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Metal-Free Bifunctional Ordered Mesoporous Carbon

for Reversible Zn-CO2 Batteries
Sanshuang Gao, Yifan Liu, Zhongyuan Xie, Yuan Qiu,* Longchao Zhuo, Yongji Qin,
Junqiang Ren, Shusheng Zhang, Guangzhi Hu,* Jun Luo, and Xijun Liu*

relating to the nonaqueous electrolytes,

The fabrication of Zn-CO2 batteries is a promising technique for CO2 fixation such as gel polymer/ionic liquid elec-
and energy storage. Herein, nitrogen-doped ordered mesoporous carbon trolyte.[1,12] Unlike Li/Na-CO2 batteries,
(NOMC) is adopted as a bifunctional metal-free electrocatalyst for CO2 aqueous Zn-CO2 battery, constructed
reduction and oxygen evolution reaction in the near-neutral electrolyte. The with inert Zn and aqueous electrolyte,
exhibits a high theoretical discharge
ordered mesoporous structures and abundant N-dopings of NOMC facilitate
voltage of 1.14  V (based on CO2 splitting
the accessibility and utilization of the active sites, which endow NOMC with to CO) and energy density of 949 Wh kg−1
excellent electrocatalysis performance and outstanding stability. Especially, a (calculated from the theoretical capacity
nearly 100% CO Faradaic efficiency is achieved at an ultralow overpotential of Zn).[13] Furthermore, regarding the
of 360 mV for CO2 reduction. When constructed as an aqueous recharge- cathodic CO2 reduction reaction (CO2RR,
able Zn-CO2 battery using NOMC as the cathode, it yields a high peak power CO2 + 2H+ +2e− → H2O + CO) and oxygen
evolution reaction (OER, H2O → 1/2O2  +
density of 0.71 mW cm−2, a good cyclability of 300 cycles, and excellent energy
2H+  + 2e−), the overall CO2 splitting
efficiency of 52.8% at 1.0 mA cm−2. (CO2  → 1/2O2  + CO) can be realized.[14]
However, the low Faradaic efficiency (FE)
and the accompanying hydrogen evolution
Burning fossil fuels has caused excessive emission of CO2, reaction (HER, 2H+ + 2e− → H2 and 2H2O + 2e− → 2OH− + H2)
which deteriorates the environment and creates many energy largely impedes the efficiency of the cathodic CO2 reduction.[15]
issues.[1,2] Great efforts are devoted to developing renewable Therefore, development of efficient bifunctional catalysts for
and eco-friendly strategies for CO2 utilization.[3–9] As a newly CO2RR and OER catalysts is strongly desired in the Zn-CO2
viable technology, rechargeable metal-CO2 batteries, combining battery energy system.
anodic metal with cathodic CO2 reduction to mimic artificial Currently, metal-based nanomaterials are the most inves-
photosynthesis, can realize sustainable electricity supplement tigated catalysts for Zn-CO2 battery.[16–18] Wang et  al. prepared
and value-added chemical production simultaneously.[9–11] Ir@Au cathode with 52.9% energy efficiency based on CO2
However, current nonaqueous metal-CO2 batteries (such as Li/ splitting at 1.0 mA cm–2 discharge current density and remark-
Na-CO2 batteries) still suffer from some disadvantages: the low able 90% FE of CO (FECO), providing a promising strategy for
operating voltages and energy densities caused by the low theo- CO2 conversion via a safe and eco-friendly pathway.[13] Wang
retical capacity of active anodes; environment contamination et al. fabricated isolated Fe atoms anchored on nitrogen-doped

S. Gao, Z. Y. Xie, Dr. Y. Qiu, Dr. Y. J. Qin, Prof. J. Luo, Prof. X. J. Liu Prof. J. Q. Ren
Institute for New Energy Materials and Low-Carbon Technologies State Key Laboratory of Advanced Processing and Recycling
Tianjin Key Lab of Photoelectric Materials and Devices of Nonferrous Metals
School of Materials Science and Engineering Lanzhou University of Technology
Tianjin University of Technology Lanzhou 730050, China
Tianjin 300384, China Prof. S. S. Zhang
E-mail: qiu_hp2007@163.com; xjliu@tjut.edu.cn College of Chemistry
Dr. Y. F. Liu Zhengzhou University
Key Laboratory of Optoelectronic Devices and Systems Zhengzhou 450000, China
of Ministry of Education and Guangdong Province Prof. G. Z. Hu
Shenzhen University Institute for Ecological Research and Pollution Control of Plateau Lakes
Shenzhen 518060, China School of Ecology and Environmental Science
Prof. L. C. Zhuo Yunnan University
School of Materials Science and Engineering Kunming 650504, China
Xi’an University of Technology E-mail: guangzhihu@ynu.edu.cn
Xi’an 710048, China Prof. X. J. Liu
The ORCID identification number(s) for the author(s) of this article Key Laboratory of Civil Aviation Thermal Hazards Prevention
can be found under https://doi.org/10.1002/smtd.202001039. and Emergency Response
Civil Aviation University of China
DOI: 10.1002/smtd.202001039 Tianjin 300300, China

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Figure 1.  Synthesis and characterizations of NOMC and control samples. a) Schematic illustration of NOMC preparation. b) TEM images of NOMC.
c) XRD patterns of NOMC, OMC, and NC. d) High-resolution N1s XPS spectra of NOMC, OMC, and NC.
porous carbon, achieving a high FECO of 96% and a power
density of 0.6  mW cm−2.[19] Xie et  al. developed a porous Pd
nanosheet accompanied with enriched edges, resulting in
81.2% energy efficiency between CO2 and formic acid reversible
conversion.[20] Despite these pioneering researches, the appli-
cation of metal-free catalysts in Zn-CO2 battery is still scarce,
although they show overwhelming advantages of low price and
good cyclic stability compared with the metal-based ones.[21,22]
Herein, nitrogen-doped ordered mesoporous carbon
(NOMC) with abundant parallel channels was prepared. It
manifests an ultrahigh specific surface area, which benefits for
exposing abundant nitrogen active sites and facilitates reactant
transportation during CO2RR and OER. As a result, NOMC
reveals nearly 100% FECO and 80 h stability at –0.47  V versus
reversible hydrogen electrode (vs RHE) for CO2RR. Meanwhile,
at the cathode electrode, the OER overpotential at 10 mA cm−2
is only 586 mV in the 0.8 m KHCO3 electrolyte. Benefiting from
the excellent bifunctional performance of NOMC, the as-con-
structed rechargeable Zn-CO2 battery achieves a peak power
density of 0.71 mW cm–2 and energy efficiency of 52.8%. More-
over, it maintains an outstanding FECO of 76% at a discharge
current density of 1.0 mA cm−2, as well as 300-times cyclability.
As shown in Figure 1a, NOMC was synthesized via a pyrolysis-
etching method, by using ethylenediamine (EDA)-tetrachlo-
romethane (CCl4) complex as carbon/nitrogen resources and
SBA-15 as the pore-forming agent (see details in the Experi-
mental Section).[23] The transmission electron microscopy
(TEM, Figure 1b and Figure S1, Supporting Information) images
show that the ordered meso- and microporous structure were
perfectly inherited from SBA-15 zeolite (Figure S1, Supporting
Information), which would not only accelerate the transpor-
tation of reactants/intermediates but also expose abundant
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active nitrogen sites for electrocatalysis.[24,25] The energy-dis-
persive X-ray (EDX) spectroscopy elemental mappings show
that nitrogen elements are distributed homogenously over the
entire carbon matrix of NOMC (Figure S2, Supporting Informa-
tion). For comparison, the ordered mesoporous carbon (OMC)
and nitrogen-doped carbon (NC) samples were also success-
fully synthesized (Figures S3 and S4, Supporting Information).
For OMC, similar ordered channels are uniformly generated as
NOMC excepting the absence of nitrogen element. In contrast,
the abundant nitrogen element is distributed uniformly on NC,
while no pores/channels can be discerned.
The N2 adsorption–desorption isotherms confirm that
NOMC and OMC (Figure S5, Supporting Information) have
a large specific surface area of 794.6 and 713.5 m2 g−1, respec-
tively. Moreover, both of them show similar hierarchical pore
structures, with a micropore size <2  nm and a mesopore
size around 6  nm. X-ray diffraction (XRD) patterns of NC in
Figure 1c display a bump at around 23.5°, corresponding to the
(002) plane of graphitic carbon.[26] The (002) plane of NOMC
and NC shift to a higher angle, which is attributed to that the
heteroatom N-doping compresses the interlayer distance of
graphene.[27] Raman spectroscopic measurements show two
peaks located at ≈1590 cm−1 (G band) and 1320 cm−1 (D band),
relating to the sp2-type graphitized carbon and the sp3-type dis-
order carbon, respectively.[28,29] The intensity ratios of D band
to G band (ID/IG) of NOMC, OMC, and NC are calculated to
be 1.03, 1.01, and 1.08, respectively, suggesting a similar degree
of graphitization and disorder in these samples (Figure S6,
Supporting Information).[30] X-ray photoelectron spectroscopy
(XPS) survey spectrum of NOMC (Figure S7, Supporting Infor-
mation) shows a chemical composition of carbon (88.8 at%),
nitrogen (5.9 at%), and oxygen (5.3 at%). However, the nitrogen
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Figure 2.  CO2RR and OER electrochemical characterization of the NOMC in near-neutral solution, with OMC and NC for comparison. a) CO2RR linear
sweep voltammetry curves in CO2 and N2-saturated 0.8 m KHCO3 electrolyte with a scan rate of 10 mV s–1. b) CO Faradaic efficiency in potentiostatic
electrolysis. c) The CO Faradaic efficiency and current density of NOMC from long-term stability tests for 80 h at −0.47 V vs RHE. d) OER linear sweep
voltammetry curves of NOMC, OMC, and NC in 0.8 m KHCO3 electrolyte with a scan rate of 10 mV s–1. e) Tafel plots for OER. The current densities
were calculated based on the geometric area.

content in NC is 6.9 at%, slightly higher than that of NOMC,
possibly because the introduction of SBA-15 template enlarged
the surface area of EDA-CCl4 polymer and accelerated the emis-
sion of N-rich species during the calcining process in NOMC.
On the contrary, no distinguishable nitrogen-related signals
can be detected for OMC, consistent with the EDX mapping
results in Figure S3 (Supporting Information). From the high-
resolution C 1s XPS spectra of both NOMC and NC, the CN
and CN bonds can be fitted at 285.5 and 288.1 eV, respectively,
indicating the successful doping of nitrogen into the carbon
substrate[31] (Figure S8, Supporting Information). The pyri-
dinic-N, pyrrolic-N, graphitic-N, and oxidized-N can be detected
in both NOMC and NC at the binding energies of 398.2, 399.6,
401.1, and 403.0  eV, respectively (Figure  1d).[32,33] The contents
of pyridinic-N and graphitic-N in NOMC (Table S1, Supporting
Information), which play an important role in CO2 reducing to
CO,[34,35] are comparable to those of NC.
The catalytic activities of NOMC toward CO2RR were inves-
tigated in an H-type cell in 0.8 m CO2-saturated KHCO3.
Linear sweep voltammetry (LSV) curves were recorded under
CO2- and N2-saturated electrolyte conditions, respectively. As
shown in Figure  2a, the CO2-saturated electrolyte boosts the
current density and motivates onset potential positively than
the N2-saturated ones, suggesting that NOMC, OMC, and NC
all possess CO2RR activity.[36,37] Furthermore, NOMC exhibits
an overwhelming CO2RR current density of −15.9 mA cm–2 at
−0.8 V vs RHE, much higher than that of OMC (−2.7 mA cm–2)
and NC (−2.1 mA cm–2). The gas chromatography (GC) and 1H
nuclear magnetic resonance (1H NMR) spectrometer were car-
ried out to quantitatively analyze reduction products (Figure S9,
Supporting Information). Impressively, only CO was detected
as a single product with nearly 100% at an extremely low
overpotential of 360  mV (−0.47  V vs RHE) (Figure  2b and
Figures S10 and S11, Supporting Information). However,
NC and OMC only obtained the maximum FECO of 52.2%
(−0.57  V vs RHE) and 2.9% (−0.87  V vs RHE) (Figure S12,
Supporting Information), respectively. This excellent CO2RR
performance of NOMC also surpasses most of the previously

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reported metal-free and even noble catalysts (Table S2, Sup-
porting Information).
To unravel the reason for the high CO2RR performance of
NOMC, the electrochemical impedance spectroscopy (EIS)
analysis was conducted (Figure S13, Supporting Information).
As shown, the NOMC possesses a smaller diameter of the
semicircle in high frequency, indicating higher conductivity
and electronic transfer kinetics of NOMC compared with OMC
and NC.[38,39] Furthermore, the electrochemically active sur-
face areas (ECSA) of the samples were also tested according
to the double-layer capacitance (Cdl) method.[40] As displayed
in Figure S14 (Supporting Information), NOMC exhibited a
3.2 times higher ECSA value than that of NC. The CO current
densities (jco) of NOMC and NC were further normalized by
the ECSA as shown in Figure S15 (Supporting Information).
At −0.57 V vs RHE, ECSA-corrected jco value of NOMC can be
calculated as 45.9 µA cm−2, obviously higher than that of NC
(18.3 µA cm−2). Considering the similar nitrogen content for
the two samples (Table S1, Supporting Information), the higher
CO2RR activity of NOMC can be attributed to its higher expo-
sure to active sites and better mass transferability.[24,41] It is sug-
gested that the CO2 transport can be enhanced by the porosity
of the electrode through increasing the gas permeability and
effective diffusivity.[42] For OMC, the ECSA-corrected jco value
is much lower than that of NOMC and NC, suggesting poor
intrinsic activity. These two control samples highlight the
importance of abundant N-doping and pore channels in NOMC
for CO2RR. Besides, the CO2RR stability of NOMC was evalu-
ated by prolonged chronopotentiometry under the optimal
potential. Attractively, it showed super stability for as long as
80 h (Figure 2c), during which process the NOMC continuously
converted CO2 to CO with FECO values maintaining over 90%
and current density without obvious decay.
We further performed the density functional theory (DFT)
calculations to study the effects of N-modification on the
intrinsic reactivity of NOMC. Pyridinic-N and graphitic-N
were used to mimic the N-doping in NOMC because of their
good CO2RR activity.[34,43] As shown in Figure S16 (Supporting
Information), the CO2 reduction to CO proceeds via coupled
proton–electron transfer steps. The limiting potential originates
from the formation of COOH* because of the maximum uphill
energy barrier. Apparently, the required energy barrier to form
the COOH* on pyridinic-N and graphitic-N is significantly
lower than that on graphitic-C, indicating the high CO2RR
activity of N-doping sites. It indicates the important role of
N-doping for CO2RR and explains the high CO2RR activity of
NOMC over OMC.
The OER LSVs of NOMC, NC, and OMC were also inves-
tigated in 0.8 m KHCO3 electrolyte. As shown in Figure  2d,
NOMC possessed a current density of 10 mA cm–2 at 1.82 V vs
RHE. The performance surpasses other carbon-based metal-
free catalysts in the near-neutral condition.[22] At the same
potential of 1.82  V vs RHE, OMC just showed a current den-
sity of 6.4 mA cm–2, whereas NC displayed a current density of
8.0 mA cm–2. The higher OER performance of NOMC empha-
sizes the importance of the N-doping and exposed surface of
the catalysts in OER.[44,45] The superior OER activity of NOMC
was also confirmed by the kinetics analysis. As shown in
Figure  2e, NOMC possessed a Tafel slope of 397.5  mV dec–1,
Small Methods 2021, 5, 2001039 2001039  (4 of 6)
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lower than that of the OMC (404 mV dec–1) and NC (483.5 mV
dec–1) samples.[46] Therefore, the high performance of NOMC
toward CO2RR and OER makes it a promising cathode for
aqueous rechargeable Zn-CO2 batteries.
An aqueous Zn-CO2 battery was designed using NOMC as
a cathode as shown in Figure  3a and Figure S17 (Supporting
Information). The basic 6.0 m KOH with 0.2 m Zn(CH3COO)2
was used as anolyte, and near-neutral 0.8 m KHCO3 was
applied as catholyte. The two compartments were separated
by a bipolar membrane to maintain their pH values and avoid
cross contaminations.[13] The CO2RR occurred on the cathode
during the discharge process, which was driven by the dis-
solution of Zn foil on the anode. OER happened during the
charging process, which was accompanied by the deposition
of Zn on the anode.[1,13,19] The discharge and charge polariza-
tion curves and the corresponding power density of a single
Zn-CO2 battery are shown in Figure  3b,c. A maximum power
density of 0.71 mW cm–2 can be achieved at a current density of
3.0 mA cm–2, which is even larger than the Fe single-atom based
ones (Table S3, Supporting Information).[19] Furthermore, at a
discharge current density of 0.5 mA cm–2, a discharge voltage of
0.48 V was obtained with an energy efficiency of 53.2% and an
energy density of 308.64  Wh kg–1 (Table S4, Supporting Infor-
mation). As the discharge current increases to 1.0  mA cm–2,
the energy efficiency comes to 52.8% and the energy density
comes to 257.2 Wh kg–1, comparable with the noble Ir@Au cata-
lyst (Table S3, Supporting Information).[13] The Zn-CO2 battery
can afford a stable open-circuit voltage of 0.9  V as shown in
Figure 3d. Two series-connected Zn-CO2 batteries based on the
NOMC cathode can power a small light-emitting diode (LED)
light, showing a stale voltage of 1.79 V (Figure S18, Supporting
Information). Furthermore, the CO gaseous product shows
a stable FE of 67–76% when discharged at a constant current
density of 0.5–2.0  mA cm–2, suggesting the outstanding CO2-
to-CO conversion ability and operation durability of the Zn-CO2
battery device in a wide discharge current range (Figure  3e).
Besides, the NOMC-based Zn-CO2 battery shows stable charge
and discharge curves at a constant current density (Figure S19,
Supporting Information), and the galvanostatic discharge–
charge cycling curves at 1.0  mA cm–2 maintained stable volt-
ages during 300 cycles and 100 h (Figure  3f). The TEM, EDX
images, and XRD pattern of NOMC after stability tests con-
firmed the maintaining of its morphology and ordered pore
structure (Figures S20 and S21, Supporting Information). In
this respect, the metal-free cathode-based Zn-CO2 battery is
promising as an effective CO2 conversion and energy storage
device in terms of its good discharge property and stability.
In summary, we have prepared an N-doped ordered
mesoporous carbon as a bifunctional metal-free electrocata-
lyst for CO2 reduction and oxygen evolution reaction. As a CO2
reduction cathode in 0.8 m KHCO3, the catalyst shows a CO2-
to-CO conversion with nearly 100% FE at a 360 mV overpoten-
tial. During the near-neutral oxygen evolution process, it needs
1.82  V vs RHE to afford 10  mA cm–2. The control samples
confirm the important role of the ordered mesoporous struc-
ture and N-doping during the electrocatalysis. When assem-
bled as an aqueous rechargeable Zn-CO2 battery with Zn foil,
it demonstrates a maximal power density of 0.71  mW cm–2.
Furthermore, the outstanding high energy efficiency of 52.8%
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Figure 3.  The performance of the aqueous rechargeable Zn-CO2 electrochemical cell. a) Schematic representation of the Zn-CO2 battery. b) Discharge
and charge polarization curves with a scanning rate of 10 mV s–1. c) Power density curves of the assembled Zn-CO2 battery. d) The open-circuit voltage.
Inset is the photograph of one Zn-CO2 battery. e) Galvanostatic discharge curves at different current densities and the corresponding CO Faradaic
efficiencies. f) Galvanostatic discharge–charge cycling curves at 1.0 mA cm–2.

and an energy density of 257.2 Wh Kg–1 are achieved when dis- Data Availability
charged at 1.0  mA cm–2. Moreover, it demonstrated a stable
Research data are not shared.
CO2-to-CO reduction with 67–76% Faradaic efficiency at dif-
ferent current densities and superlong stability of more than
100 h (300 cycles). This work demonstrates the metal-free
NOMC catalyst as an efficient, cost-effective, and robust cathode Keywords
for reversible Zn-CO2 batteries. bifunctional catalysts, carbon dioxide reduction, metal-free catalysts,
nitrogen-doped ordered mesoporous carbon, Zn-CO2 batteries

Supporting Information Received: October 28, 2020

Revised: December 17, 2020
Supporting Information is available from the Wiley Online Library or
Published online: January 18, 2021
from the author.

Acknowledgements
S.S.G. and Y.F.L. contributed equally to this work. This work was financially
supported by National Key R&D Program of China (2017YFA0700104
and 2019YFC1804400), National Natural Science Foundation of China
(21601136, 62005173, 51971157, 22075211, 21677171, 21505154, 51621001
and 51761165012), Tianjin Science Fund for Distinguished Young
Scholars (19JCJQJC61800), the Science and Technology Development
Fund of Tianjin Education Commission for Higher Education (No.
2018KJ126) and the Double Tops Joint Fund of the Yunnan Science and
Technology Bureau and Yunnan University (2019FY003025).
Conflict of Interest
The authors declare no conflict of interest.
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