SOFC Electrode Compatibility: Pr4Ni3O10 with Electrolytes

Received: 19 October 2023
Revised: 14 February 2024
Accepted: 19 February 2024
DOI: 10.1002/fuce.202300176
RESEARCH ARTICLE
Chemical compatibility of solid oxide fuel cell air electrode
Pr4Ni3O10±δ with commercial electrolytes
V. E. Tagarelli1
J. Vega-Castillo2,3
1 Centro Atómico Bariloche (CAB),
Comisión Nacional de Energía Atómica
(CNEA), S.C de Bariloche, Argentina
2 Consejo Nacional de Investigaciones
Científicas y Técnicas (CONICET), La
Plata, Argentina
3 YPF- Tecnología (Y-TEC), Berisso,
Argentina
Correspondence
A. Montenegro-Hernández, Centro
Atómico Bariloche (CAB), Comisión
Nacional de Energía Atómica (CNEA), Av
Bustillo 9800 (8500), S.C de Bariloche,
RN, Argentina.
Email: [email protected]
Funding information
Consejo Nacional de Investigaciones
Científicas y Técnicas, Grant/Award
Number: PIP-06795; Agencia Nacional de
Promoción Científica y Tecnológica,
Grant/Award Number: PICT 2019-03721
A. Montenegro-Hernández1,2
Abstract
The chemical reactivity between Pr4 Ni3 O10±δ (3-PNO) electrodes and
Y0.08 Zr0.92 O1.96 (YSZ), Ce0.9 Gd0.1 O1.95 (GDC), and La0.9 Sr0.1 Ga0.8 Mg0.2 O2.85
(LSGM) electrolytes was analyzed by electrochemical impedance spectroscopy
and X-ray diffraction. 3-PNO powders were synthesized by two different chemical routes, one of them uses hexamethylenetetramine (HMTA) as a complexing
agent (route A) while the other citrates (route B). The samples observed by scanning electron microscopy presented different microstructures; route A powders
present small submicronic grains with an open microstructure while route B
powders are formed by larger well-connected grains. The polarization resistance
(RP ) values for 3-PNO/YSZ cells are one order of magnitude higher than those
of 3-PNO/GDC and 3-PNO/LSGM cells. The RP for both cells 3-PNO/GDC
and 3-PNO/LSGM and its evolution in time suggest that chemical reactivity
takes place during the adhesion treatment and electrochemical measurements.
The microstructure plays a crucial role in RP and the degradation rate; 3-PNO
obtained by route A (3-PNO-HMTA) exhibits the best electrochemical performance since these powders present a well-loose morphology and a large exposed
area. However, this fact makes them active chemically, so the increase of RP
with time is slower for 3-PNO electrodes prepared by route B (3-PNO-Cit), since
the rate of chemical reactivity with the electrolyte is slower.
KEYWORDS
chemical compatibility, EIS, electrode, Ruddlesden Popper phase, SOFC cell
1
INTRODUCTION
Fuel cells are devices that convert chemical energy into
electrical energy through an electrochemical reaction.
Unlike batteries, which store energy and run down, in
the fuel cell it is possible to generate electrical energy
continuously as fuel is supplied. In particular, solid oxide
fuel cells (SOFCs) are electrochemical devices made of
solid materials that operate at high temperatures and,
in some cases, can operate in both fuel and electrolytic
modes. They are composed of two electrodes, separated
Fuel Cells. 2024;1–8.
by a dense electrolyte, each element requires materials
with specific characteristics in terms of their transport and
electrocatalytic properties, thermodynamic stability, and
microstructure [1, 2]. In the fuel mode, energy conversion
is driven by the chemical potential difference of oxygen
between the cathode and anode. At the anode, the fuel (H2 ,
CH4 , CO, hydrocarbons, and biofuel) is oxidized while at
the cathode the O2 in the air is reduced to compensate for
the potential difference. The circuit is closed by the passage
of electrons through the interconnectors and the passage
of O−2 ions through the dense electrolyte. In this way, the
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© 2024 Wiley-VCH GmbH.
1
fuel reacts with the oxygen ions resulting in the formation
of H2 O, electrons, and heat. One of the major drawbacks
of SOFCs is their high operating temperature which leads
to some problems, such as chemical degradation, mainly
at the interface between the cell components [3–9].
As mentioned, the oxygen reduction semi-reaction
occurs at the cathode and it is necessary to have a material with well mixed conduction properties (electronic and
ionic), since this contributes to increasing the sites where
the reaction occurs, unlike a purely electronic conductor
in which the electrochemical reactions are restricted to
the triple points in the three-phase boundary [10]. The
processes involved in oxygen reduction depend on temperature, oxygen partial pressure, and electrode characteristics. In this sense, the Ruddlesden Popper phase (RP)
[11–13] with structure Lnn+1 Nin O3n+1 (Ln: La, Pr, Nd) is
one of the most widely studied systems at present due to its
promising electrochemical properties of mixed ionic and
electronic conduction [14]. Its crystal structure consists of
“n” layers of perovskites (LnNiO3 ) alternating with “rock
salt” LnO layers along the c-axis [14]. Numerous investigations on higher order RP phases have been reported, all
of them aimed at improving the electrochemical properties
by modifying compositions and optimizing the microstructure. In this regard, Yatoo et al. have reported the synthesis
of LaPr3 Ni3 O10 and La2 Pr3 Ni3 O10 phases to be used as
cathode in SOFCs [15]. Montenegro Hernandez concludes
in her work that the Pr2 NiO4 (n = 1) phase is not stable
under operating conditions [16] while other authors report
thermal stability for Pr4 Ni3 O10±δ (3-PNO) phase (n = 3) at
979 K [17, 18] and also presents excellent electrochemical
performance with a specific area resistance of 0.25 Ω cm2
at 873 K [19].
Early reports by Zhang et al. of the 3-PNO phase report
an orthorhombic-type structure with Fmmm space group
[20], however, this structure has been refuted by Tsai
et al. who through a neutron diffraction study on the crystal structure conclude that the asymmetric broadening
of the peak located at 46◦ of 2θ and the discordance in
the intensity of the diffraction peak located at 47.5◦ are
due to a lower symmetry in the crystal structure, which
corresponds to a monoclinic- type structure [21].
This work presents a systematic characterization of
the electrochemical performance of 3-PNO electrode
material by electrochemical impedance spectroscopy
(EIS). The thermal stability of this compound and its
chemical compatibility with commercial electrolytes
Y0.08 Zr0.92 O1.96 (YSZ), Ce0.9 Gd0.1 O1.95 (GDC), and
La0.9 Sr0.1 Ga0.8 Mg0.2 O2.85 (LSGM) were evaluated at
different temperatures. To the best of our knowledge, this
study is the first to report the effect of the microstructure
and the chemical reactivity of 3-PNO with YSZ, GDC, and
LSGM materials on the electrochemical performance of
the 3-PNO electrodes.
2
EXPERIMENTAL
2.1
Sample preparation and
characterization
3-PNO samples were synthesized by two different methods: route A uses hexamethylenetetramine (HMTA) as
a complexing agent [22] and route B uses citrates, both
derived from Pechini method. The first one involves a
sol gel formation by polymerization of acetyl acetone and
HMTA [23], while the second one uses citric acid and ethylene glycol as chelating agent and polymeric precursor,
respectively. In the route A stoichiometric amounts of precursor Pr6 O11 and Ni (CH3 COO)2 .H2 O were dissolved in
acetic acid (120 mL) with HMTA and acetyl acetone, in a
molar ratio of 3:1 (ligand: metal) to obtain the sample (2 g).
In the route B, Pr6 O11 and Ni(NO3 )2 hexahydrate were used
as precursors. The oxide was dissolved in 30% v/v nitric
acid solutions and then slowly heated until all the liquid
evaporated. Nickel nitrate was added, and the mixture was
dissolved in distilled water with citric acid and ethylene
glycol. In order to remove the solvent excess and promote
polymerization, the solutions were heated until a dark gel
was obtained. Afterwards both gels were annealed: gel A at
573 K for 2 h and gel B at 673 K for 2 h. Finally, the resulting
powders were ground in an agate mortar and heat treated
at 1323 K for 96 h in O2 .
The phase purity and the structural characterization of
all obtained samples were carried out by X-ray diffraction (XRD) at room temperature. XRD analysis was made
with XRD diffractometer (Panalytical Empyream) with Cu
(Kα1 and Kα2 ) radiations. All XRD patterns of prepared
nickelates were refined using Rietveld method [24] within
Fullprof Package software.
The morphology and particle size of synthesized nickelates were analyzed by scanning electron microscopy
(SEM). The SEM images were obtained from a FEI-Nova
Nano SEM 230 microscope.
2.2
Chemical compatibility
characterization
The chemical reactivity test between 3-PNO sample with
commercial GDC (GDC 10-M Source: Fuel cell materials),
YSZ (TZ-8Y Source: TOSOH Corporation), and LSGM
(LSGM-P Source: Fuel cell materials) powders was performed by mixing 100 mg of nickelate and 100 mg of
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2
F I G U R E 1 (a) Photograph of the top view and schematic of a symmetric cell and (b) scanning electron microscopy (SEM) micrograph of
a cross section of Pr4 Ni3 O10±δ (3-PNO)-Cit deposited on Ce0.9 Gd0.1 O1.95 (GDC) pellet.
TA B L E 1
Pellets dimensions.
Electrolyte
Diameter
(mm)
Thicknesses
(mm)
GDC
18
1.22
YSZ
16
1.23
LSGM
7
1.25
Abbreviations: GDC, Ce0.9 Gd0.1 O1.95 ; LSGM, La0.9 Sr0.1 Ga0.8 Mg0.2 O2.85 ; YSZ,
Y0.08 Zr0.92 O1.96 .
electrolyte powders. The mixture was grinded and
annealed at 973, 1223, and 1273 K for 72 h in atmospheric
air. After each treatment, XRD was performed on the mixture, at room temperature. The phase reaction products
were identified using “Crystallographic Open Database
(COD)” [25–31].
The electrochemical performance over the time
of porous 3-PNO electrodes was achieved by EIS.
This characterization was made using dense YSZ,
GDC, and LSGM electrolytes, on symmetrical
Ag/electrode/electrolyte/electrode/Ag cell configuration (Figure 1(a)); Ag was used as the current collector.
Symmetrical cells were prepared by depositing a porous
layer of 3-PNO on both sides of electrolyte pellets. Dense
electrolytes are obtained by pressing commercial YSZ,
GDC, and LSGM powders and sintering at 1623 K for YSZ
and GDC and at 1723 K for LSGM, for 6 h, getting pellets
with dimensions according to Table 1.
EIS measurements were performed using a frequency
response analyzer coupled to a potentiostat (Autolab
PGSTAT 30). The data acquisition was performed in a frequency range of 1–MHz. An alternating current signal of
5 mV of amplitude was applied to the cell, under zero direct
current polarization.
EIS spectra were recorded in the temperature range
from 773 up to 1073 K using an air flow of 100 mL/min
(composition: 20% O2 /80% N2 ).
In order to monitor the performance of the cells over
time, EIS measurements were also carried out at 973 K as
a function of time, for a while of 216 h.
Electrode powders were dispersed with polyvinyl
butyral, polyvinylpyrrolidone, isopropanol, and α- terphineol. The electrolyte substrates were covered onto
both flat sides with the obtained electrode ink using spin
coating technique. Afterwards, the symmetrical assemblies were heat treated at 1223 K for 1 h in air to promote
electrode/electrolyte adhesion. The average electrode
thickness obtained is approximately 30 µm, as shown in
Figure 1(b).
3
3.1
RESULTS AND DISCUSSION
Crystal structure
XRD data from both types of synthesized 3-PNO confirmed
the presence of the pure phase, as observed in Figure 2(a)
and (b). The diffractograms were refined in the monoclinic
P 21/a space group; the lattice parameters and estimated
crystallite sizes are summarized in Table 2. These values are in agreement with previously reported results,
for example, Vibhu [18] uses an orthorhombic symmetry
to refine laboratory XRD data and obtains similar lattice parameter values. Bassat uses three different synthesis
routes and obtains the same lattice parameter values [19].
Zhang [20] also uses an orthorhombic symmetry obtaining
similar lattice parameters and more recent high resolution
neutron diffraction studies by Tsai et al. [21] suggest that
phase 3-PNO has a lower degree of symmetry.
The goodness of fit parameters of this refinement was
Rwp = 3.11; Rp = 2.18, Rexp = 1.93, and χ2 = 2.59.
Both diffractograms in Figure 2 reveal the same crystal structure although the broadening of the peak widths
suggests a larger size of coherent diffraction domains in
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3
FIGURE 2
refinement.
TA B L E 2
X-ray diffractograms of Pr4 Ni3 O10±δ (3-PNO) powders synthesized by (a) A and (b) B routes together with Rietveld
Lattice parameters and crystallite size of 3-PNO powders.
a (Ǻ)
Sample
b (Ǻ)
c (Ǻ)
β (◦ )
Size (nm)
3-PNO-HMTA
5.3759
5.4647
27.5458
90.3039
87.6
3-PNO-Cit
5.3743
5.4624
27.5431
90.2479
173.7
Abbreviations: 3-PNO, Pr4Ni3O10±δ; HMTA, hexamethylenetetramine.
the 3-PNO-Cit samples. The crystallite size obtained from
the Rietveld refinement of the 3-PNO-HMTA samples is
roughly half that of 3-PNO-Cit samples.
The crystal structure of the RP phases with n = 3, is
described as a tetragonal lattice with I4/mmm symmetry,
in which the oxygens occupy the octahedral vertex sites
with the transition metal (BO6 structure) at the center,
while the rare earth metal occupies the A site. However,
the crystal structure has a lower degree of symmetry, which
results in a distortion of the alignment angle of the NiO6
octahedra. Due to these angular distortions, the Ni–O bond
distances are affected by increasing values in the ab plane,
with larger distances in the octahedra close to the rock salt
layer. The Ni–O bond distances in the c-direction are also
increased; nevertheless, it is noticeable that in the inner
perovskite layers the Ni–O bond distances do not change.
The Pr–O bonds of the rock salt layers are also increased
[21].
3.2
Microstructure
Figure 3(a) and (b) show SEM images of 3-PNO powders
obtained by routes A and B, respectively. The samples
display different morphologies: the 3-PNO-HMTA powders show agglomerates constituted by small submicronic
grains with high porosity and poor connectivity (see
Figure 3(a)), while the 3-PNO-Cit powders present irregular agglomerates with dense surfaces (see Figure 3(b)).
The observed agglomerates in both samples are typical for
compounds obtained by Pechini’s routes.
The particle size of the 3-PNO-HMTA samples is in the
order of 1 µm while the particle size of the 3-PNO-Cit samples is larger than 10 µm, this modifies the active surface
area which is also observed in the area specific resistance
(ASR) values obtained by EIS analysis.
3.3
Thermal stability and chemical
compatibility
3-PNO phase resulted unchanged after being annealed at
973 K in air, for 30 days, as revealed by the XRD patterns
before and after as shown in Figure 4(a).
On the other hand, Figure 4(b) shows the diffractograms
of 3-PNO electrodes after annealed at higher temperatures
in air. The XRD remained the same at temperatures up to
1223 K. However, after annealing at 1273 K for 8 h the phase
decomposes into Pr2 NiO4 (see Figure 4(b)). Similar results
have been obtained by Bassat et al. [19].
The optimal temperature for promoting the adhesion
of 3-PNO onto electrolyte was determined to be 1223 K.
For this reason, the compatibility between 3-PNO electrode
and commercial electrolytes powders was evaluated at this
temperature. Figure 5 shows the XRD patterns of the 3PNO-HMTA and electrolyte powders mixtures after heat
treatment. After 72 h, the diffractogram of 3-PNO/GDC
mixture shows a large decomposition of the 3-PNO phase
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4
FIGURE 3
Scanning electron microscopy (SEM) images of Pr4 Ni3 O10±δ (3-PNO) powders synthetized by (a) A and (b) B routes.
F I G U R E 4 X-ray diffractograms of Pr4 Ni3 O10±δ (3-PNO) powders after different heat treatments. Thermal stability at (a) operating
temperature 973 K and (b) adhesion with electrolyte temperature. (♦) Pr4 Ni3 O10±δ and (∆) Pr2 NiO4 .
and the apparition of higher order RP PrNiO3−δ perovskite
(Figure 5(a)), while for 3-PNO with LSGM mixture, additional peaks are observed at 24.5◦ , 31.9◦ , and 44.4◦ of
2θ corresponding mainly to (La2−x Srx )NiO4−δ ; and the
reflections observed at 44.4◦ and 58.5◦ were attributed to
PrSrGaO4 (see Figure 5(c)). For 3-PNO with YSZ mixture,
the reflections observed at 29◦ and 59.6◦ of 2θ correspond
to Pr2 Zr2 O7 phase (Figure 5(b)).
(La2−x Srx )NiO4−δ and PrNiO3−δ perovskites show a
metal-like behavior over the temperature range studied
[32, 33]. On the other hand, the compound observed as a
product of the reaction between 3-PNO and YSZ is a band
insulator [34], with a band gap of 3.46 eV [35].
3.4
Electrochemical characterization
In Figure 6, the Nyquist plots recorded at 973 K in air
for 3-PNO-HMTA using LSGM, YSZ, and GDC electrolyte
are compared. It can be observed that the polarization
resistance (RP ) is higher for the 3-PNO/YSZ/3-PNO cell.
This fact suggests that the chemical reactivity between 3PNO and YSZ affects more markedly the electrochemical
performance, compared to 3-PNO with GDC and LSGM
electrolytes. This result is in agreement with that observed
by XRD after compatibility tests (see Figure 5). The presence of Pr2 Zr2 O7 , observed as a product of the reaction
between 3-PNO and YSZ, causes resistive losses, due
to its poor electrical transport properties, similar results
have been observed by Montenegro-Hernandez [16, 36]
and Lee and Oh [37]. In the case of the 3-PNO/LSGM,
there are multiple factors that influence the RP behavior [38], so it is not possible to attribute the impairment
observed only to the presence of this phase reaction product. Finally, for 3-PNO/GDC cells, PrNiO3−δ perovskite has
been reported to have a lower performance than 3-PNO
[19] and Pr2 NiO4 [33] phases with RP values up to six times
higher.
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5
treatments.
ASR = 𝑅P 𝐴∕2
(1)
Cells conformed by 3-PNO-Cit showed a linear growth
trend, with a degradation rate (RD ) of 3.35 mΩ cm2 h−1
with LSGM electrolyte and 1.77 mΩ cm2 h−1 with GDC
electrolyte. A break in the linear trend was observed for
the cells conformed by electrodes synthesized by route
A. In 3-PNO-HMTA/LSGM cells this break occurred at
160 h of operations whereas in 3-PNO-HMTA/GDC, it
took place at 50 h of operation. Taking into account
the initial and final values of the ASR, the 3-PNOHMTA/LSGM cell showed a degradation of 81%, the
3-PNO-HMTA/GDC cell showed a degradation of 113%,
the 3-PNO-Cit/LSGM cell showed a degradation of 34%,
and the 3-PNO-Cit/GDC cell showed a degradation of
24%. For electrodes constituted by small particles, the
contact area with the electrolyte is augmented. This
fact indicates that the degradation is faster than electrodes made of powders with larger particle size [16].
Since the size of the particles determines the reaction
zone and also the mechanism controlling the oxygen
electrode reaction. The difference in the RD between
3-PNO-HMTA and 3-PNO-Cit would be due to the difference in the microstructure. Keep in mind that HMTA
powders present a well-loose morphology and a large
exposed area making them very chemically active. To our
knowledge, neither the reactivity of 3-PNO with commercial electrolytes nor the electrochemical response over
time and its relation to the reactions occurring at the
electrode-electrolyte interface has been reported previously.
F I G U R E 5 X-ray diffractograms of (a) Pr4 Ni3 O10±δ (3-PNO)hexamethylenetetramine (HMTA)/Ce0.9 Gd0.1 O1.95 (GDC), (b)
3-PNO-HMTA/Y0.08 Zr0.92 O1.96 (YSZ), and (c)
3-PNO-HMTA/La0.9 Sr0.1 Ga0.8 Mg0.2 O2.85 (LSGM) powder mixtures
after heat treatment at 1223 K in air. (♦) Pr4 Ni3 O10 , (∆) GDC, (*)
YSZ, (y) LSGM, (●) La2−x Srx NiO4−δ , (■) PrSrGaO4 , (▽) Pr2 Zr2 O7 ,
and (r) PrNiO3−δ .
Figure 7 shows the variation of the 3-PNO ASR with
time at 973 K using GDC and LSGM as electrolytes. The
ASR is computed by Equation (1), where RP is the polarization resistance and A is the cathode geometric area [39]. It
can be observed that the ASR of both cells increases with
time, probably due to the formation of reaction products
at the electrode/electrolyte interface [36]. The reactivity
suggested by the increase of ASR, may occur not only due
to the long periods at temperatures of EIS measurement,
but also due to the previous electrode/electrolyte adhesion
4
CONCLUSIONS
3-PNO single phase was obtained by two chemical synthesis routes, SEM images of the obtained samples
showed that the methods yielded powders with different microstructures. Studies of its chemical reactivity
with YSZ, GDC, and LSGM electrolytes by EIS and XRD
showed that 3-PNO reacts with the three electrolyte
materials. This chemical reactivity impacts the electrochemical performance. The greatest degree of chemical reactivity was observed using YSZ as electrolyte
and the ASR value was as high as approximately 30
Ω cm2 at 973 K, one order of magnitude higher than
those of cells with GDC and LSGM electrolytes. On the
other hand, it was observed that the chemical reactivity depends on the microstructure of the 3-PNO; in the
case of powders with a well-loose morphology and a
large exposed area, the increase of RP with time is faster
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6
F I G U R E 6 Comparison of (a) Nyquist and (b) Z" vs frequency plots of cathodes of Pr4 Ni3 O10±δ (3-PNO)-hexamethylenetetramine
(HMTA) measured at T = 973 K using different electrolytes.
AC K N OW L E D G M E N T S
This work was financially supported by Comisión
Nacional de Energía Atómica (CNEA), Consejo Nacional
de Investigaciones Científicas y Técnicas (CONICET PIP
06795), and Agencia Nacional de Promoción de Ciencia y
Tecnología (ANPCyT PICT 2019-03721).
ORCID
A. Montenegro-Hernández
0816-278X
https://orcid.org/0000-0002-
REFERENCES
F I G U R E 7 Area specific resistance (ASR) values as function of
time at 973 K of (a) Pr4 Ni3 O10±δ (3-PNO)/Ce0.9 Gd0.1 O1.95
(GDC)/3-PNO and (b) 3-PNO/La0.9 Sr0.1 Ga0.8 Mg0.2 O2.85
(LSGM)/3-PNO cells indicating the RD .
than the electrodes made with powders with irregular
agglomerates with dense surfaces. Although the electrode obtained by route A exhibits more tendency to
react chemically than those prepared by route B, its ASR
values are lower so, its electrochemical performance is
better.
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How to cite this article: V. E. Tagarelli, J.
Vega-Castillo, A. Montenegro-Hernández, Fuel
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