Efficient electroreduction of CO2 to C2 products over B-doped oxide-derived copper

Article abstract of DOI:10.1039/c8gc02389a

B-Doped oxide-derived-Cu is a highly efficient electrocatalyst for transformation of CO₂ to C2 products. The faradaic efficiency of C2 products could reach 48.2%, with a high current density of 33.4 mA cm^-2 at low potentials in 0.1 M KHCO₃ electrolyte. The excellent performance of the catalyst is mainly attributed to Cu⁺ species stabilized by the introduction of B.

Full text of DOI:10.1039/c8gc02389a

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DOI: 10.1039/C8GC02389A
B-doped oxide-derived-Cu achieves the total Faradaic efficiency for C2 products of 48.2 % via
stabilizing Cu+ species.

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COMMUNICATION
Efficient electroreduction of CO to C2 products over B-doped
2
Oxide-derived copper
a,b
a,b
a,b
a,b
a
a
a
Received 00th January 20xx,
Accepted 00th January 20xx
Chunjun Chen, Xiaofu Sun,* Lu Lu, Dexin Yang, Jun Ma, Qinggong Zhu, Qingli Qian, and
a,b
Buxing Han*
DOI: 10.1039/x0xx00000x
www.rsc.org/
B-doped oxide-derived-Cu is highly efficient electrocatalyst for oxide-derived copper (OD-Cu) has been discovered as a simple
transformation of CO to C2 products. The Faradaic efficiency of method to decrease the overpotential and increase the
C2 products could reach 48.2 % with a high current density of 33.4 selectivity towards multi-carbon products for CO A
2
[30-31]
2
RR.
electrolyte. The recent report of oxygen plasma-activated OD-Cu catalysts
excellent performance of the catalyst is mainly attributed to much achieved an ethylene Faradaic efficiency (FE) of 60% at −0.9 V
-
2
mA cm at low potentials in 0.1 M KHCO
3
+
Cu species stabilized by the introduction of B.
versus reversible hydrogen electrode (RHE), which can be
[32]
+
attributed to the presence of abundant Cu species.
In
The worldwide increasing emission of CO
climate change issue and environment pollution. As CO
safe and abundant C1 resource, it is very desirable to convert
CO to value-added chemicals or fuels through clean and
economical chemical processes for the sustainable
2
has caused serious
another case, the thick OD-Cu films showed higher selectivity
for ethane and ethanol than the thin OD-Cu films, which can
2
is a
+
[33]
be attributed to a higher content of Cu sites. These systems
have been verified that the C2+ products production was
2
+
+
promoted by Cu species, but Cu species were not stable at
negative potentials. Development of OD-Cu-based catalysts
[
1-7]
development of human civilization.
reaction of CO (CO RR) is regarded as a prospective pathway,
because the used electricity can be generated from renewable
Electroreduction
+
with high stablity of Cu species, which can realize high
2
2
selectivity of C2+ products in CO
2
RR, is still highly desired.
[
8-10]
energy sources, such as solar and wind.
efforts have been explored to improve the activity of CO
produce C1 products (such as CO, formic acid and
Up to date, many
The incorporation of boron (B) atom into catalysts is an
[28, 34-35]
2
RR to
efficient approach to promote CO
RR.
A boron-doped
2
Pd catalyst has been reported to boost formate production
over wide potential window, which results from the doped B
[11-20]
methanol).
2
However, reduction of CO to C2+ products
[
34]
usually shows poor selectivity and requires large
downshifted d band centre of surface Pd atoms. B-doped
nanodiamond electrodes overcomes the usual limitation of the
low yield of higher-order products, and exhibits very high FE
[21-22]
overpotential.
It would certainly be desirable to discover
2
an electrocatalyst that can directly reduce CO to C2+ products
[35]
with high selectivity and energy efficiency.
(
74%) for formaldehyde production.
It was been reported
Cu-based materials were found to be the most promising
electrocatalysts for converting CO to C2+ products, such as
ethylene, ethane, ethanol, acetic acid and n-propanol.
Many methods have been applied to enhance the activity of
CO to C2+ products over Cu-based catalysts, including
modifying morphology,
that B-doped Cu nanoparticles with stable electron localization
[28]
2
can boost CO
can affect the electronic configuration of the surrounding
atoms and further enhance the activity of CO RR. Therefore,
conversion. These indicated that the doped B
2
[
23-24]
2
2
we believe that the introduction of B into OD-Cu can modify
the electronic structure of Cu, and potentially lead to improve
[25]
[26]
[27]
changing the size,
alloying,
[28]
[29]
doping, and modifying with other molecules. In particular,
2
the selectivity and stability for CO RR to C2+ products.
Herein, we prepared B-doped OD-Cu (B-OD-Cu). It was
found that the B-OD-Cu could enable selective conversion of
a.
Beijing National Laboratory for Molecular Sciences, CAS Key Laboratory of Colloid
2
CO to C2 products. The total FE of C2 (ethylene, ethane and
and Interface and Thermodynamics, CAS Research/Education Center for
Excellence in Molecular Sciences, Institute of Chemistry, Chinese Academy of
Sciences, Beijing 100190, P. R. China
ethanol) could reach 48.2% with a current density of 33.4 mA
-2
cm at low applied potentials in 0.1 M KHCO electrolyte. The
3
E-mail: sunxiaofu@iccas.ac.cn; hanbx@iccas.ac.cn
School of Chemistry and Chemical Engineering, University of Chinese Academy of
Sciences; Beijing 100049, China.
b.
high catalytic activity of B-OD-Cu is attributed to abundant
+
catalytic activity sites as well as the numerous Cu species,
Electronic Supplementary Information (ESI) available: [details of any
supplementary information available should be included here]. See
DOI:10.1039/x0xx00000x
which was stabilized by the doped B.
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The procedures to synthesize B-OD-Cu are shown suggests that the surface B atoms are sub-oxidized, indicating an
schematically in Fig. 1. Briefly, the polished Cu foils were first effective electron transfer from Cu to B in the B-OD-Cu. Besides, the
immersed into a chemical bath, which is prepared with NaOH, actual content of B determined by XPS was 3.46 at%.
K
2
S
2
O
8
and deionized water. After 4 h, a film of Cu(OH)
generated. Then the solution of B was dropped on the
surface of Cu(OH) film, and dried at 80 °C. The obtained B
Cu(OH) film was calcined at 500 °C under air for 3 h in a
2
was
2
O
3
2
2 3
O -
2
muffle furnace to get B-doped oxided copper (B-O-Cu). After
that, B-O-Cu was electrochemically reduced at -2.0 V vs. RHE
for 500 s and B-doped oxide-derived copper (B-OD-Cu) was
obtained. In order to explore the role of doped B, OD-Cu was
prepared by the same method as B-OD-Cu except with no
addition of B O solution.
2
3
Fig. 2 A) SEM image of B-O-Cu. B) SEM image of B-OD-Cu. The inset
image is the high magnification of B-OD-Cu. (The bar was 200 nm.) C)
TEM image and elemental mappings of B-OD-Cu. The bar was 500 nm.
D) XRD patterns of the different samples: Cu(OH)
OD-Cu (c) and OD-Cu (d).
2
(a), B-O-Cu (b), B-
The CO
were tested using a typical H-type cell with CO
.1 M KHCO solution (pH 6.8) as electrolyte. As revealed by
2
RR activities of B-OD-Cu, OD-Cu, Cu(OH)
2
and Cu foil
[4]
2
-saturated
0
3
linear sweep voltammetry (LSV) in Fig. S2, B-OD-Cu achieved
the highest total current density from -0.6 V to -1.2 V vs. RHE.
Fig. 1 Schematic illustration of the procedures to prepare B-OD-Cu.
The onset potential of CO
2
RR for B-OD-Cu the tangent line
method, was -0.47 V, which was lower than that of OD-Cu (-
.51 V), Cu(OH) (-0.53 V) and Cu (-0.69 V). Controlled
potential electrolysis of CO at each given potential were
performed to quantify the gas product by gas chromatography
[38]
Scanning electron microscope (SEM) images of B-O-Cu and
B-OD-Cu are shown in Fig. 2. It can be seen that the as-
synthesized B-O-Cu has a plate-like morphology and the
surface was smooth with no observable structural defects (Fig.
0
2
2
(
GC) and the liquid product by nuclear magnetic resonance
NMR) spectroscopy. As shown in Fig. 3, Fig. S3 and S4, various
2A). However, after electrochemical reduction, the surface of
(
B-OD-Cu became much rougher and many individual
nanodomains are observed (Fig. 2B). The element composition
of B-OD-Cu was determined by the energy dispersive X-ray
spectroscopy (EDS), indicating homogeneous distribution of
Cu, O and B in the obtained B-OD-Cu (Fig. 2C).
products, including ethylene, ethane, ethanol, CO, methane,
formate and H , were detected with a combined FE of around
00 % for all the studied catalysts. In detail, B-OD-Cu reached a
total FE for C2 products of 48.2 % at -1.05 V vs. RHE (Fig. 3A)
2
1
-2
with a current density of 33.4 mA cm , while OD-Cu could only
achieve a maxmum FE of 30.5 % for C2 products (Fig. 3B). At a
low applied potential of -0.7 V vs. RHE, B-OD-Cu also exhibited
a FE of 27.1 % for C2 products, while for OD-Cu, the FE for C2
was only 1.8 %. This indicates that the introduction of B atoms
can decrease applied potential and increase selectivity of C2
X-ray diffraction (XRD) was used to check the crystal
structure change in the preparation process of B-OD-Cu (Fig.
2
D). After treatment of Cu foil in NaOH-K
solution, the diffraction peaks of Cu(OH) can be observed in
the XRD pattern. The new diffraction peaks in B-O-Cu can be
assigned to Cu (BO(OH) OH) (PDF 38-0595), which indicated
that Cu(OH) can react with B
2 2 8
S O aqueous
2
2
2
3
2
products. Interestingly, when using Cu(OH) as the working
2
2
O
3
to form Cu
2
(BO(OH)
2
OH)
3
at
electrode, C2 products cannot be detected untill the potential
was -0.9 V vs. RHE. The maximum FE for C2 products was only
o
500 C in air. After the electroreduction of B-O-Cu, the peaks
of Cu
2
(BO(OH)
2
OH)
3
disappeared and the peaks of Cu
(BO(OH) OH)
O and Cu. X-ray photoelectron spectroscopy (XPS) was
2
O were
2
4.4 % at -1.1 V vs. RHE (Fig. 3C). Besides, no C2 products can
be detected over the pure Cu film at low applied potential (Fig.
D). When the potential was higher than -1.05 V vs. RHE, only
observed, demonstrating that Cu
to Cu
2
2
3
was reduced
2
3
employed to study the chemical states of the B species on B-OD-Cu
surface. As shown in Fig. S1, the B 1s binding energy is 192 eV,
a little of ethylene was produced, and the maximum FE for
ethylene reached 15.2 % at -1.2 V vs. RHE. As shown in Fig. 3E
and Fig. S5, B-OD-Cu have the highest total current density and
0
[36]
3+
[37]
which was between B (186-187 eV)
and B (∼193 eV) . It
2
| J. Name., 2012, 00, 1-3
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C2 partial current density than those of OD-Cu, Cu(OH)
COMMUNICATION
2
and Cu performance of CO
2
RR was examined over different B-OD-Cu
film. The total current density reached 8.1, 14.2, 21.2, 26.1, electrodes with varying B content at -1.05 V vs. RHE (Fig. S9).
-
2
3
3.4, 36.2 and 41.2 mA cm at -0.7, -0.8, -0.9, -1.0, -1.05, -1.1 We can see that the FEs for C2 products have the similar trend
and -1.2 V, respectively. For C2 partial current density, it can with the content of B in B-OD-Cu, indicating that B was crucial
-
2
reach 2.2 mA cm when the applied potential was only -0.7 V to CO
2
RR.
vs. RHE, which is also very high. This indicates that the
introduction of B into OD-Cu can promote the CO
rate and decrease the applied potential.
2
reduction
Fig. 4 A) The reduction current density at -1.05 V vs. RHE plotted against
the square root of scan rate for B-OD-Cu (a), OD-Cu (b), Cu(OH) (c) and Cu
d). B) Nyquist plots for different electrodes in CO -saturated 0.1mol/L
KHCO electrolyte: B-OD-Cu (a), OD-Cu (b), Cu(OH) (c) and Cu (d) . C) Cu 2p
2
(
2
3
2
XPS peak for B-OD-Cu and OD-Cu. D) LMM Auger spectra of Cu for B-OD-Cu
and OD-Cu.
Additionally, with regard to the notable enhancement of
catalytic activity for B-OD-Cu, the electrochemical active
surface area was characterized and shown in Fig. 4A. According
to the measured double-layer capacitance, B-OD-Cu had the
largest electrochemical active surface area, which was
estimated to be roughly 1.3, 2.0 and 5.5 times higher than that
Fig. 3 A) FE for C2 products over B-OD-Cu at different potentials. B) FE
for C2 products over OD-Cu at different potentials. C) FE for C2
of OD-Cu, Cu(OH)
2
and Cu foil. It indicated that B-OD-Cu had
RR. The electrochemical
2
products over Cu(OH) at different potentials. D) FE for C2 products
more catalytic active sites for CO
2
over Cu film at different potentials. E) Total current density for
different electrodes at different potentials: B-OD-Cu (a), OD-Cu (b),
impedance spectroscopy (EIS) was also tested, and the Nyquist
plot was obtained by running the experiment at an open
circuit potential (Fig. 4B). B-OD-Cu showed the lowest
interfacial charge transfer resistance and electron transfer to
B-OD-Cu electrode surface in electrolyte is more facile than to
other electrode surface. It ensures a faster electron transfer to
2
Cu(OH) (c) and Cu film (d). F) Time curves of the electrolysis processes
over B-OD-Cu at -1.05 vs. RHE and the FE for the products.
Furthermore, the long-term stability of B-OD-Cu was tested
at -1.05 V vs. RHE for 10 h (Fig. 3F). It can be seen that both
the current density and the FE for C2 products was stable with
time during the entire period. The SEM image, XRD and XPS
spectra for B-OD-Cu after the electrolysis of 10 h were given in
Fig. S6-S8. The difference before and after electrolysis process
was not notable, further indicating the excellent stability of the
B-OD-Cu.
•
−
CO
for CO
According to previous reports,
C2+ products over Cu-based catalysts in CO
2
for forming reduced CO
2
intermediate, which was vital
2
RR.
[30, 32, 33]
the high selectivity of
RR can be
2
+
attributed to the high content of Cu species. Hence, we
attempted to compare the valence state of Cu for B-OD-Cu and
OD-Cu by using the semi-in-situ X-ray photoelectron
To clarify the role of B content on CO RR performance, we
2
[39]
spectroscopy method. The detailed operation was described
also synthesized a series of B-OD-Cu with different B contents
by using the same method except for changing the
in the Supporting Information. As shown in Fig. 4C, the Cu 2p
+
XPS showed that Cu or Cu state exists in B-OD-Cu and OD-Cu,
0
concentration of B O solution. The contents of B for different
2
3
2+
and no Cu peaks were observed. However, it was difficult to
B-OD-Cu samples were determined by the XPS spectra (Table
S1). It can be seen that the actual B content increased with the
+
distinguish between Cu and Cu states in the Cu 2p peak due
0
+
to the close similarity in the binding energies of the Cu and
increasing B O solution concentration, and kept unchange
2
3
0
Cu states.
[40]
-1
The Auger Cu LMM line was further used to
when the concentration reached 0.36 mol L . The
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+
analyze the surface state (Fig. 4D). It can be seen that Cu was 13 L. A. Diaz, N. Gao, B. Adhikari, T. E. Lister, E. J. Dufek and A.
0
D. Wilson, Green Chem. 2018, 20, 620.
14 Q. Zhu, J. Ma, X. Kang, X. Sun, J. Hu, G. Yang, B. Han, Sci.
China Chem. 2016, 59, 551.
the main species in B-OD-Cu and only a little intense of Cu
0
was observed. However, for OD-Cu, both Cu and Cu species
+
0
existed and Cu was the main species on the surface. This
1
5 H. Yang, S.-F. Hung, S. Liu, K. Yuan, S. Miao, L. Zhang, X.
Huang, H.-Y. Wang, W. Cai, R. Chen, J. Gao, X. Yang, W. Chen,
Y. Huang, H. M. Chen, C. M. Li, T. Zhang, B. Liu, Nat. Energy
+
indicates that the doped B can stabilize abundant Cu species,
which can improve the activity of CO
products.
2
RR to generate C2
2
018, 3, 140.
1
1
1
1
6 S. Hernández, M. Amin Farkhondehfal, F. Sastre, M. Makkee,
G. Saracco and N. Russo, Green Chem. 2017, 19, 2326.
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483.
Conclusion
In conclusion, we have found that B-OD-Cu exhibits excellent
performance for CO RR to C2 products. The FE of C2 products
2
-2
can reach 48.2 % with a current density of 33.4 mA cm when
the content of doped B is 3.46 at%. The introduction of B can
not only promote the activity of C2 products, but also enhance
2
2
0 X. Kang, X. Sun, Q. Zhu, X. Ma, H. Liu, J. Ma, Q. Qian and B.
Han, Green Chem. 2016, 18, 1869.
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2
the stability of CO reduction. The high catalytic activity of B-
OD-Cu can be mainly attributed to more catalytic sites and
+
stable Cu species. We believe that introduction of light
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There are no conflicts to declare.
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Acknowledgements
The work was supported by National Natural Science
Foundation of China (21533011,21733011), the National Key
Research
2017YFA0403102), and Chinese Academy of Sciences (QYZDY-
SSW-SLH013).
and
Development
Program
of
China
(
2
3
3
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