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Harley Quinn

Publications and source records attributed to Harley Quinn.

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PANDA-film: an automated system for electrodeposition of polymer thin films and their wetting analysis

Thin polymer films are widely used as functional and protective coatings. However, determining the composition and processing conditions that produce a desired function is a tedious process due to the large number of factors that must be considered and the manual nature of most synthesis and characterization methods. Self-driving labs (SDLs), or robotic systems that prepare and test materials samples, are designed to overcome this bottleneck by enabling the efficient exploration of complex parameter spaces. In this paper, we report the development and testing of the polymer analysis and discovery array (PANDA)-film, a modular SDL for electrochemically synthesizing polymer films and then determining their water contact angle as a measure of surface energy. The system is designed to be highly modular and based upon a lowcost gantry platform to facilitate adoption. In addition to validating fluid handling and electrochemical tasks, we introduce two novel modular capabilities that enable PANDA-film to run sustained campaigns to study the wetting properties of films: (1) an electromagnetic capping/decapping system to mitigate fluid evaporation, and (2) a top-down optical method to determine water contact angle based upon reflectance. These capabilities are validated by depositing and characterizing a poly(allyl methacrylate) (PAMA) film using electrodeposition of polymer networks (EPoN). Comprehensive details for replicating the hardware and software of PANDA-film are included.

physics.ins-det

PANDA: A self-driving lab for studying electrodeposited polymer films

We introduce the polymer analysis and discovery array (PANDA), an automated system for high-throughput electrodeposition and functional characterization of polymer films. The PANDA is a custom, modular, and low-cost system based on a CNC gantry that we have modified to include a syringe pump, potentiostat, and camera with a telecentric lens. This system can perform fluid handling, electrochemistry, and transmission optical measurements on samples in custom 96-well plates that feature transparent and conducting bottoms. We begin by validating this platform through a series of control fluid handling and electrochemistry experiments to quantify the repeatability, lack of cross-contamination, and accuracy of the system. As a proof-of-concept experimental campaign to study the functional properties of a model polymer film, we optimize the electrochromic switching of electrodeposited poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) films. In particular, we explore the monomer concentration, deposition time, and deposition voltage using an array of experiments selected by Latin hypercube sampling. Subsequently, we run an active learning campaign based upon Bayesian optimization to find the processing conditions that lead to the highest electrochromic switching of PEDOT:PSS. This self-driving lab integrates optical and electrochemical characterization to constitute a novel, automated approach for studying functional polymer films.

physics.app-ph

Screening for electrically conductive defects in thin functional films using electrochemiluminescence

Multifunctional thin films in energy-related devices often must be electrically insulating where a single nanoscale defect can result in complete device-scale failure. Locating and characterizing such defects presents a fundamental problem where high-resolution imaging methods are needed to find defects, but imaging with high spatial resolution limits the field of view and thus the measurement throughput. Here, we present a novel high-throughput method for detecting sub-micron defects in insulating thin films by leveraging the electrochemiluminescence (ECL) of luminol. Through a systematic study of reagent concentrations, buffers, voltage, and excitation time, we identify optimized conditions at which it is possible to detect features with areas ~500 times smaller than the area interrogated by a single pixel of the camera, showing high-throughput detection of sub-micron defects. In particular, we estimate the minimum detectable features to be lines as narrow as 2.5 nm in width and pinholes as small as 35 nm in radius. We further explore this method by using it to characterize a nominally insulating phenol film and find conductive defects that are cross-correlated with high-resolution atomic force microscopy to provide feedback to synthesis. Given the inherent parallelizability and scalability of this assay, it is expected to have a major impact on the automated discovery of multifunctional films.

physics.app-ph