Bipyridine-Assisted Assembly of Au Nanoparticles on Cu Nanowires To Enhance the Electrochemical Reduction of CO2

Article abstract of DOI:10.1002/anie.201905318

We report a new strategy to prepare a composite catalyst for highly efficient electrochemical CO₂ reduction reaction (CO₂RR). The composite catalyst is made by anchoring Au nanoparticles on Cu nanowires via 4,4′-bipyridine (bipy). The Au-bipy-Cu composite catalyzes the CO₂RR in 0.1 m KHCO₃ with a total Faradaic efficiency (FE) reaching 90.6 % at ?0.9 V to provide C-products, among which CH₃CHO (25 % FE) dominates the liquid product (HCOO^?, CH₃CHO, and CH₃COO^?) distribution (75 %). The enhanced CO₂RR catalysis demonstrated by Au-bipy-Cu originates from its synergistic Au (CO₂ to CO) and Cu (CO to C-products) catalysis which is further promoted by bipy. The Au-bipy-Cu composite represents a new catalyst system for effective CO₂RR conversion to C-products.

Full text of DOI:10.1002/anie.201905318

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Accepted Article
Title: Bipyridine-assisted assembly of Au nanoparticles on Cu
nanowires to enhance electrochemical reduction of CO2
Authors: Jiaju Fu, Wenlei Zhu, Ying Chen, Zhouyang Yin, Yuyang Li,
Juan Liu, Hongyi Zhang, Junjie Zhu, and Shouheng Sun
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To be cited as: Angew. Chem. Int. Ed. 10.1002/anie.201905318
Angew. Chem. 10.1002/ange.201905318
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10.1002/anie.201905318
Angewandte Chemie International Edition
COMMUNICATION
Bipyridine-assistedassembly of Au nanoparticles on Cu
nanowires to enhance electrochemical reduction of CO2
Jiaju Fu[a, b, ‡], Wenlei Zhu[a, ‡], Ying Chen[b], Zhouyang Yin[a], Yuyang Li[a], Juan Liu[b], Hongyi Zhang[a],
Jun-Jie Zhu*[b] and Shouheng Sun*[a]
Abstract: We report a new strategy to prepare a composite catalyst
for highly efficient electrochemical CO2 reduction reaction (CO2RR).
The composite catalyst is made by anchoring Au nanoparticles on Cu
nanowires via 4,4’-bipyridine (bipy). The Au-bipy-Cu catalyzes the
CO2RR to C-products in 0.1 M KHCO3 with a total Faradaic efficiency
(FE) reaching 90.6% at −0.9 V among which CH3CHO (25% FE)
dominates the liquid product (HCOO−, CH3CHO, and CH3COO− )
distribution (75%). The enhanced CO2RR catalysis demonstrated by
Au-bipy-Cu originates from its synergistic Au (CO2 to CO) and Cu (CO
to C-products) catalysis which is further promoted by bipy. The Au-
bipy-Cu represents a new catalyst system for effective CO2RR
conversion to C-products.
Electrochemical CO2 reduction reaction (CO2RR) under ambient
conditions is an important approach to understand CO2RR and to
improve CO2RR conversion efficiency for renewable energy
applications.[1] Past studies on electrochemical CO2RR have
shown that it is possible to convert CO2 to CO with high activity
and selectivity on metal-based nanostructured surfaces.[2]
However to convert CO2 efficiently to hydrocarbon products has
been challenging. Nanostructured Cu must be present and the
side reaction, hydrogen evolution reaction (HER), in the aqueous
electrolyte solution often competes with the main CO2RR,
lowering the CO2RR selectivity and efficiency,[3] unless CO is
reduced directly[4].Here we reportthe enhanced CO2RR catalysis
of the Au-Cu composite catalyst for the selective formation of C-
products. In this study, we assembled Au NPs on Cu NWs using
4,4’-bipyridine(bipy) as a linker, forming a new composite catalyst
Au-bipy-Cu (Figure 1a). The electrochemical CO2RR in aqueous
solution of 0.1 M KHCO3 showed Au/Cu mass-dependent
selectivity with Au/Cu =1/2 ratio yielding the highest selectivity to
C-products with a total FE of 90.6% at −0.9 V (vs. RHE, same
hereinafter) among which CH3CHO (25% FE) dominates the
liquid product (HCOO−, CH3CHO, and CH3COO−) distribution
(75%). Our studies demonstrate a new approach to tune
synergistic catalysis of the Au-bipy-Cu composite catalyst for
selective electrochemical CO2RR to hydrocarbons or
oxygenated-hydrocarbons.
Figure 1.(a) Schematic illustration ofAu-bipu-Cu compositecatalyst.(b-d) TEM
images of(b) 8 nm Au NPs,(c) 50 nm wide Cu NWs and(d) Au-bipy-Cu-1/1.(e)
HRTEM image ofa local area ofAu-bipy-Cu-1/2.
8 nm Au NPs and 50 nm wide Cu NWs were specifically selected
to make Au-bipy-Cu as the Au NPs have been demonstrated to
be efficient for CO2 reduction to CO[2a] and 50 nm wide Cu NWs
were more selective for CO reduction to C2-hydrocarbons.[5]
Monodispersed 8 nm Au NPs were synthesized by reduction of
HAuCl4 with borane tert-butylamine complex in a solution mixture
of oleylamine and 1,2,3,4-tetrahydronaphthalene as reported.[2a]
50 nm wide Cu NWs were synthesized by reduction of CuCl with
oleylamine at 180°C, which was modified from the reported
method.[6] Transmission electron microscopy (TEM) images of 8
nm Au NPs and 50 nm wide Cu NWs are shown in Figure 1b&c
respectively. To prepare Au-bipy-Cu, Cu NWs or Au NPs was
dispersed in a chloroform solution of 100 mM bipy and the mixture
was stirred at room temperature for 12 h (to prepare Cu-bipy) or
6 h (to prepare Au-bipy). Then the Au-bipy and Cu-bipy were
mixed together in chloroform at 25°C and stirred for 6 h to obtain
Au-bipy-Cu. The mass ratio of Au/Cu in the Au-bipy-Cu was
controlled by the amount of Au NPs and Cu NWs added in the
assembly process, and was determined by inductively coupled
plasma - atomic emission spectroscopy (ICP-AES). We foundthat
in the Au/Cu mass ratios between 1/1 – 1/3, the Au NPs and Cu
NWs were all included in the final Au-bipy-Cu composites.
Therefore, we denote the composites as Au-bipy-Cu-1/1 (Figure
S1a), Au-bipy-Cu-1/2 (Figure 1d), and Au-bipy-Cu-1/3 (Figure
S1b) respectively. As a comparison, simply mixing Au NPs and
Cu NWs without the bipy treatment gave only the random mixture
of NPs and NWs (Figure S2). High-resolution TEM (HRTEM)
[a]
[b]
J. Fu, Dr. W. Zhu,Z. Yin, Y. Li, Dr. H. Zhang and Prof. S. Sun
DepartmentofChemistry
Brown University
Providence,RhodeIsland 02912,United States
E-mail:ssun@brown.edu
J. Fu, Y. Chen,J.Liu and Prof. J. J. Zhu
State Key LaboratoryofAnalytical Chemistryfor Life Science
School ofChemistryand Chemical Engineering,
Nanjing University
Nanjing 210023,China
E-mail:jjzhu@nju.edu.cn
[‡]
These authors contribute equallyto this work.
Supporting information for this article can be found under:
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10.1002/anie.201905318
Angewandte Chemie International Edition
COMMUNICATION
image of the Au-bipy-Cu-1/2 (Figure 1e) shows that after Au NP
coupling to Cu NW via bipy, the lattice spacing of Au (111) and
Cu (111) are measured to be 0.24 and 0.21 nm respectively,
which are very close to that of face-centered cubic (fcc) Au (111)
(0.235 nm) and fcc Cu (111) (0.209 nm), indicating that the
coupling between Au NPs and Cu NWs via bipy does not affect
NP/NW lattice structures.
The successful exchange of oleylamine with bipy on the NP and
NW surfaces was characterized by infrared (IR) and ultra-violet-
visible (UV-Vis) spectroscopy. IR spectra of the Au NPs and Cu
NWs afterthe surfactantexchange show characteristicabsorption
peaks of bipy in 1400~1600 cm-1 (C=N, C=C stretching) and 3000
cm-1 (C-H stretching) (Figure S3).[7] The UV-Vis spectra show
strong absorption of 4, 4’-bipyridine at 265 nm from free bipy, Cu-
bipy and Au-bipy, not from the as-synthesized Cu NWs (Figure
S4). The plasmonic absorption peaks of Au NPs at 526 nm and
Cu NWs at 570 nm (Figure 2a) are unchanged upon the
replacement of oleylamine by bipy. However, once Au NPs are
landed on the Cu NW surface, the 570 nm Cu peak shifts slightly
to 567 nm and Au NP plasmonic absorption becomes invisible
due likely to the plasmonic coupling between Au and Cu,[8]
indicating that Au and Cu are strongly coupled via bipy in the Au-
bipy-Cu structure.
Figure 3. (a) LSV curves of Au-bipy-Cu catalysts in N2/CO2-saturated 0.1 M
KHCO3 solution and Au-bipy,Cu-bipyin CO2-saturated 0.1 M KHCO3 solution.
(b) CO product FE of Au-bipy-catalyzed CO2RR at different potentials. (c)
Product FEs of Cu-bipy-catalyzed CO2RR at different potentials. (d) Total FEs
of Au-bipy-Cu-catalyzed CO2RR at different potentials. (e) Product FEs of Au-
bipy-Cu-1/2-catalyzed CO2RR at different potentials. (f) FE of liquid products
obtained from Au-bipy-Cu-1/2-catalyzed CO2RR.
Linear scan voltammetry (LSV) measurements of Au-bipy, Cu-
bipy, and Au-bipy-Cu catalysts in N2- or CO2-saturated 0.1 M
KHCO3 (Figure 3a) show these catalysts induce higher
reduction currents at lower reduction potentials in the CO2-
saturated solution. The CO2RR catalyzed by Au-bipy produces
CO with over 80% FE in −0.7 ~ −0.9 V (Figure 3b), similar to
what was reported on Au NP catalysis for the CO2RR to CO.[2a]
This indicates that the modification of Au NPs with bipy does
not change the CO2RR selectivity of the 8 nm Au NPs. As a
comparison, the Cu-bipy is less selective and its CO2RR
catalysis yields CO (<12% FE) and formate (<15% FE), as well
as C2H4 (<5%) in −0.6 ~ −1.1 V (Figure 3c).Ata more negative
reduction potential −1.2 V or beyond, the reaction selectivity is
tuned more towards C2H4 with the FE increased steadily to
23% at −1.5 V, which is similar to what was observed in Cu
NW-catalyzed CO2RR.[5] The Au-bipy-Cu shows very different
CO2RR activity and selectivity from either Au-bipy or Cu-bipy.
First, the composite catalyst shows the Au/Cu mass ratio-
dependent catalysis, and Au-bipy-Cu-1/2 is the most active
catalyst for the CO2RR in all reduction potentials studied
(Figure 3d).Second, the Au-bipy-Cu-1/2 catalyzes the CO2RR
with an overall FE of C-products reaching 90.6% with the
products containing CO, HCOO−, CH4, C2H4, CH3CHO, and
CH3COO− (Figure 3e). To confirm all these carbons are from
CO2, not from bipy attached to the composite catalyst, we
performed electrochemical reduction of 13CO2 and the
Figure 2. (a) UV-Vis spectra of Au-bipy, Cu-bipy, and Au-bipy-Cu. (b) CVs of
Cu NWs,Cu-bipy,Au-bipy-Cu in N2-saturated 0.1 M KHCO3 and Au-bipy-Cu in
CO2-saturated0.1 M KHCO3.
Electrochemical properties of the carbon-supported Au-bipy-Cu
were studied by cyclic voltammetry (CV) (see the Supporting
Information for sample preparation). Figure 2b shows the CVs of
Cu, Cu-bipy, and Au-bipy-Cu in N2- and CO2-saturated 0.1 M
KHCO3 (Au NPs have no redox peaks in the potential range we
studied, Figure S5). Cu NWs have two typical reduction peaks at
0.5 V (Cu(II)/(Cu(I)) and 0.3 V (Cu(I)/Cu(0)).[9] When bipy binds to
the Cu surface, both peaks shift cathodically to 0.47 V and 0.25 V
respectively, and the Cu(I)/Cu(0) peak becomes weak and broad.
When Cu-bipy is further modified with Au, as in Au-bipy-Cu, the
Cu(I)/Cu(0) peak disappears. These indicate that the presence of
bipy stabilizes Cu(II) and Cu(I) states more efficiently via the bipy
bonding and shifts the Cu(I)-bipy reduction center from Cu(I) to
bipy, which is further enhanced by Cu-bipy-Au interaction. These
CV studies support what we have observed in the UV-Vis studies
that bipy plays an important role in coupling Cu with Au in the Au-
bipy-Cu structure. In the CO2-saturated 0.1 M KHCO3, the
Cu(II)/Cu(I) peak shifts further cathodically and higher current is
generated due to the CO2RR involved in the scanning process
(Figure 2b).
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10.1002/anie.201905318
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COMMUNICATION
representative 13C-products of CH3CHO, HCOO-, and
CH3COO- were characterized by negative electrospray
ionization (ESI) high performance liquid chromatography-mass
spectrometry (HPLC-MS) and 1H nuclear magnetic resonance
(1H NMR) spectroscopy (Figure S7). The peak of m-1/z = 45
can be assigned to 13C-labelled CH3CHO, and that of m/z = 46
or 61 is from 13C-labelled HCOO- or CH3COO- (Figure S7a).
The presence of 13C in HCOO- is further evidenced by
presence of a proton doublet in the NMR spectrum of HCOO-,
which is the result of the H-13C coupling (Figure S7b). These
support that the carbon source of the CO2RR products is from
CO2.[10] An interesting catalysis feature of the Au-bipy-Cu-1/2
is that at −0.5 V, the main product is CO (65% FE) due to the
Au-catalyzed CO2RR, and at more negative reduction
potentials, Cu NWs are activated and CO FE is reduced,
leading to the formation of multi-carbon products among which
C2H4 and CH3CHO (as confirmed by 1H NMR (Figure S6) are
the main gasand liquid products respectively,which is different
from the CO reduction reaction on thepure Cu NWs where only
gaseous C2-hydrocarbons (C2H4 + C2H6, 60% FE) were
obtained.[5] The liquid products contain HCOO−, CH3CHO, and
CH3COO− (Figure 3f), and CH3CHO (25% FE) dominates the
product distribution (75%), which is the highest aldehyde
selectivity ever reported for the electrochemical reduction of
CO2 or CO.[3e, 11] During 6 h of continuous CO2RR at -0.9 V, we
saw no current density drop from 13 mA·cm-2 (Figure S8) and
the reaction FE stayed at 80%.
total FE reaching 90.6%. Among three different liquid products
(HCOO−, CH3CHO, and CH3COO−) generated from the
CO2RR, CH3CHO has a FE fraction of 75%, the highest
selectivity ever reported for the electrochemical CO2RR to
aldehyde. The enhanced CO2RR catalysis of the Au-bipy-Cu
originates from the synergistic effects among Au (for CO2 to
CO), Cu (for CO coupling) and bipy (for the CO2* stabilization
and protonation). The assembly strategy demonstrated here
can be easily extended to prepare many other composite
catalysts, making it possible totune and optimize their catalysis
for CO2RR to specific hydrocarbons or oxygenated
hydrocarbons.
Acknowledgements
The work at Brown University was supported by the American
Chemical Society Petroleum Research Fund (57114-ND5) and in
part by the Center for the Capture and Conversion of CO2, a
Center for Chemical Innovation funded by the National Science
Foundation, CHE-1240020. We thank the International
CooperationFoundation from Ministry of Science and Technology
of China (2016YFE0130100), National Natural Science
Foundation of China (21834004) and the program B for
Outstanding PhD candidate of Nanjing University (Nos.
201801B024 and 201801B025) for support. The authors would
like to thank Chuan Chai at Nanjing University of Chinese
Medicine for the help on HPLC-MS analysis.
The Au-bipy-Cu catalyzed CO2RR shows Au/Cu mass ratio
dependent catalysis. The CO2RR catalyzed Au-bipy-Cu-1/1
yielded only CO and H2 (Figure S9).Thepresenceof too many
Au NPs shields the surface of Cu NWs, making the Au-bipy-
Cu less effective as a composite catalyst for the CO2RR. On
the other hand, when the Au NPs are anchored only on a
fraction of Cu NWs, as in Au-bipy-Cu-1/3, the CO2RR process
is complicated and the products containmore C1 (FE of < 30%)
than C2 products (FE < 15%) (Figure S10).
Keywords: Electrocatalysis • CO2 reduction • Nanoparticles •
keyword 4 • keyword 5
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COMMUNICATION
COMMUNICATION
The electrochemical reduction of CO2
to hydrocarbons is enhanced by
assembling Au nanoparticles and Cu
nanowires via bipyridine, which
provide the synergistic effects among
Au (for CO2 to CO), Cu (for CO
coupling) and bipy (for the CO2*
stabilization and protonation).
Jiaju Fu, Wenlei Zhu, Ying Chen,
Zhouyang Yin, Yuyang Li, Juan Liu,
Hongyi Zhang, Jun-Jie Zhu* and
Shouheng Sun*
Page No. – Page No.
Bipyridine-assisted assemblyof Au
nanoparticles on Cu nanowires to
enhance electrochemical reduction of
CO2
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