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High performance ceria-bismuth bilayer electrolyte

Cite this: DOI: 10.1039/x0xx00000x
low temperature solid oxide fuel cells (LT-SOFCs)
fabricated by combining co-pressing with drop-coating
Published on 24 March 2015. Downloaded by Rice University on 14/04/2015 02:04:41.

Received 00th December 2014, Jie Hou,a Lei Bi, b,* Jing Qian, a Zhiwen Zhu, c Junyu Zhang a and Wei Liua,d,*
Accepted 00th January 2014

DOI: 10.1039/x0xx00000x

www.rsc.org/

The Sm0.075Nd0.075Ce0.85O2-δ-Er0.4Bi1.6O3 bilayer structure film, and a doped ceria (DCO) layer on the reducing side to improve the
which showed an encouraging performance in LT-SOFCs, thermodynamic stability of the bismuth oxide layer, by shielding it
from very low PO .Several studies have demonstrated that the
was successfully fabricated by a simple low cost technique 2

combining one-step co-pressing with drop-coating. electrochemical properties of ceria-based SOFCs can be effectively
improved using the ceria/bismuth oxide bilayer electrolyte
The major challenge for solid oxide fuel cells (SOFCs) structure.1-3, 5-7, 10, 17-20 Though various fabrication methods were
commercialization is to lower its operating temperature to low employed for ceria-bismuth bilayer electrolyte cells, such as spin
temperatures (LTs, ≤650 °C) while still maintaining a desirable cell coating, DC (Direct Current) magnetron sputtering, pulsed laser
performance. The LT operation (450-650 °C) can potentially provide deposition (PLD) and so on,2, 3, 6, 17, 18 most of which required
a better stability and lower costs due to reduced thermal and advanced small-scale techniques and the operating temperature was
chemical stresses and an increased range of material choices, as well relative high above 550 °C. Therefore, the low cost fabrication of
as reduced energy consumption and faster start-up times for portable SBO electrolyte film fuel cells with reasonable performance at LT
applications.1-3 Highly conductive electrolyte materials play one of down to 450 °C still remains a challenge. Furthermore, limited
the most important roles in lowering the operating temperature.4 compatible cathodes for the ceria-bismuth bilayer electrolyte cells
Isovalent cation stabilized bismuth oxides (SBO) are particularly were developed, though Ahn et al18 exploited the cathode
attractive because of their superior ionic conductivity at LTs, which Er0.4Bi1.6O3-Bi2Ru2O7 (ESB-BRO7) for GDC|ESB bilayer
is about 1-2 orders of magnitude higher than those of zirconia-based electrolyte and achieved very high electrochemical performance,
electrolytes.1, 5-8 However, bismuth-based materials could which contains the noble metallic element Ru. Then seeking new
decompose to metallic bismuth in the presence of the reducing gas low cost cathode materials for ceria-bismuth bilayer electrolyte is
such as H2 or CH4.9 Therefore, they could not be used at the fuel side imperative.
which makes it a poor choice by itself as an electrolyte for SOFCs. Here a simple low cost fabrication technique combining one-step co-
In contrast, the bismuth-based materials can be exposed to the air pressing with drop-coating was developed for the anode-DCO-SBO
side since it is intended to be a pure oxide ionic conductor and bilayer electrolyte half cells. The ESB and Sm0.075Nd0.075Ce0.85O2-δ
thermodynamically stable under oxygen partial pressure down to 10- (SNDC)21, 22 were chosen as the SBO and DCO electrolyte,
13
atm.2, 6, 10, 11 To date, many works were focused on the ceria-based respectively. Hence, encouraging electrochemical performances at
electrolytes to lower the operating temperature.4, 12-14 Virkar et al15, 16 LTs with a novel composite cathode ESB-La0.74Bi0.1Sr0.16MnO3-δ
have pioneeringly proposed a two-layer fuel cell electrolyte structure (ESB-LBSM) were achieved and produced the maximum power
with YSZ used as a blocking layer to prevent ceria reduction, density (MPD) output of 130 mW cm-2 at 450 °C that is the largest
whereafter Wachsman et al7 developed the ceria/bismuth oxide power output for this type of SOFCs.
bilayer electrolyte consisting of an SBO layer on the oxidizing side Figure 1 shows the XRD patterns of SNDC, ESB, LBSM and the
dry-mixed composite powder ESB-LBSM fired at 700, 650, 850 and
a
CAS Key Laboratory of Materials for Energy Conversion & Collaborative 750 °C for 3h, respectively. Indexing of these patterns clearly
Innovation Center of Suzhou Nano Science and Technology, University of Science
reveals that ESB possesses the same cubic symmetry of space group
and Technology of China, Hefei 230026, PR China
b
Physical Sciences and Engineering Division, King Abdullah University of Science Pm-3m with SNDC which has the pure phase with cubic fluorite
and Technology (KAUST), Thuwal 23955-6900, Saudi Arabia structure. It also suggests that no obvious reactions occurred between
c
Institute of Urban Environment, Chinese Academy of Sciences, Xiamen 361021, the fluorite structure ESB and the perovskite structure LBSM after
PR China heat treatment at 750 °C and this temperature is applied for the
d
Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese
Academy of Sciences, Hefei 230031, PR China
composite cathode firing in this study.
Email: [email protected](W. Liu); [email protected](L. Bi) Seen from Figure 2.(a), the SNDC electrolyte is totally dense and the
Fax: +86 551 63602586; Tel: +86 551 63600941 grain size ranges from around 1 to 2 µm which has the ability to

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10.1039/C4TA06864E

block ESB electrolyte layer from the exposure to the reducing obtained at the very low sintering temperature 800 °C. The ESB
atmosphere. As SNDC is a good ionic conductor electrolyte electrolyte layer is also sufficiently dense to block the electronic flux
material, the dense film is beneficial for blocking the gas and from SNDC in reducing atmospheres. Figure 2.(c) shows the
allowing the transport of oxygen ions. It can also be clearly observed morphology of the interface between ESB and SNDC electrolyte of

Journal of Materials Chemistry A Accepted Manuscript

from Figure 2.(b) that dense ESB electrolyte by drop-coating was the tested cell. Though the cell has suffered a heating and subsequent
cooling process during testing, the ESB electrolyte layer still bonds
to the SNDC membrane tightly. This firm adhesion confirms that the
SNDC film shows a good thermal matching with the ESB electrolyte
that is consistent with Wachsman’s conclusion,6, 7, 10 which is an
important consideration in the design of the DCO-SBO bilayer
electrolyte for high performance low temperature SOFCs (HPLT-
SOFCs). Shown in Figure 2.(d) is the cross-sectional view of the
four-layer single cell, both anode and cathode well adheres on both
side of the SNDC-ESB bilayer structure without any sign of
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cracking or delamination. Apart from blocking gas leakage during

operation, the high-quality SNDC|ESB bilayer electrolyte film
definitely ensures fast oxygen ions transport through the electrolyte
and thereby decrease internal resistance of the single cell.
Interestingly, SNDC could prevent the reduction of ESB by the
reducing gas while ESB could hold back electronic current from
SNDC in reducing atmospheres, which state clearly that the two
electrolyte films could protect each other. Notably, the well-designed
configuration is quite in favor of mass and charge transfer in the cell
and thus the cell is expected to attain good electrochemical
Figure 1. XRD patterns of SNDC, ESB, LBSM and the dry-mixed composite performance.
powder ESB-LBSM fired at 700, 650, 850 and 750 °C for 3h, respectively.

Figure 2. Cross-section SEM images of (a) SNDC and (b) ESB electrolyte layer, the interface between ESB and SNDC electrolyte layer, and (d) the single cell
with bilayer electrolyte SNDC|ESB after testing.

In order to evaluate SNDC|ESB bilayer film for HPLT-SOFCs, including 10GDC|5ESB (0.78 V at 650 °C),6 10GDC|4ESB (0.77 V
button cells using NiO-SNDC as anode and SNDC|ESB bilayer film at 650 °C)18 and SDC|YSB (0.887 V at 500 °C)17. Moreover, the
as electrolyte with ESB-LBSM cathode was fabricated and measured current relsuts show higher MPDs than many ceria-bismuth bilayer
under conventional conditions (humidified hydrogen as the fuel gas; electrolytes reports, such as SDC|YSB (571 mW cm-2 at 600 °C),17
static air as the oxidant). The typical I-V and power density curves SDC|YSB (381 mW cm-2 at 650 °C),2 GDC|ESB (588 mW cm-2 at
for the single cell NiO-SNDC|SNDC|ESB|ESB-LBSM at 450-650 650 °C),3 GDC|ESB (667 mW cm-2 at 600 °C)23. Some studies show
°C is shown in Figure 3. The open-circuit voltages (OCVs) after higher OCV values with lower MPDs, while some display higher
anode reduction are 0.80, 0.855, 0.902, 0.943 and 0.97V, MPDs accompanied with lower OCVs. Considering the relatively
corresponding to the MPDs are 980, 788, 515, 292 and 130 mW cm-2 low cost and facile fabrication technique used, the electrochemical
at 650, 600, 550, 500 and 450 °C, respectively. The OCV values are performance in this work has its particular advantages. Although
higher than most of the previously reported similar single cells, Ahn et al18 reported it that the GDC|ESB bilayer electrolyte cell

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DOI: 10.1039/C4TA06864E

achieved the MPD of 1.95 W cm-2 at 650 °C, it has no low Typical electrochemical impedance spectra (EIS) at 450-650 °C with
temperature performance down to 450 °C given, and many other SNDC|ESB bilayer electrolyte cell was measured under open-circuit
works report the cell performance at similar conditions.1, 3, 6 conditions to provide an insight understanding of how SNDC|ESB
Noticeably, the SNDC|ESB bilayer structure cell in this assignment bilayer film and ESB-LBSM cathode work, as shown in Figure 4.(a).

Journal of Materials Chemistry A Accepted Manuscript

has the largest power output below 550 °C compared with the In the EIS plots, the high-frequency intercept corresponds to the
performance of anode-supported cells with ceria-bismuth bilayer ohmic resistance (Ro) of the cell which is mainly contributed by the
electrolytes reported in literature as summarized in Table 1, such as electrolyte resistance, and the difference between the high frequency
GDC|ESB (88 mW cm-2 at 450 °C),23 SDC|YSB (223 mW cm-2 at and the low frequency intercept with the real axis represents the
500 °C)17 and SDC|YSB (153 mW cm-2 at 550 °C)2. So the cell in interfacial polarization resistance (Rp) of the cell. Figure 4.(b) shows
this study has made a significant progress for LT operation in the values of Ro, Rp and the total resistances Rt (Rt= Ro+Rp) of the
SOFCs down to 450 °C. bilayer film cell estimated from the impedance spectra. The
SNDC|ESB bilayer electrolyte cell has low Ro values of 0.139, 0.169
0.225 0.326 0.506 Ω cm2 and the Rp of 0.038, 0.081, 0.216, 0.754
and 2.494 Ω cm2 at 650, 600, 550, 500 and 450 °C, respectively. It is
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clear that the corresponding electrochemical reactions are thermally

activated processes for all resistances decrease with increasing
temperature. The Rp of the cell decrease from 2.494 to 0.038 Ω cm2
with increasing temperature from 450 to 650 °C, while the Ro only
decreases from 0.506 to 0.139 Ω cm2 under the same conditions.
Meanwhile, the ratio of Rp/Rt are 21.35%, 32.50%, 49.00%, 69.83%
and 83.14% at 650, 600, 550, 500 and 450 °C, respectively.
Obviously, at temperatures higher than 550 °C, Ro dominates the
total resistance, indicating it should be more important to decrease
Ro to further improve the cell performance. Noticeably, the cell Rp
governs the downward trend of Rt and plays a major role in
determining the Rt of the cell below 500 °C. Therefore, at lower
temperatures, more attention should be paid to decrease the Rp. Then
the major issues of developing HPLT-SOFCs are to develop
Figure 3. I-V and I-P curves of the single cell NiO-SNDC|SNDC|ESB|ESB- electrolytes with sufficiently high ionic conductivity to reduce the Ro
LBSM measured at 450-650°C. and to explore electrodes with high activity to decrease the Rp, and

Table 1. Comparison of the fuel cell performance of anode-supported cells using DCO-SBO bilayer electrolyte films reported in the literature and in the
present study.

Year[reference] DCO thickness and fabrication SBO thickness and fabrication Cathode MPD(mW cm-2)

700 650 600 550 500 450

200620 GDC(84µm) YSBa)(16µm) Pt 260 - - - - -
co-pressing screen-printing
200918 GDC(10µm) ESB(4µm) ESB-BRO - 1.95×103 - - - -
spray-coating PLD
20103 GDC(50µm) ESB(20µm) ESB-BRO - 588 - - - -
co-pressing screen-printing
GDC(20µm) ESB ESB-BRO - 614 - - - -
spray-coating drop-coating
GDC(10µm) ESB ESB-BRO - 1.45×103 - - - -
spray-coating PLD
20102 SDC(26µm) YSB(6µm) YSB-La0.85Sr0.15MnO3-δ - 381 266 153 - -
co-pressing DC magnetron sputtering
201117 SDC(26µm) YSB(6µm) YSB-Ag - - 571 380 223 -
co-pressing DC magnetron sputtering
20126 GDC(10µm) ESB(5µm) ESB-BRO - 1.47×103 - - - -
spin-coating drop-coating
201223 GDC(24µm) ESB(2µm) ESB-La0.8Sr0.2MnO3-δ - 1013 667 343 185 88
spin-coating spin-coating
This work SNDC(20µm) ESB(20µm) ESB-LBSM - 980 788 515 292 130
co-pressing drop-coating
a)
Y0.25Bi0.75O1.5 (YSB)

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10.1039/C4TA06864E

Figure 4. (a) EIS of the single cell NiO-SNDC|SNDC|ESB|ESB-LBSM

measured under open-circuit conditions from 450 to 650 °C, (b) the
temperature dependence of the ohmic resistance (Ro), polarization resistance
(Rp) and total resistance (Rt), as well as the ratio Rp/Rt of the single cell with

Journal of Materials Chemistry A Accepted Manuscript

SNDC|ESB bilayer electrolyte, (c) the Arrhenius plots for Ro and Rp
estimated from the EIS, and (d) comparison of conductivity of various solid
electrolytes in Arrhenius plots. (SNDC, ESB1, 5 and SNDC|ESB bilayer
electrolyte under fuel cell conditions in this work which is maily decided by
the cell ohmic contribution)

thus to enhance the cell performance, which ultimately realizes LT

operations for SOFCs. Furthermore, as shown in Figure 4.(c), the
activation energy (Ea) of the Ro and Rp are 0.27 and 1.06 eV when
the temperature is higher than 600 °C, whereas the Ea are 0.4 and
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1.25 eV below 600 °C, respectively. From the Ea of Ro, we can see
that SNDC|ESB bilayer electrolyte has easier oxygen ions transport
compared with monolayer electrolyte SNDC and even ESB which
have higher Ea (0.74 eV for SNDC, and 1.12 eV and 0.83 eV when
below and exceed 600 °C shown in Figure 4.(d)1, 5). Simultaneously,
the Ea for ESB-LBSM cathode is close to ESB-La0.8Sr0.2MnO3-δ
which is 1.23 eV based ESB electrolyte reported by Lee et al.23 For
most of the bismuth oxides stabilized with lanthanide dopants (Dy,
Ho, Er, Tm, and Yb), the conductivity activation energy (Ea)
increases below 600 °C due to an order-disorder transition of the
oxygen sublattice.5, 23 As Ro is dominated by the electrolyte
resistance, the conductivity of the SNDC|ESB bilayer electrolyte
film under fuel cell conditions can be estimated based on the Ro
values and film thickness ( σ = L / ( Ro × S ) , where σ is conductivity,
L is the film thickness and S is effective area). The ionic
conductivity values of SNDC|ESB bilayer film were 0.14, 0.116,
0.087, 0.06 and 0.039 S cm-1 at 650, 600, 550, 500 and 450 °C,
respectively. Figure 4.(d) shows the comparison of conductivity of
various solid electrolytes in Arrhenius plots. Interestingly,
SNDC|ESB bilayer electrolyte reveals higher ionic conductivity than
ESB below 550°C, which indicates that the DCO-SBO bilayer film
is superior to the single ESB electrolyte at LT operation. It is worth
to be mentioned that the ionic conductivity values of SNDC and
ESB are all tested in the air, in which two oxygen ions may require
to get across the energy barrier to form one oxygen molecule to
ensure the oxygen transport. However, for the SNDC|ESB in the
single cell working conditions in this work, the H2 could react with
O2- easily which will promote the overall oxygen reduction reactions
that may lead to the oxygen transport and consumption. So the
conductivity values obtained here is higher even than ESB obtained
in the air below 550 °C is possible. Therefore, the DCO-SBO bilayer
structure is an optimal combination.

Conclusions

In summary, a simple low cost fabrication technique was developed

for anode-supported DCO-SBO bilayer configuration and a novel
low cost composite cathode material ESB-LBSM was successfully
applied for ceria-bismuth oxide bilayer electrolyte cell. The
SNDC|ESB bilayer structure film showed the largest fuel cell
performance ever reported for ceria-bismuth bilayer electrolytes at
LT operation below 550 °C, to the best of our knowledge, suggesting
that the facile fabrication technique provided an effective and
interesting way to fabricate DCO-SBO bilayer electrolyte films with
encouraging performance at LTs and could be beneficial to the
application of SBO materials for HPLT-SOFCs.

Experimental Section

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DOI: 10.1039/C4TA06864E

SNDC, ESB and LBSM powders were synthesized via a citric and Rp of the cells under open circuit conditions were
acid-nitrate gel combustion process.24, 25 The raw materials for determined from the impedance spectra.
synthesis of SNDC powders were Sm2O3 (99.9%, 3N,

Journal of Materials Chemistry A Accepted Manuscript

Sinopharm Chemical Reagent Co., Ltd (SCR)), Nd2O3 (99.9%, Acknowledgements
3N, SCR) and Ce(NO3)3•6H2O (AR, ≥99.0%, SCR). Er2O3
This work was supported by Ministry of Science and
(99.9%, 3N, SCR), Bi(NO3)3•5H2O (AR, ≥ 99.0%, SCR) and
Technology of China (Grant No: 2012CB215403). The project
La2O3 (99.9%, 3N, SCR), Bi(NO3)3•5H2O, Sr(NO3)2 (AR,
was also supported by the National Science Foundations of
≥99.5%, SCR), MnCO3 (CP, 44.0-48.0%Mn, SCR) served as
China (Grant No: 51408582).
the raw materials for ESB and LBSM powders, respectively.
After the combustion, the as-prepared ash-like powders were
Notes and references
calcined at 700, 650 and 850 °C for 3 h in air to obtain SNDC, 1. E. D. Wachsman and K. T. Lee, Science, 2011, 334, 935-939.
ESB and LBSM powders, respectively. 2. L. Zhang, C. Xia, F. Zhao and F. Chen, Mater. Res. Bull., 2010, 45,
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The NiO-SNDC composite powders with a weight ratio of 6:4 603-608.

3. J. S. Ahn, M. A. Camaratta, D. Pergolesi, K. T. Lee, H. Yoon, B. W.
for the anode substrates were mixed NiO with SNDC powders Lee, D. W. Jung, E. Traversa and E. D. Wachsman, J. Electrochem.
and 20 wt.% starch was added as the pore former. The anode Soc, 2010, 157, B376.
supported half cell with monolayer SNDC electrolyte was 4. W. Sun, Z. Shi, J. Qian, Z. Wang and W. Liu, Nano Energy, 2014, 8,
fabricated by a co-pressing method26 and then co-fired at 1400 305-311.
5. K. T. Lee, H. S. Yoon and E. D. Wachsman, J. Mater. Res., 2012, 27,
°C for 5 h to obtain NiO-SNDC|SNDC half cell. The thickness 2063-2078.
of the monolayer SNDC film was controlled by varying the 6. K. T. Lee, D. W. Jung, M. A. Camaratta, H. S. Yoon, J. S. Ahn and E.
amounts of the powders used. The ESB electrolyte film was D. Wachsman, J. Power Sources, 2012, 205, 122-128.
7. E. D. Wachsman, Jayaweera, N. Jiang, D. M. Lowe and a. B. G.
fabricated by a drop-coating process on SNDC substrate Pounds, J. Electrochem. Soc., 1997, 144, 233.
followed by co-firing at 800 °C for 10 h in air.27, 28 The ESB 8. K. Z. Fung, H. D. Baek and A. V. Virkar, Solid State Ionics, 1992, 52,
powders were firstly dispersed in ethanol with polyvinyl butyral 199-211.
9. H. Kruidhof, K. J. D. Vries and A. J. Burggraaf, Solid State Ionics,
(PVB, binder, 4%) and triethanolamine (TEA, dispersant, 6%), 1990, 37, 213-215.
and were then ball milled for 24 h to obtain the ESB electrolyte 10. J.-Y. Park, H. Yoon and E. D. Wachsman, J. Am. Ceram. Soc., 2005,
suspension. The ESB suspension was deposited onto SNDC 88, 2402-2408.
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substrate by a transferpettor. The electrolyte film thickness can
Ionics, 1992, 52, 213-218.
be controlled by varying the suspension volume during coating. 12. J. Qian, Z. Zhu, J. Dang, G. Jiang and W. Liu, Electrochim. Acta,
For full cell preparation, ESB powder was mixed with LBSM 2013, 92, 243-247.
in weight ratio 1:1 thoroughly together with a 10 wt.% 13. J. Qian, Z. Tao, J. Xiao, G. Jiang and W. Liu, Int. J. Hydrogen Energy,
2013, 38, 2407-2412.
ethylcellulose-terpineol binder to prepare the composite 14. W. Sun and W. Liu, J. Power Sources, 2012, 217, 114-119.
cathode slurry ESB-LBSM. The slurry was then painted onto 15. K. Mehta, R. Xu and A. Virkar, J. Sol-Gel Sci. Technol., 1998, 11,
dense ESB electrolyte membrane and fired at 750 °C for 3 h in 203-207.
16. A. V. Virkar, J. Electrochem. Soc, 1991, 138, 1481-1487.
air to form porous cathode layer. Ag paste was applied to the 17. L. Zhang, L. Li, F. Zhao, F. Chen and C. Xia, Solid State Ionics, 2011,
cathode as a current collector and Ag wire was employed as the 192, 557-560.
conducting wire. The effective area of the cathode layer in 18. J. S. Ahn, D. Pergolesi, M. A. Camaratta, H. Yoon, B. W. Lee, K. T.
Lee, D. W. Jung, E. Traversa and E. D. Wachsman, Electrochem.
single cell was 0.237 cm2 while the cell diameter and the anode Commun., 2009, 11, 1504-1507.
area were 12.00 mm and 1.131 cm-2, respectively. 19. J.-Y. Park and E. D. Wachsman, Ionics, 2006, 12, 15-20.
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SNDC-ESB bilayer structure cell was tested in a home-made 23. K. T. Lee, D. W. Jung, H. S. Yoon, A. A. Lidie, M. A. Camaratta and
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cell testing system at 450-650 °C. Humidified hydrogen (~3% 24. W. Sun, L. Yan, B. Lin, S. Zhang and W. Liu, J. Power Sources, 2010,
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about 0.03 atm was achieved by bubbling H2 through water at 26. W. Sun, L. Yan, Z. Shi, Z. Zhu and W. Liu, J. Power Sources, 2010,
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Shanghai Chenhua)(0.1-100 kHz, 5 mV as AC amplitude). Ro

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High performance ceria-bismuth bilayer electrolyte low

Journal of Materials Chemistry A Accepted Manuscript

temperature solid oxide fuel cells (LT-SOFCs) fabricated by
combining co-pressing with drop-coating

Jie Hou,a Lei Bi, b,* Jing Qian, a Zhiwen Zhu, c Junyu Zhang a and Wei Liua,d,*
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The LT high performance SNDC-ESB bilayer structure cell was successfully

fabricated by combining one-step co-pressing with drop-coating.