Best practices for automated electrochemistry (tool and workflow design)

Tools
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  1. What existing solutions/examples have you implemented or heard about?
  2. How is the movement of the (usually working) electrode in and out of the electrolyte handled?
  3. How are automated electrical disconnects and re-connects handled, if at all?
  4. How do you approach liquid handling for hazardous materials (e.g., KOH) which can also be at high temperatures? (e.g., materials used, safety / robustness / cost)

cc @nisfisker, @nipun.0092, @yangbai

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Here are some references you might find interesting:

Parallel Reaction System: https://pubs.acs.org/doi/10.1021/acsmeasuresciau.3c00022
Homemade System (similar to our OT setup): DOI: 10.1016/j.device.2023.100103
John Gregoire’s Work on HT Electrocatalysis Measurement: This paper includes a system capable of collecting gas products, which the above two systems lack. https://pubs.acs.org/doi/full/10.1021/acsenergylett.1c02762

The ability to handle hazardous materials depends on the materials used to construct the reactor. Most reactors should be capable of this, especially those made with PEEK. However, high-temperature reactions are more challenging, as they often require reactors made from stable, heat-conductive metals like titanium. This can introduce risks such as metal contamination in the reaction and metals are usually electrical conductive. So, we typically use PEEK, although it is unsuitable for high-temperature reactions. Recently, Kelvin and I have been discussing materials that are non-Econductive, thermally conductive, and chemically resistant for reactor construction—Kelvin might have some ideas on this.

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I’ve been working with Matthias Gramlich and Bojan Micevski on a 3D printed electrochemical cell for fuel cell catalyst tests. Most of the development history including discussion, images, videos, and links to CAD files are available in the following issues:

I’ll get something more condensed soon, and full docs will move to GitHub - AccelerationConsortium/echem-cell: A custom, 3D printed electrochemical cell for autonomous electrochemistry, targeted at fuel cell electrolysis studies. (as of 2025-04-04 currently just placeholders).

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You can see the cell in operation at the back of this picture:

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  1. My exposure to existing solutions for HT electrocatalysis and screening is down to redox.me and IKA. Whilst their solutions are quite decent, I feel that they’re a bit too dear for many labs that might want to experiment with electrochemistry, and this domain isn’t their strength. Investing significant sums (up to US$2k in some instances!) might be a bit much if one’s not sure if the process will work for them!
  2. The electrodes, in the form of plates, are manually inserted into the electrolyte chamber after the chamber has been filled with the required volume of electrolyte. The process is currently not automated, which is one of the reasons our research team implemented the CNC-based liquid dispenser that can work with organic solvents, allowing for the dispensing of organic electrolytes.
  3. I’m not aware of any automated solutions for handling the connection and disconnection of electrodes to the potentiostat cables. I’d be keen on any idea that helps us smooth this process!
  4. The considerations and allowances we must make for handling organic solvents are paramount; all components that may come into contact with the electrolyte should be resistant to the solvent in question. For electrosynthesis, if we were to avoid the dark road of fluoropolymers (reducing our dependency on fluoropolymers is a key goal of our lab, so I’m not inclined to pursue the path of fluoropolymers), we must keep solvent compatibility in mind whilst preparing our components. I would absolutely test the solvent compatibility myself before committing, as I learnt this the hard way!
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