulting in etching of silicon features with rotational geometry.

Annealing effects on the coercivity of SmCo5 nanoparticles

The enhanced coercivity of ball milled nanoparticles of SmCo5 has been attributed to the reduced particle size, but the milling process introduces additional strain which can also affect the coercivity. Here the effects of size and strain are decoupled from each other using a combination of x-ray diffraction, electron microscopy, and coercivity measurements. Ball milled SmCo5 nanoparticles were annealed under different temperature, time, and atmospheric conditions to minimize the strain without chemically altering the sample, and with minimal grain growth and sintering. X-ray diffraction was used to determine if phase changes had occurred, and to monitor the average grain size and strain. From scanning electron microscopy the log-normal size distributions were found and no evidence of sintering was revealed. The sample coercivities were measured by superconducting quantum interference device following annealing.