Accelerated screening of gas di
ff
usion electrodes
for carbon dioxide reduction
†
Ryan J. R. Jones,
Yungchieh Lai, Dan Guevarra, Kevin Kan, Joel A. Haber
and John M. Gregoire
*
The electrochemical conversion of carbon dioxide to chemicals and fuels is expected to be a key
sustainability technology. Electrochemical carbon dioxide reduction technologies are challenged by
several factors, including the limited solubility of carbon dioxide in aqueous electrolyte as well as the
di
ffi
culty in utilizing polymer electrolytes. These considerations have driven system designs to
incorporate gas di
ff
usion electrodes (GDEs) to bring the electrocatalyst in contact with both a gaseous
reactant/product stream as well as a liquid electrolyte. GDE optimization typically results from manual
tuning by select experts. Automated preparation and operation of GDE cells could be a watershed for
the systematic study of, and ultimately the development of a materials acceleration platform (MAP) for,
catalyst discovery and system optimization. Toward this end, we present the automated GDE (AutoGDE)
testing system. Given a catalyst-coated GDE, AutoGDE automates the insertion of the GDE into an
electrochemical cell, the liquid and gas handling, the quanti
fi
cation of gaseous reaction products
via
online mass spectroscopy, and the archiving of the liquid electrolyte for subsequent analysis.
Introduction
The development of gas di
ff
usion electrodes (GDEs) has
enabled electrochemical carbon dioxide reduction to achieve
industrially-relevant current densities while avoiding both
parasitic hydrogen evolution, which is o
en observed when
using proton-conducting polymer electrolytes, and parasitic
sorption of the carbon dioxide, which is o
en observed when
using hydroxide-conducting polymer electrolytes.
1
A GDE
mimics the triple phase boundary of membrane electrode
assemblies (MEAs) used for electrochemical hydrogen technol-
ogies,
2
with the polymer electrolyte replaced by a liquid, o
en
aqueous, electrolyte. While strategies for managing the gas-
liquid-solid boundary of the reactant stream, electrolyte, and
catalyst are less mature than those of MEAs, considerable
progress has been made in GDE systems by employing
a hydrophobic gas di
ff
usion layer (GDL), such as polytetra-
uoroethylene (PTFE), with a metal catalyst coating on the
electrolyte-facing side.
3
The manual assembly and operation of GDEs into electro-
chemical cells present an opportunity to accelerate experimen-
tation
via
automation. Materials acceleration platforms (MAPs)
4
comprise strategies for integrating experiment automation and
data science, which hold great promise for developing
electrocatalysts in general
5
and CO
2
reduction systems in
particular.
6
In the ecosystem of MAPs for electrocatalyst
discovery, a host of techniques have been developed for bulk
liquid electrolytes,
7
–
9
including for CO
2
reduction with analyt-
ical quanti
cation of product distribution.
10
–
14
Driven mostly by
fuel cell technologies, high throughput screening has also been
demonstrated for MEAs.
15,16
Building upon these concepts, high
throughput screening of GDEs for the electroreduction of
dinitrogen was demonstrated with a 16-channel parallel testing
system.
17
In the present work, we demonstrate an instrument that
automates GDE cell assembly and screening in a manner suit-
able for future incorporation in a MAP
via
integration with
robotic synthesis and GDE sample exchange. We are not aware
of comparable hardware for automating the operation of a GDE
electrochemical cell for incorporation into a MAP. The
description of the instrument and its validation using a PTFE-
supported Cu GDE are provided below. The ESI
†
and associ-
ated data repository include pseudo-code for operation, Python
code for incorporation into the HELAO-async
18
instrument
control platform, a fabrication guide, machining instructions
for custom parts, computer drawings, and a bill of materials
with estimated pricing.
Results and discussion
AutoGDE mechanical design
The objectives for the AutoGDE design include automation of
gas and liquid handling, coupling to analytical detection of
Division of Engineering and Applied Science, California Institute of Technology,
Pasadena, CA 91125, USA. E-mail: gregoire@caltech.edu
†
Electronic supplementary information (ESI) available: Chronoamperometry
data as well as the detailed description, pseudocode for operation, and bill of
materials for AutoGDE. See DOI:
https://doi.org/10.1039/d4dd00061g
Cite this:
Digital Discovery
,2024,
3
,
1144
Received 28th February 2024
Accepted 27th April 2024
DOI: 10.1039/d4dd00061g
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reaction products, and simplifying the exchange of working
electrodes to enable future automation of sample loading and
unloading. This last aspect required the greatest departure from
traditional GDE experimentation, which relies on manual
assembly of fasteners and gaskets to maintain hermetic seals
during operation. While modern and future robotics may rival
the dexterity of human GDE assemblers, we aimed to simplify
the mechanical insertion of a GDE sample into the electro-
chemical cell as well as the establishment of an operational gas-
electrolyte-catalyst boundary. Toward this end, we commenced
with a cell design composed of 3 custom
xtures corresponding
to the core components of a GDE electrochemical cell: the
counter electrode (CE), working electrode (WE), and gas
handling (GH)
xtures.
Each
xture is machine from polyether ether ketone (PEEK)
and contains liquid or gas handling ports. The bill of materials
for building the AutoGDE system, not including analytical
detection of reaction products, is summarized in Table S1.
†
The
CE and WE
xtures contain electrical contacts for interfacing to
the power supply or potentiostat. The CE and WE
xtures are
separated using a polymer membrane, which is Selemion
anion-exchange membrane in the present work.
A cross-section drawing of an assembly of these
xtures is
shown in Fig. 1. Atop the mounting platform, which is
mechanically coupled to the lab bench
via
rigid framing, the GH
xture is a
ffi
xed and is intended to remain stationary. The CE
xture on top can be retracted
via
a spring-loaded translation
stage and motor. When in the
“
engaged
”
position, the spring-
loaded stage and motor enable controlled application of
ca.
200 N of downward force to maintain the o-ring seals between
the CE
xture and membrane, the membrane and WE
xture,
and the WE and GH
xtures. With the CE
xture in the
“
dis-
engaged
”
positions, the WE
xture is removable along with the
GDE sample, which is held in place with a friction
t of the GDL
paper with a regular octagon pro
le whose
ca.
8 mm outer
diameter is
ca.
5% larger than the bored hole in the WE
xture.
Upon engaging the CE
xture to establish a sealed cell, the
nal mechanical preparation of the cell involves compression of
the GDL interface piston to a force of
ca.
100 N using a linear
actuator (Firgelli Automation). This piston resides within the
GH
xture, where a gasket creates an air-tight seal around its
perimeter while providing
exibility in its vertical position so
that in the
“
engaged
”
(raised) position, the piston presses the
catalyst layer atop the GDE against the working electrode
contact ring. This positioning also establishes a gas
ow path
from the perimeter of the piston, laterally through the GDL, to
the center bore of the piston. A photograph of the AutoGDE
system and the
xtures in engaged and disengaged states are
shown in Fig. 2.
AutoGDE incorporation in autonomous work
ows
We pause the description of the AutoGDE instrument to high-
light the future action items for incorporation of the instrument
in a fully-automated MAP: (1) the preparation of the GDE
sample, which involves pro
ling of the GDL to the appropriate
size and application of a catalyst on one side of the GDL; (2) the
insertion of the GDL in the WE
xture, or one of several
Fig. 1
The AutoGDE electrochemical cell. The cross-section view shows the cell's three custom PEEK
fi
xtures (shaded yellow) atop the
mounting platform. The ports in each
fi
xture are labelled by their purpose and/or ancillary pump and valve components to which they are
connected. The GDL interface piston and gas handling
fi
xture (bottom) manage the delivery of gas to the catalyst and to subsequent analytical
characterization of reaction products. The working electrode
fi
xture (middle) manages the electrical contact to the catalyst as well as the working
electrolyte. Separated by a membrane, the counter electrode
fi
xture (top) features a porous counter electrode and recirculating electrolyte.
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duplicate WE
xtures; (3) the placement of the WE
xture atop
the GH
xture; (4) the connection of tubing to the 2 liquid
handling ports on the WE
xture; and (5) the connection of the
potentiostat to the wire that is attached to the working electrode
contact ring, which is embedded within the WE
xture. We
assert that automation of these steps is achievable with stan-
dard lab automation practices and focus the present work on
the description of AutoGDE operation that is agnostic to how
the WE
xture that was positioned and connected. To be clear,
these steps were performed manually to generate the data of the
present work.
AutoGDE liquid and gas handling
As shown in Fig. 1, the CE
xture contains a central inlet port for
electrolyte, which passes through a porous stainless-steel frit,
which serves as the counter electrode. The electrolyte is
returned to its reservoir
via
a peristaltic recirculation pump
attached to four symmetric
“
electrolyte out
”
ports. The
at
lower surface of the porous counter electrode provides
mechanical stability for the membrane. The counter electrode,
electrolyte, and membrane are intended to be used for testing
any number of GDE electrodes.
The GH
xture contains a single gas inlet port for
owing gas
around the perimeter of the piston, through the GDL, and into
the central exhaust port, which interfaces to analytical detection
of gaseous reaction products. The present work employs
a quadrupole mass spectrometer (MS, Hiden HPR20) for quasi-
real-time product analysis.
The GH
xture also plays a pivotal role in the preparation of
the WE electrolyte, which commences by closing the gas inlet
port and applying a
ca.
100 Torr vacuum on the center port of
the GDL interface piston, which also evacuates the WE
xture
through the porous GDE. By closing the electrolyte pumping
port of the WE
xture and connecting the electrolyte manifold
pump to an electrolyte reservoir open to atmosphere, the
vacuum within the WE
xture pulls electrolyte into the
xture
and against the GDE. While any trapped gas between the elec-
trolyte and GDE is readily evacuated, the electrolyte does not
ow through the GDE due to the hydrophobicity of the GDL.
This initial wetting of the GDE automates one of the trickiest
parts of traditional GDE cell preparation. We note that the
tubing for the electrolyte manifold port approaches but not
touches the membrane. The proximity helps ensure that no
bubbles get caught on the membrane surface, which could
cause an open circuit condition, and the small displacement
and angled cut of the tube ending helps ensure that the
membrane does not seal the tube end upon commencement of
the vacuum-
ll procedure.
The
nal preparation of the cell for electrochemical testing
involves connecting the WE electrolyte manifold port to waste
and pumping electrolyte into the WE
xture through the elec-
trolyte pumping port, which removes the air gap in the tubing
and
ushes electrolyte through the WE chamber, ensuring
electrolyte contact to the membrane. A reference electrode, in
this case Ag/AgCl (Innovative Instrument Inc. LF-2-24, 2 mm
diameter, 24 mm barrel leak-free reference electrode), can be
inserted
via
a tee adjacent to the electrolyte pumping port, in
which case this electrolyte
ow step contacts the reference
electrode to the working electrode chamber near the working
electrode surface. With the electrolyte management complete,
the reactant gas
ow commences, which in the present work is 3
sccm of CO
2
, followed by electrochemical experimentation. The
electrolyte used in the present work is aqueous 1 M potassium
bicarbonate.
Given the
ca.
2 mL of internal volume of tubing between the
GDL and the inlet port to the mass spectrometer, the 3 sccm
ow rate corresponds to a
ca.
40 s delay between the formation
of gaseous products at the working electrode and their detec-
tion in the mass spectrometer. This delay time is measured as
the di
ff
erence between the start of a CA measurement and the
rst detection of products in the MS and is used to shi
the MS
time axis to better match that of the electrochemistry data.
To enable o
ff
-line quanti
cation of reaction products dis-
solved in the WE electrolyte, the electrolyte can be archived
upon completion of the electrochemistry. By connecting the
electrolyte manifold port to the desired vial, air (or another gas)
is pumped into the electrolyte pumping port to push practically
all electrolyte from the WE
xture, including its attached
tubing, to the vial. In the present work,
ca.
15 sccm of air
via
a peristaltic pump provides near complete removal of the elec-
trolyte from the WE
xture. The volume of electrolyte within the
tubing, which remains from the electrolyte
lling procedure, is
comparable to the volume of the WE chamber, which results in
dilution of the reaction products by approximately a factor of 2.
When using analytical methods with excellent levels of detec-
tion, for example liquid-injection gas chromatography (GC) and
high-performance liquid chromatography (HPLC) in the
present work (Thermo Trace 1310 and Ultimate 3000), the
dilution is inconsequential. The total amount of liquid product
Fig. 2
The AutoGDE electrochemical cell and mounting hardware.
The realized version of the electrochemical cell in Fig. 1 is shown with
its mounting platform, as well as the linear actuators for engaging the
GDL interface piston (bottom) and compressing the counter electrode
fi
xture to the stack of cell components (top).
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in the vial is the lower limit of that synthesized during the
electrochemical experiment due to possible loss of product, for
example
via
incomplete electrolyte extraction from the cell,
product evaporation during electrochemistry or during elec-
trolyte extraction, and product crossover through the
membrane.
To rinse the cell and/or load fresh electrolyte for further
electrochemical interrogation of the GDE sample, the electro-
lyte manifold port is connected to waste and
ca.
2.1 mL of
electrolyte is pumped through the electrolyte pumping port,
which
ushes the WE
xture. When interrogation of the loaded
sample is completed, the above air-pumping procedure is per-
formed to extract all remaining liquid from the working elec-
trode
xture, e
ff
ectively preparing the working electrode
chamber for exchange with a new GDE sample.
To facilitate quantitative analysis of the MS data, a calibra-
tion experiment can also be performed by switching the gas
stream to a calibration gas with known concentrations of
products of interest. In the present work, the calibration gas is
1% C
2
H
4
,5%H
2
, and 5% CH
4
with balance CO
2
and is diluted
by CO
2
to obtained di
ff
erent levels of concentrations.
AutoGDE demonstration and validation
To prepare nominally duplicate electrodes, two GDE samples
were extracted from a PTFE GDL sheet (0.45
m
m Aspire Lami-
nated membrane from lot# 685459, Sterlitech corporation)
coated with
ca.
300 nm of evaporated Cu. Each GDE was oper-
ated using a sequence of cyclic voltammetry (CV) and chro-
noamperometry (CA) experiments, with the CVs assessing the
time-resolved product analysis and the CAs used for product
quanti
cation and evaluation of reproducibility between
comparable experiments with the nominally duplicate
electrodes.
CVs acquired with 3 voltage cycles at 50 mV s
−
1
and 20 mV
s
−
1
scan rates from
−
0.33 to
−
1.33 V
vs.
RHE (without resistance
compensation) are shown in Fig. 3. The working electrode
current density is calculated on a geometric area basis corre-
sponding to the 0.155 cm
2
aperture of the WE
xture. The MS
signal (pressure) for H
2
,CH
4
, and C
2
H
4
are shown in subse-
quent panels, along with the ratio of the MS signal from CO
2
to
the total for C-containing gases, which approximates the
pressure-based, single-pass conversion e
ffi
ciency of the CO
2
to
hydrocarbon products. While CO is a known prominent reac-
tion product, its MS quanti
cation is hampered by overlap with
aCO
2
fragment, and the liquid products are not quanti
ed for
the CV experiments. We note that additional calibrations are
required to fully interpret the MS signal from a time-varying
product stream.
13
To quantitatively validate the AutoGDE for CO
2
reduction on
a Cu GDE, a series of CA experiments were performed, each with
a fresh working electrode electrolyte, which was archived for
subsequent liquid product analysis. The time series data for the
CA experiments is shown in Fig. S1.
†
The time integral over each
10 min CA experiment was used to quantify the total electro-
chemical charge and partial current densities for each quanti-
ed product, as shown in Fig. 4 and Table S2,
†
which shows the
approximately reproduced values for the electrochemical and
partial current densities at 3 CA potentials. We note that in
some experiments at applied bias below
−
1.33 V
vs.
RHE, the CA
experiment appears unstable, which we attribute to degradation
of the GDE
via
extended operation at current densities in excess
of 50 mA cm
−
2
.
Although CO
2
RR performance on GDE could vary among
electrochemical cell designs due to variation in, for example,
mass transport and current distribution,
19
our AutoGDE
produces CO
2
RR product distributions commensurate with
traditional Cu-based GDEs. To quantitatively compare faradaic
Fig. 3
Cyclic voltammograms and associated gaseous products for a Cu GDE operated in the AutoGDE system with online mass spectroscopy.
The 3 voltage cycles are show with 2 di
ff
erent scan rates. The gaseous products are shown as the MS partial pressure for mass-to-atomic number
(
m
/
z
) values of 2, 15, and 26 for H
2
,CH
4
, and C
2
H
4
, respectively. The CO
2
signal (
m
/
z
=
22) is normalized by the sum of partial pressures for C-
containing products.
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e
ffi
ciencies (FE), we consider the results acquired near
−
1.1 V
vs.
RHE, a potential commonly used to evaluate Cu catalyst in
bicarbonate electrolytes due to the prevalence of C
2+
products
over H
2
. Our results of 48% FE toward C
2+
products and 14% for
H
2
are commensurate with the literature values of 40% and
15%, respectively (see Table S2
†
).
20
Regarding the acceleration in experiment throughput, the
time spent acquiring electrochemical data can be considered to
be independent of the level of experiment automation. Auto-
mation shortens the time spent on other experiment steps, with
ancillary bene
ts including increased reproducibility and
robust data tracking. For the AutoGDE demonstration reported
herein, there are 2 primary experiment preparation steps. The
rst step is the assembly of the electrochemical reactor with
a new GDE sample, which for a traditional GDE experiment
comparable to those presented herein takes 15
–
25 min due to
the multi-step manual cell assembly. The equivalent time on the
AutoGDE is less than 1 min, providing an approximate 20-fold
acceleration. Second, electrolyte handling involves cell cleaning
and (re)
lling electrolyte, which occurs prior each electro-
chemical experiment for which independent liquid product
characterization is desired, as well as archiving of the electro-
lytes for subsequent liquid product detection. These liquid
handling tasks require at least 10 minutes of human researcher
time with traditional methods, while AutoGDE reduces the time
to 3 min and does not require human intervention to manage
the electrolyte (or to subsequently start an electrochemical
experiment). The overall increase of experiment throughput
must be ascertained for a given electrochemical testing protocol
and the availability of human researchers for conducting
multiple experiments. More detailed comparison between
conventional- and Auto-GDE can be found at the ESI.
†
AutoGDE safety and build validation
In addition to standard chemical and electrical safety practices,
the speci
c safety concerns include a mechanical pinch hazard
due to the motorized pressurization of the cell components, as
well as a tubing rupture hazard if the inlet gas pressure is not
limited and gas
ow becomes obstructed. As with all GDE
experiments, the catalyst may su
ff
er from delamination from
the GDL, resulting in a potential exposure to unsupported
nanomaterials.
The assembly instructions provided in the instrument
design repository are intended to produce a fully functional
AutoGDE system, assuming manual insertion of the GDE into
the WE
xture and incorporation of that
xture into the system.
The diagnostic port noted in Fig. 1 can be attached to a pressure
gauge to leak-check the system. The calibration gas can be used
to validate the product detection. Upon these checks, the elec-
trochemical operation of the cell, for example
via
reproduction
of the data in Fig. 4 or S1,
†
is the ultimate validation of the
AutoGDE build.
The most common anticipated issue is an open circuit
condition. Diagnostic steps for identifying the cause of the open
circuit include checking the electrical contact between the
catalyst and the WE contact ring, which can be done with the
WE
xture removed from the cell, or by removing the CE
xture
and membrane to enable line of site access to the catalyst
surface so that it can be electrically contacted to check
connectivity with the WE contact wire. The cause of an
electrolyte-based open circuit conditions can be harder to
identify. One strategy is to test the electrolyte
ll of each
chamber. For the WE chamber, replace the CE
xture and
membrane with a transparent plate so that the presence of
bubbles on the top of the cell can be visually observed. Similarly,
operating the CE
xture with a transparent plate can be used to
con
rm electrolyte penetration through the porous counter
electrode to the plate.
The AutoGDE build has been replicated at Caltech, and given
that the design is being shared with the community
via
this
manuscript, we are not aware of any other replication at the
time of manuscript preparation. The computer drawings and
machining instructions are provided under an open hardware
license to facilitate such replication.
Conclusions
We present the AutoGDE instrument, which automates the
preparation and operation of a gas di
ff
usion electrode sample,
demonstrated herein for electroreduction of CO
2
with a poly-
crystalline copper catalyst supported on a PTFE GDL. While
Fig. 4
Chronoamperometry results for a sequence of 10 min exper-
iments with the same GDE sample and fresh electrolyte. The time
series data in Fig. S1
†
is averaged to provide the total and current partial
densities for the electrochemistry and gaseous products (quanti
fi
ed
using the same MS channels as Fig. 3). The liquid products are analyzed
with o
ff
-line GC and HPLC characterization of the electrolyte from
each CA measurement. A second GDE sample was measured on
adi
ff
erent day at 3 of the CA potentials, showing reproduction of the
potential-dependent product distribution.
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automation of sample handling has been well demonstrated in
the
eld, the automation of liquid and gas handling in gas
di
ff
usion electrochemical cells, as well as integration with
analytical detection of reaction products, is uniquely enabled by
AutoGDE. We present this open hardware design to enable
future development of MAPs for GDE-based electrochemical
devices.
Data and code availability
The instrument control so
ware is available at
https://
github.com/High-Throughput-Experimentation/helao-async
,
with dependencies in
https://github.com/High-Throughput-
Experimentation/helao-core
. These repositories contain the
MIT License. The hardware design for AutoGDE is comprised
of drawings and machining instructions, assembly
instructions, pseudo-code for instrument operation, python
code for the HELAO sequence for collection of demonstration
data, data
les acquired for the present work, and the source
code for the analysis and plotting of those data, which are
provided under the CERN Open Hardware License, CERN-
OHL-P,
via
CaltechData at
https://data.caltech.edu/records/
f40n8-cv274
(doi:
https://doi.org/10.22002/f40n8-cv274
).
Author contributions
R. J. J. and J. M. G. designed AutoGDE with input from all co-
authors. R. J. J. and Y. L. assembled AutoGDE. D. G., K. K.,
and Y. L. developed the instrument control so
ware. Y. L.
procured and analyzed the demonstration data. J. M. G. was the
primary author of the manuscript with contributions from all
authors. R. J. R and Y. L. were the primary authors of the
assembly and operation instructions. J. A. H. and J. M. G.
supervised the project.
Con
fl
icts of interest
J. M. G. is an industrial consultant for experiment automation.
Acknowledgements
This material is based on work performed by the Liquid
Sunlight Alliance, which is supported by the U.S. Department of
Energy, O
ffi
ce of Science, O
ffi
ce of Basic Energy Sciences, Fuels
from Sunlight Hub under Award Number DE-SC0021266. The
Resnick Sustainability Institute at Caltech is acknowledged for
its support of enabling infrastructure and facilities. The authors
thank Aidan Fenwick, Gavin Heim, and Theodor Agapie for
helpful discussion, and Aidan Fenwick for deposition of the Cu
on the GDE.
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