A Multifunctional Microfluidic Platform for High‐Throughput Experimentation of Electroorganic Chemistry

Mo, Yiming; Rughoobur, Girish; Nambiar, Anirudh M. K.; Zhang, Kara; Jensen, Klavs F.

doi:10.1002/ange.202009819

Cited by 9 publications

(9 citation statements)

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“…1 . The instrument was custom-built for autonomous operations by the authors of the present article and is essentially an automated liquid handler at the front end (inspired by previous lab automation 26 ), and a flow-through liquid electrolyte characterization tool at the back end. Given a specified electrolyte, Clio will create it by mixing together feeder solutions and measure the ionic conductivity, viscosity, and density of the liquid sample.…”

Section: Resultsmentioning

confidence: 99%

Autonomous optimization of non-aqueous Li-ion battery electrolytes via robotic experimentation and machine learning coupling

et al. 2022

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Developing high-energy and efficient battery technologies is a crucial aspect of advancing the electrification of transportation and aviation. However, battery innovations can take years to deliver. In the case of non-aqueous battery electrolyte solutions, the many design variables in selecting multiple solvents, salts and their relative ratios make electrolyte optimization time-consuming and laborious. To overcome these issues, we propose in this work an experimental design that couples robotics (a custom-built automated experiment named "Clio”) to machine-learning (a Bayesian optimization-based experiment planner named "Dragonfly”). An autonomous optimization of the electrolyte conductivity over a single-salt and ternary solvent design space identifies six fast-charging non-aqueous electrolyte solutions in two work-days and forty-two experiments. This result represents a six-fold time acceleration compared to a random search performed by the same automated experiment. To validate the practical use of these electrolytes, we tested them in a 220 mAh graphite∣∣LiNi0.5Mn0.3Co0.2O2 pouch cell configuration. All the pouch cells containing the robot-developed electrolytes demonstrate improved fast-charging capability against a baseline experiment that uses a non-aqueous electrolyte solution selected a priori from the design space.

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Section: Resultsmentioning

confidence: 99%

Autonomous optimization of non-aqueous Li-ion battery electrolytes via robotic experimentation and machine learning coupling

et al. 2022

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“…Mo et al developed a microfluidic device using interdigitated electrodes (IDEs) providing automated kinetics measurement of electrocatalysts (Figure 2b ). 19 Ingeniously, the authors configured a cyclic voltammetry (CV) flow cell with a 0.75 mm deep pocket in front of the working electrode in order to use the classical CV analytical equation 66 for automated electroanalysis. The measured kinetic constants were compared to those obtained from a traditional cyclic voltammetry cell to ensure validity and repeatability.…”

Section: High-throughput Screening For Electrocatalystsmentioning

confidence: 99%

“…92 93 94 Mo et al microfabricated an interdigitated electrode (IDEs) with interelectrode distance of 10 μm, enabling sub-second molecular diffusion between cathode and anode (Figure 4a ). 95 This intensified mass transfer allowed a high current density even when electrolyzing a 15 μL reagent solution. The implementation of IDEs significantly expedites the screening process of finding the optimal condition for α-amino C–H arylation reactions.…”

Section: Miniaturization Of Screening Devicesmentioning

confidence: 99%

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Accelerated Electrosynthesis Development Enabled by High-Throughput Experimentation

Chen

2023

Synthesis

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Electrochemical synthesis has recently emerged as an environmentally benign method for synthesizing value-added fine chemicals. Its unique reactivity has attracted significant interests of synthetic chemists to develop new redox chemistries. However, compared to conventional chemistry, the increased complexity caused by electrode materials, supporting electrolytes, and setup configurations create obstacles for efficient reaction discovery and optimization. The recent increasing adoption of high-throughput experimentation (HTE) in synthetic chemistry significantly expedites the synthesis development. Considering the potential of implementing HTE in electrosynthesis to tackle the challenges of increased parameter space, this short review aims at providing recent advances in the HTE technology for electrosynthesis, including electrocatalysts screening, device miniaturization, electroanalytical methods, artificial intelligence, and system integration. The discussed contents also cover some topics in HTE electrochemistry for areas other than synthetic chemistry, hoping to spark some inspirations for readers to use interdisciplinary techniques to solve challenges in synthetic electrochemistry.

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“…29,30 Notably, despite significant recent advances, a general, standardized HTE reactor that satisfies these desirable criteria remains elusive. 31 Herein, we report the design of a 24-well plate high-throughput electrosynthesis reactor, namely HTe -Chem, that presents all the aforementioned features and capabilities. By showcasing a selection of electrosynthetic transformations, we demonstrate the versatility of this new reactor for reaction discovery, optimization, and library synthesis in a variety of electrochemical applications.…”

Section: Introductionmentioning

confidence: 99%

Unlocking the Potential of High-Throughput Experimentation for Electrochemistry with a Standardized Microscale Reactor

Rein¹,

Annand²,

Wismer³

et al. 2021

Preprint

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Organic electrochemistry has emerged as an enabling and sustainable technology in modern organic synthesis. Despite the recent renaissance of electrosynthesis, the broad adoption of electrochemistry in the synthetic community and, especially in industrial settings, has been hindered by the dearth of general, standardized platforms for high-throughput experimentation (HTE). Herein, we disclose the design of the HTe-Chem, a high-throughput microscale electrochemical reactor that is compatible with existing HTE infrastructure, and enables rapid evaluation of a broad array of electrochemical reaction parameters. Utilizing the HTe-Chem to accelerate reaction optimization, reaction discovery, and chemical library synthesis is illustrated using a suite of oxidative and reductive transformations under constant current, constant voltage, and electrophotochemical conditions.

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A Multifunctional Microfluidic Platform for High‐Throughput Experimentation of Electroorganic Chemistry

Cited by 9 publications

References 50 publications

Autonomous optimization of non-aqueous Li-ion battery electrolytes via robotic experimentation and machine learning coupling

Autonomous optimization of non-aqueous Li-ion battery electrolytes via robotic experimentation and machine learning coupling

Accelerated Electrosynthesis Development Enabled by High-Throughput Experimentation

Unlocking the Potential of High-Throughput Experimentation for Electrochemistry with a Standardized Microscale Reactor

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