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A0711
CO2 con e sion o syn he ic uels using non-CRM
ca alys s
M. Fazio*, S. C. Zignani, M. Pascale, V. Chiodo, S. Maisano, N. Mondello,
A. Ca bone, A. A icò
Ins i u e o Ad anced Ene gy Technologies (ITAE) o he I alian Na ional Resea ch Council
(CNR);
*Con ac co esponding au ho s: www.EFCF.com/Con ac Reques
Abs ac
To da e CO2 inc easing emissions in o he a mosphe e ep esen a signi ican en i onmen al
h ea ha needs o be hal ed. Elec ochemical educ ion o CO2 (CO2RR) is deemed o be
one o he mos p omising echniques o con e CO2 and wa e in o g een uels, hus
educing CO2 emissions and s o ing enewable ene gy. Pas s udies ha e shown ha he
ange o p oduc s ha can be ob ained om CO2RR a e highly dependen on he
elec oca alys employed. Among he mos commonly used elec oca alys s o
elec ochemical CO2 educ ion in alkaline condi ions he e is coppe , which
elec ochemically con e s CO2 in o mo e han 30 p oduc s, including hyd oca bons and
alcohols [1], howe e , Cu-based elec odes p esen poo selec i i y owa ds he o ma ion
o speci ic p oduc s. Ne e heless, a highe e iciency o he ca alys owa d CO2RR can be
ob ained by p ope enginee ing he ca aly ic su ace in o de o ha e a su icien numbe o
ac i e si es. Expe imen al da a demons a ed ha a mix u e o Cu-based s uc u es wi h
oxidizing s a es going om 0 o 2 can be ob ained o he ca hode h ough he oxala ed
me hod whils a NiFeOx based ca alys was p epa ed o he anode acco ding o he co-
p ecipi a ion p ocedu e. A memb ane elec ode assembly (MEA) was de eloped by cold
p essing anode, ca hode and a comme cial anion exchange memb ane as a polyme ic solid
elec oly e. Elec odes we e p epa ed by sp ay coa ing deposi ion o a ca aly ic inks,
p epa ed by sonica ing a ce ain amoun o he syn he ized powde in e hanol, on a sui able
suppo espec i ely a Sig ace GDL o he ca hode and Bekae Ni el o he anode.
Elec ochemical expe imen s we e ca ied ou wi h a comple e ze o-gap cell ope a ing unde
alkaline condi ions a a 300 mA cm2 cu en densi y. Da a om gas-ch oma og aphic (GC)
analyses o liquid and gaseous e luen s om he ca hode ou le s eam we e ound o be in
line wi h esul s ea u ed in he li e a u e ega ding he p omo ion o in e media es ha may
lead o seconda y eac ions wi h p oduc ion o gases such as H2, CO, C2H4 alongside o
ca bonaceous uels like E -OH and P -OH.
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In oduc ion
One o he mos p essing challenges o he mode n ime is he ansi ion o a sus ainable
and en i onmen ally- iendly economy. In he ansi ion pe iod owa ds enewable ene gies,
deca boniza ion by CO2 ecycling h ough ca bon neu al p ocesses can be conside ed a
signi ican pa h o pu sue [2]. As he inc ease o he ca bon dioxide (CO2) le els is
conside ed o be one o he main con ibu o s o global clima e change, scien i ic and
indus ial esea ch has been ocusing on he de elopmen o new sus ainable echnologies
ha can e icien ly educe CO2 emissions by con e ing hem in o aluable p oduc s.
Elec ochemical educ ion o CO2 (CO2RR) could ep esen a po en ial solu ion o he
en i onmen al p oblem by using enewable elec ici y o con e he excess o CO2 in o e-
uels and aluable chemicals: by employing elec ical ene gy, in ac , i is possible o con e
CO2 in o smalle compounds including ca bon monoxide (CO), o mic acid (HCOOH),
me hane (CH4), e hylene (C2H4), and alcohols. E icien ca alys design ep esen s a
undamen al s ep o achie e signi ican esul s wi h his echnology: p ope ly s uc u ed
ca alys s, based on CRM- ee ma e ials, can, as a ma e o ac , p omo e he desi ed
eac ions wi h high selec i i y, s abili y, and cos -e ec i eness as hei con igu a ion is
di ec ly ela ed o hei elec ochemical p ope ies [3-5]. By employing a sui able ca alys , i
is possible o educe he ac i a ion ene gy o hese eac ions, hus con eying chemical
ans o ma ions owa d a ge p oduc s as well as inc easing he o e all e iciency o he
p ocess. Among he mos commonly used elec oca alys s o CO2RR in alkaline condi ions,
coppe -based elec oca alys s ep esen he mos p omising ma e ial o CO2RR as coppe
can elec ochemically con e s CO2 in o mo e han 30 p oduc s, including hyd oca bons and
alcohols [1], howe e , a he same ime, hey show poo selec i i y owa ds he o ma ion o
speci ic p oduc s. This may ep esen a majo d awback o he de elopmen o ad anced
and selec i e ma e ials; howe e , i p o es ha a highe e iciency o he ca alys owa d
CO2RR could be ob ained by p ope enginee ing he ca aly ic su ace in o de o ha e a
su icien numbe o ac i e si es [6].
This s udy ocuses on he ad anced cha ac e iza ion o a ious ca alys s designed o
op imize CO2 con e sion ia elec oly ic p ocesses. Mul iple expe imen al echniques we e
employed o assess he physical and chemical p ope ies o he de eloped elec oca alys s
in o de o de e mine he majo ac o s ha in luence hei pe o mance. Mo eo e , he
elec ochemical pe o mance o he de eloped ca alys s in CO2 educ ion was ho oughly
in es iga ed by he means o pola iza ion cu es, impedance spec oscopy, and
ch onoampe ome y expe imen s wi h he pu pose o e alua ing hei eac i i y and
elec ical s abili y. Resul s om elec ochemical s udies a e u ilized o unde s and he cha ge
ans e e iciency, as well as he dynamics o CO2 molecule adso p ion and deso p ion a
he ca alys ’s ac i e si es.
1. Scien i ic App oach
1. Elec oca alys de elopmen
Non-CRM elec oca alys s o bo h ca hode and anode e olu ion eac ions ha e been
de eloped and assessed in o de o be employed in CO2RR. In pa icula , he in es iga ed
ca alys s a e, espec i ely, he NiFe-Laye ed Double Hyd oxide (LDH) o he anode and a
Cu-based ca alys ha has been designed o he ca hode. The de eloped ma e ials a e
p ope ly enginee ed o be ope a ed a high cu en densi ies wi h low o e po en ials, hus
displaying a high ac i e su ace a ea and minimal deg ada ion a es. A cos -e ec i e and
e icien co-p ecipi a ion me hod is employed as he main syn he ic ou e in o de o ob ain
ca alys powde s wi h he desi ed cha ac e is ics [7]. Bo h ex-si u and in-si u
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cha ac e iza ions o he de eloped ma e ials a e ca ied ou in o de o e alua e he ca alys
p ope ies and include he de e mina ion o c ys alli e size and ac i e phase dispe sion and
he ca alys s’ e iciency and s abili y unde wo king condi ions. The in-si u pe o mance
assessmen s a e conduc ed in he p esence o an AEM (Anion Exchange Memb ane)
ionome and elec oly e in a ze o-gap cell elec olyse .
1.1 Oxygen e olu ion elec oca alys
NiFe oxide-hyd oxide (LDH) based anode ca alys was syn hesized wi h he pu pose o
imp o ing he ca aly ic ac i i y and s abili y in alkaline en i onmen o oxygen e olu ion
eac ion. The bime allic ca alys e ec i ely con ibu es o s abilize eac ion in e media es
and imp o e he o e all eac ion kine ics. The unique laye ed s uc u e o LDHs supplies a
la ge su ace a ea and abundan ac i e si es, which a e essen ial o OER, and p omo e he
inse ion and mobiliza ion o hyd oxide ions, assis ing he elec oca aly ic p ocess.
1.2 CO2 e olu ion elec oca alys
Coppe -based non-noble me al oxides a e conside ed p omising elec oca alys s o he
elec ochemical educ ion o CO2, a g eenhouse gas, o hei capabili y o con e ing i in o
mo e han 30 p oduc s ha include aluable hyd oca bons and alcohols, he eby
con ibu ing o ca bon ecycling and he de elopmen o sus ainable ene gy sou ces.
Coppe (Cu) compounds a e especially e ec i e o he CO2 educ ion p ocess o hei
abili y o s abilize eac ion in e media es. Mo eo e , he o ma ion o se e al coppe
oxida ion s a es (Cu0, Cu1+, Cu2+) pe mi s di e en eac ion ou es wi h he de elopmen o
a ious p oduc s o in e es such as me hane (CH4), e hylene (C2H4), and e hanol (C2H5OH)
[8]. As a esul s, di e en syn hesis pa hways o design coppe -based oxides wi h di e en
mo phologies and composi ions (e.g., coppe oxide (CuO) and cup ous oxide (Cu2O)) ha e
been unde in es iga ion in o de o ob ain ad anced elec oca alys powde s o CO2RR
wi h sui able ca aly ic p ope ies, such as su ace a ea, po osi y, and ion conduc ion and
enhance he ca alys ’s CO2 educ ion e iciency.
Coppe -based oxide ca alys s’ pe o mances can be in luenced by nume ous ac o s such
as elec oly e composi ion, eac ion condi ions (e.g., pH, empe a u e) along wi h hei
physical p ope ies, he e o e, in o de o achie e high ac i i y and selec i i y in CO2
con e sion, an op imiza ion o hese elemen s is necessa y.
2. Expe imen s
2.1. Syn hesis o OER ca alys
Nickel Ni a e Hexahyd a e (Ni(NO3)2∙6H2O, Sigma Ald ich) and I on Ni a e Nonahyd a e
(Fe(NO3)3∙9H2O, Sigma Ald ich) we e dissol ed in ul apu e dis illed wa e , hen he solu ion
was placed in a hea ed wa e ba h, whe e i was s i ed a 60 °C. When he solu ion eaches
he desi ed empe a u e, a 2 M solu ion o sodium hyd oxide (NaOH) solu ion is added
d opwise un il pH 9 is achie ed. The suspension is hen main ained a pH 9 and 60 °C and
hen s i ed o 3 hou s. A e wa ds, he o med p ecipi a e is il e ed and washed wi h ho
ul apu e dis illed wa e (app ox. 40 °C) and, las ly, d ied a 80 °C in an o en o 24 hou s.
2.1.1 Physical- chemical cha ac e iza ions
The physicochemical p ope ies o he syn hesized elec oca alys we e ho oughly
in es iga ed by se e al cha ac e iza ion echniques including XRD and XRF. Fo he X- ay
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di ac ion (XRD) in es iga ion was used a D8 Ad ance di ac ome e (B uke AXS,
Ge many), ope a ing wi h a Ni b- il e ed Cu-Kα adia ion (λ = 1.5406 Å) in he 2θ ange 5–
100° a 40 kV and 20 mA and a scan s ep o 0.03° s−1. XRD echnique was used o analyze
he c ys alline phase o he NiFe anode ca alys de eloped. Fig. 1 shows he egis e ed XRD
pa e ns in which h ee di e en s uc u es ela ed, espec i ely, o Ni(OH)2∙0.75H2O ,
Ni(OH)2 and FeO(OH). Bo h b oad and hinne peaks a e obse ed in he pa e ns and a e
ela ed o a mix u e o ine and la ge c ys alli e sizes o he pa icles. Th ough he Sche e
o mula, i was possible o calcula e an a e age c ys alli e size o 45.7 Å (4.57 nm).
Fig.1 XRD pa e ns o he NiFe (LDH) anodic ca alys .
X- ay luo escence analysis (XRF) was ca ied ou using an S8 TIGER spec ome e (B uke
AXS, Ge many) o e alua e he ca alys elemen al composi ion. The ins umen , equipped
wi h a hodium anode ube (powe 4 kW and 75 µm Be window and LiF 220 c ys al analyze),
allowed o ob ain semi-quan i a i e esul s o he a omic a io o Ni:Fe oxide-hyd oxide. The
composi ion o he syn hesized ca alys was shown in Table 1.
Table 1. A omic composi ion o anodic NiFe (LDH) elec oca alys as assessed by XRF
analyses.
2.2. Syn hesis o HER ca alys
Coppe -based elec oca alys s ha a e usually employed on he ca hode side o he CO2
educ ion a e syn he ized by co-p ecipi a ion me hod. P ecu so s o he ma e ials a e
dissol ed in dis illed H2O, hen he solu ion is placed in o a Te lon beake ins alled in a bain-
ma ie a 60 °C. A 1 M solu ion o sodium hyd oxide (NaOH) is added d opwise o achie e
pH 9, a e wa ds he dispe sion is s i ed o 4 hou s in o de o acili a e he p ecipi a ion o
he compound ha is, hen il e ed and washed wi h ho wa e . Finally, he ca alys is d ied
in an o en a 80 °C, ea ed in a ball milling sys em a 160 pm o 17 hou s and subsequen ly
sie ed.
% a
Ni
Fe
NiFe
85.4
14.6
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2.2.1 Physical- chemical cha ac e iza ions
XRD analysis epo ed in Fig. 2 shows he di ac ion peaks o he syn hesised Cu-based
ca alys . A pa icle size o 8 nm was egis e ed.
Fig. 2 XRD pa e ns o he CuO-based ca hodic unsuppo ed ca alys .
2.3 Memb ane elec ode assembly (MEA) de elopmen and elec ochemical s udy
The ca aly ic inks we e p epa ed by dissol ing he ca alys powde (67 w .%) in e hanol and
mixing a Fuma ech ionome (33 w .%). The dispe sion is, hen, sonica ed o 30 min. A slu y
o he anode ink was deposi ed using a sp ay coa ing echnique, espec i ely, on a Nickel
Fel backing laye (Bekae ) wi h a o al me al loading o 2.5 mg cm-2 o he anode.
Cold-assembly p ocedu e was adop ed o p epa e he memb ane-elec ode assemblies
(MEAs) wi h 5 cm2 ac i e a ea o ca alys sc eening and du abili y s udies. Be o e he
assembling, i is necessa y o exchange bo h elec odes and memb ane o 24 hou s wi h
hyd oxide ions con aining solu ion in o de o ac i a e all he componen s. The MEAs we e
assembled in a single-cell housings made o nickel pla es cha ac e ized by a se pen ine low
ield channel. Te lon® gaske s we e used o seal he cell and a oid any leakage o he
elec oly e solu ion. Cell comp ession was 2.5 N m pe each ie od. Du ing all expe imen s,
he anode side was ed wi h 1 M KOH solu ion eci cula ed a a low a e o 1 ml min-1 cm-2
using a pe is al ic pump.
The MEAs we e elec ochemically cha ac e ized o de e mine he pe o mance o he
de eloped elec oca alys s. The elec ochemical in es iga ions, conce ning gal anos a ic
pola iza ion cu es (cell po en ial as a unc ion o cu en densi y) and gal anos a ic
du abili y es s (cell ol age e sus ime), we e ca ied ou wi h a Kei hley powe supply
sys em (Tek onic). Elec ochemical impedance spec oscopy (EIS) analysis was ca ied ou
wi h a PGSTAT Au olab 302 Po en ios a /Gal anos a equipped wi h a cu en boos e
(Me ohm) and a F equency Response Analyze (FRA). The impedance measu emen s
we e pe o med a h ee di e en cell ol ages (1.5 V, 1.8 V, 2 V), in a equency ange
be ween 100 MHz - 10 mHz [7].
2.3.1 Elec ochemical cha ac e iza ion o he anode ca alys
A slu y o he anode ca alys s dispe sed in e hanol was deposi ed on nickel el s supplied
by Bekae wi h a o al oxide loading o 2.5 mg cm-2. The P /C ca hode has been p epa ed
wi h a o al me al loading o 1 mg cm-2. A Fuma ech FAA3-50 anion exchange memb ane in
he OH- o m was used as sepa a o be ween anode and ca hode compa men s.
Memb ane-elec ode assemblies (MEAs), wi h 5 cm2 geome ical a ea, we e p epa ed by a
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cold-assembly p ocedu e. KOH 1M solu ion was supplied by a pe is al ic pump o he anode
compa men , a a low a e o 4 mL min.
The o e po en ial o he Ni-Fe oxide anode wi h espec o he he moneu al po en ial o
oxygen e olu ion eac ion (1.48 V) was hus de e mined om single cell expe imen s using
a benchma k P /C ca hode acco ding o he o mula:
ηNiFe− anode = ECell − ηP − ca hode − IR − E h
whe e ηNiFe-anode is he anodic o e po en ial e sus he he moneu al po en ial o he NiFe
oxide anode, Ecell is he o e all cell po en ial, ηP -ca hode is he o e po en ial o he P /C
benchma k ca hode, IR is he ohmic d op wi h R de e mined om he se ies cell esis ance
and E h is he he moneu al po en ial. The o e po en ials o he ca hodic ca alys s we e
de e mined by employing he same Ni-Fe oxide as be o e h ough he o mula:
ηca hode =ECell− IR− E h − ηNiFe− anode
in which ηca hode is he o e po en ial o he CRM ee ca hode ca alys .
3. Resul s
3.1 Elec ochemical cha ac e iza ion o he anode ca alys
NiFeOx anode elec oca alys was p epa ed a CNR-ITAE and es ed in single cell, using
P /C as ca hode and Fuma ech as elec oly e. This cell was ed wi h 1 M KOH o he anode
side. Fig. 3 compa es he pola isa ion cu e and he IR- ee cu e o he NiFe as anode-
based cell in es iga ed a 50 °C. A 1.7 V s. RHE (IR- ee), he mass ac i i y and he cu en
densi y a e, espec i ely, 140 A/g and 350 mA/cm2.
Fig. 3 Pola isa ion cu es o MEAs based on P /C as ca hode, a Fuma ech memb ane and
NiFeOx as anode o anode ma e ial cha ac e iza ion.
Fig. 4 displays EIS analyses ca ied ou a di e en po en ials (1.5V – 1.8V – 2 V). The MEA
ha moun ed NiFe LDH a he anode and P /C a he ca hode showed low se ies and
pola iza ion esis ances (Rs-in e cep a high equency wi h he x-axis), a phenomena ha
is mo e e iden in he EIS analysis eco ded a 1.8V and 2V.
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Fig. 4 EIS o he MEA based on P /C as ca hode -Fuma ech memb ane and NiFeOx as
anode o anode ma e ial cha ac e iza ion.
3.2 Elec ochemical cha ac e iza ion o he ca hode ca alys
Elec ochemical cha ac e iza ion o he ca hode ma e ial was also ca ied ou h ough
pola iza ion cu es and impedance spec oscopy analysis by de eloping a MEA
(memb ane-elec ode assembly) ha moun ed NiFe a he anode side on a Ni el po ous
anspo laye (Bekae ) and CuxO a he ca hode side coa ed on Sig ace gas di usion
laye . The o al ca alys loading was 2.5 mg cm-2 o he anode and 1 mg cm-2 o he ca hode.
Humidi ied CO2 was ed o he ca hode compa men a 65 °C, wi h a low a e o 40 mL pe
minu e.
In e ms o elec ochemical pe o mance, he co-elec olysis cell achie es 3 V/cell a 0.25 A
cm-2 and 2.6 V/cell a 1 A cm-2 in he pola iza ion cu e ca ied ou a he end o he es (Fig.
5a). A gal anos a ic es was ca ied ou by applying a 300 mA cm-2 cu en densi y o 2
hou s o e alua e cell pe o mance (Fig. 5b) and he mean cell ol age in du abili y es was
jus below 2.5 V/[email protected] A cm-2.
Figs 5c-d show he EIS analysis ca ied ou a he beginning and a he end o he s abili y
es . The se ies esis ances (Rs) and pola iza ion esis ances (Rp) a he end o he du abili y
es esul s lowe compa ed o Rs and Rp in EIS BoT (Fig. 5c). In e ms o Fa adaic e iciency,
he co-elec olysis cell achie es abou 15% o gaseous ca bonaceous p oduc s and 0.45%
o liquid ca bonaceous p oduc s. The sum o ca bonaceous p oduc s is less han 20% and
he o al ca bonaceous p oduc s and hyd ogen is 100%.
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Fig. 5 a) pola iza ion cu es (BoT) (EoT), b) du abili y es 300 mA cm-2 a 50 °C o 2 hou s,
c) EIS in es iga ions a 1.5V, 1.8V, 2V BoT; d) EIS in es iga ions a 1.5V, 1.8V, 2V EoT; e)
and ) Fa adaic e iciency o gaseous ca bonaceous, and liquid ca bonaceous p oduc s.
3.3 Conclusion
In anion exchange memb ane (AEM) elec olysis echnologies, he employmen o NiFe as
an anode ca alys p esen s se e al ad an ages in e ms o e iciency and long- e m s abili y.
The high elec oca aly ic ac i i y o NiFe in addi ion o an op imal u iliza ion o ac i e si es
de i ed by he syne gism be ween nickel and i on acili a es he oxygen e olu ion eac ion
(OER) by imp o ing ion anspo and minimizing ene gy losses, hus, enhancing he o e all
elec olysis p ocess. Fu he mo e, as a consequence o he ma e ial’s mechanical s eng h
and esis ance o co osion, NiFe can be employed o ex ended ope a ion in AEM
elec olysis sys em. Ca hodic CuO-based elec oca alys s showed signi ican po en ial o
he elec ochemical educ ion o CO2, as hey can selec i ely con e CO2 on he ca alys ’s
su ace, in o sui able e- uels and chemicals. Selec i i y owa ds a ge hyd oca bons and
compounds can be u he imp o ed by p ope enginee ing he ma e ial’s s uc u e,
composi ion, and mo phology, he e o e, enhancing he o e all con e sion e iciency.
By combining NiFe o OER and CuO o CO2RR, i is possible o imp o e he ene gy
e iciency and sus ainabili y o AEM-based elec ochemical sys ems, inc ease he
pe o mances wi h espec o eac ion selec i i y and sys em s abili y and o e a p ac ical
ou e o ansi ing o a low-ca bon economy as i di ec ly add esses ca bon u iliza ion and
mi iga ion. Fu u e esea ch e o s should ocus on u he op imizing ca alys design,
explo ing eal-wo ld ope a ing condi ions, and scaling up hese echnologies. De eloping
hese imp o emen s will be c ucial in enabling comme cial deploymen and maximizing he
en i onmen al bene i s o hese inno a i e elec ochemical p ocesses.
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Acknowledgemen s
The au ho s acknowledge he inancial suppo p o ided by EU H2020 GREEN DEAL
“ECO2FUEL” p ojec “La ge-scale low- empe a u e elec ochemical CO2 con e sion o
sus ainable liquid uels” G an Ag eemen numbe : 101037389.
Re e ences
[1] S.C. Zignani, M. Lo Fa o, A. Ca bone, A. Palella, L. Spada o, A.S. A icò, Alkaline
elec olysis using CuOx ca hode o he con e sion o ca bon dioxide in o liquid uels,
Ma e ials o Renewable and Sus ainable Ene gy 12 (2023) 141–146.
[2] J.H. Wesseling, S. Lech enböhme , M. Åhman, L.J. Nilsson, E. Wo ell, L. Coenen,
The ansi ion o ene gy in ensi e p ocessing indus ies owa ds deep deca boniza ion:
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Keywo ds: EFCF2025, H2, LowTemp. Fuel Cells & Elec olyse s, CO2 con e sion, Ze o-gap
elec ochemical cell, Syn he ic uels. CRM- ee ca alys
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