Cuprous Sulfide Nanoarrays for Selective
Electroreduction of CO2 to Formate at Low Overpotentials
Item Type Article
Authors Cai, Siting;Wang, Mengdi;Chen, Bin;Xu, Xin;Mi, Linhua;Li, Borong;Yang, Chengkai;Li, Liuyi;Zhong, Shenghong;Yu, Yan Citation Cai, S., Wang, M., Chen, B., Xu, X., Mi, L., Li, B., Yang, C., Li, L.,
Zhong, Prof. S., & Yu, Y. (2022). Cuprous Sulfide Nanoarrays for Selective Electroreduction of CO2 to Formate at Low Overpotentials. Chemical Engineering Journal Advances, 12, 100383. https://doi.org/10.1016/j.ceja.2022.100383
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Cuprous Sulfide Nanoarrays for Selective Electroreduction of CO 2 to Formate at Low Overpotentials
Siting Cai
a, Mengdi Wang
a, Bin Chen
a, Xin Xu
a, Linhua Mi
a, Borong Li
a, Chengkai Yang
a, Liuyi Li
a, Prof. Shenghong Zhong
a,b,*, Yan Yu
a,*aKey Laboratory of Advanced Materials Technologies, International (HongKong Macao and Taiwan) Joint Laboratory on Advanced Materials Technologies, College of Materials Science and Engineering, Fuzhou University, Fuzhou 350108, China
bPhysical Science and Engineering Division, King Abdullah University of Science and Technology (KAUST), Thuwal 23955-6900, Kingdom of Saudi Arabia
A R T I C L E I N F O Keywords:
Cuprous sulfide CO2 reduction Formate Electro-catalysis Carbon dioxide
A B S T R A C T
Transformation of carbon dioxide to useful fuels or chemicals is desirable to build up a sustainable society. In this study, we demonstrate that Cu2S has great potential for electrochemical CO2 reduction. They enable the selective CO2 reduction to formate starting at a low overpotential (~ 120 mV), with high current density (over -20 mA/
cm2 at -0.89 VRHE), and good Faradaic efficiency (>75%) over a broad potential window (-0.7 VRHE to -0.9 VRHE).
X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and in-situ Raman spectroscopy studies reveal that Cu2S catalysts are electrochemically stable under the reaction conditions. Further-more, Cu2S catalysts show excellent durability without deactivation following more than 15 cycles (1.0 h per cycle) of operation.
1. Introduction
Transformation of carbon dioxide to useful fuels or chemicals is desirable to build up a sustainable society. Electrochemical conversion of CO2 to value-added feedstocks or fuels is considered an attractive strategy to address the twin problems of fossil fuel depletion and envi- ronmental challenges [1–9]. This process is promising due to its mild reaction conditions [10,11], however, product selectivity, energy effi- ciency, and catalytic activity remain challenges [12–14]. Regardless of the product, this conversion process generally requires a catalyst. Inor- ganic heterogeneous electrocatalysts have stimulated more and more interests, due to their environmental friendliness, outstanding effi- ciency, facile synthesis, and great potential for large-scale applications [15]. Copper is the hottest electrocatalyst for this reaction, not only owning to it is structurally simple, easy to handle, and robust, but also because it is the only transition metal that can produce hydrocarbons and oxygenates with acceptable Faradaic Efficiency (FE) [16]. However, copper usually converts CO2 into a mixture of carbon-containing prod- ucts, where more than 16 species have been identified [17].
Copper-based catalysts also suffer from other drawbacks, such as high overpotentials [18,19] and significant hydrogen evolution reaction (HER) competition [20–22]. Recently, a lot of efforts have been made to improve the catalytic performance of Cu-based catalysts. Better product
selectivity, lower activation overpotentials, and higher current density have been achieved via tuning of catalyst morphologies [4,5,20], manipulation of oxidation states [23–25], introduction of dopants [26], increasing of grain boundaries [21,27], formation of alloys [28–30], redesign of devices [19], modification of surfaces [6,31], and engi- neering of electrolytes [11,32]. For instance, Wang and coworkers re- ported a Cu2O/CuS nanocomposites catalyst that shows a low onset potential of − 0.5 V vs RHE and exhibits excellent FE of formate of 67.6%
and a jHCOO− value of 15.3 mA/cm2 at − 0.9 V vs RHE. They found that the presence of CuS stabilizes Cu2O for CO2RR, because of the favorable band alignment [33].
Various electrocatalysts (Pb, Cd, Hg, In, Sn, and Bi) have been found to selectively reduce CO2 to formate [34–36], a potential first com- mercial product from CO2RR [13,37]. However, Pb, Cd and Hg are toxic and not suitable for real applications. The relatively low global reserve of In, Bi, and Sn and their uneven distribution on the Earth result in a high price. In contrast, Cu is an Earth abundant element that has a considerably lower price [33]. Recently, electrocatalysts based on sulfide-derived copper have attracted a lot of interests. Unlike most of Cu-based catalysts produce a mixture of carbon-containing chemicals, sulfide-derived (or sulfur doped) copper produce formate as an exclusive CO2RR product at low overpotentials [12,38–42], making it an outstanding candidate for producing formate. Sulfide-derived Cu for
* Corresponding author.
E-mail addresses: [email protected] (Prof.S. Zhong), [email protected] (Y. Yu).
Contents lists available at ScienceDirect
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https://doi.org/10.1016/j.ceja.2022.100383
Received 5 June 2022; Received in revised form 10 August 2022; Accepted 11 August 2022
Chemical Engineering Journal Advances 12 (2022) 100383
2 CO2RR to produce formate was first reported by Zhu et al. in 2016, a FEformate of 85% was achieved in a 0.5 M 1-butyl-3-methylimidazolium tetrafluoroborate (BmimBF4) in acetonitrile (MeCN) electrolyte [42].
Later on, a few works in aqueous electrolyte were published. A maximum 70%~80% Faradaic efficiency toward formate at − 0.8 VRHE
~0.9 VRHE was reported by different groups [38,39,41]. However, sulfide-derived copper catalysts are usually prepared by in situ electro- reduction of CuS, the resulted catalysts contain S, metallic Cu, CuS, Cu2O, Cu2S and CuSO4. Such complicated components make it difficult to figure out the active species that accounts for the tuned selectivity [38]. Considering the amount of Cu2S increased after CO2RR in CuS-derived Cu catalyst system [38] and the fact that Cu2S is stable under a potential not more negative than -0.9 VRHE [38,40]. We hy- pothesized that Cu2S is active for CO2RR thus the promoted formate selectivity in CuS-derived Cu catalysts may be ascribed to the formation of Cu2S. Herein, Cu2S nanoarrays were prepared and their CO2RR per- formance was evaluated (Table 1) to verify the hypothesis.
2. Experimental section 2.1. Materials
Copper foil (0.25 mm thick, 99.98% trace metal basis), copper wire (99.9%), potassium bicarbonate (99.95%), sodium hydroxide (97%), deuterium oxide (99.9 atom % D), ethanol (98%), dimethyl sulfoxide (99.7%), formic acid (95%) were purchased from Sigma-Aldrich. Carbon dioxide (99.99%), Hydrogen sulfide (99.5%), Nitrogen (99.99%), Argon (99.99%), and Helium (99.99%) were purchased from Air Liquide. All potentials were measured against an Ag/AgCl reference electrode (3.0 M KCl, World Precision Instruments).
2.2. Preparation of Cu2S catalysts
Cu2S catalysts were prepared by a vapor sulfurization method. A pristine Cu foil was first electropolished in a 1M NaOH solution for 30 min at a current density of 10 mA cm−2, then the polished Cu foil was put inside a horizontal quartz tube for sulfurization. During the sulfu- rization process, a pure N2 flow of 500 mL/min was first introduced into the tube for 4 min. Then the N2 flow was replaced by an H2S gas flow of 200 mL/min for 5 min. The tube was subsequently sealed and kept under the H2S atmosphere at room temperature for 16 h.
2.3. Catalysts characterization
The morphology of the catalysts was observed by an FEI Nova Nano
630 Scanning Electron Microscopy (SEM). X-ray diffraction (XRD) pat- terns were recorded by a Bruker D2-phaser desktop diffractometer.
Samples for TEM measurements were suspended in ethanol and dispersed ultrasonically. Drops of suspensions were applied on a copper grid coated with carbon. High-resolution transmission electron micro- scopy (HRTEM) was performed on a FEI Titan 60-300 electron micro- scope under 300 kV. HAADF-STEM images were obtained on FEI Titan 60–300 Microscope operated at 300 kV. And elemental mapping anal- ysis was collected by the TEM equipped with an energy-dispersive X-ray spectroscope (EDS). X-ray photoelectron spectroscopy (XPS) was con- ducted using a Kratos Axis Ultra DLD spectrometer equipped with a monochromatic Al Kα X-ray source (hν=1486.6 eV) operating at 150W, a multi- channel plate and delay line detector under a vacuum of 1*10−9 mbar. The survey and high-resolution spectra were collected at fixed analyzer pass energies of 160 and 20 eV, respectively. Binding energies were referenced to C1s peak at 284.8 eV (sp3 hybridized carbon). In-situ Raman spectrum were recorded on a Bruker SENTERRA Raman spec- trometer, operating at 50 ×magnification. Cu2S catalysts were excited with a 532 nm laser.
2.4. Catalysts evaluation
All the electrochemical experiments were carried out in an air-tight, glass frit-separated two-compartment, three-electrode electrochemical cell using a Biologic VMP-300 potentiostat. All the applied potentials are reported as RHE potentials scale, unless otherwise stated. IR compen- sation was conducted manually, where the cell resistance was evaluated by Electrochemical Impedence Spectroscopy (EIS). During the electro- chemical reduction, as prepared Cu2S catalysts were used as working electrode. A carbon rod and an Ag/AgCl in saturated KCl were used as counter and reference electrodes, respectively. And CO2 gas was continuously bubbled into the cathodic compartment at a rate of 10 mL/
min. The eluent was delivered directly to the sampling loop of an online pre-calibrated gas chromatograph (Agilent 7890B) which was equipped with two TCD channels. The Faradaic efficiencies (FEs) of products were calculated as below:
εFaradaic=αnF Q
where α is the number of electrons transferred (α =2 for formate); n is the number of moles of the product, which is calculated from its con- centration in the electrolyte as determined by NMR (formate) or from an online GC (CO and H2); F is the Faraday constant (96,485 C⋅mol−1); Q represents all the charge passed throughout the process and it is calcu- lated by the integration of the i-t curve.
After 1 hour reduction, the liquid products were collected from electrolyte and analyzed using a Bruker AV-III 700MHz liquid 1H-NMR spectrometer. A small amount of dimethyl sulfoxide (DMSO) in D2O was sealed in a coaxial insert as an external reference. After calibration of the external reference with standard product solution, NMR tubes were then rinsed with deionized water and the collected electrolyte for three times.
500 µL solution were transferred into NMR tube for analysis. During the NMR analysis 64 cycles of scan were performed, and peaks shift were recorded, peaks area (DMSO was always set as 1) were calculated as an index of their amount.
3. Results and Discussion
Cu2S were prepared by a vapor sulfurization method [43], as shown in Figure 1a. Cu foil was first electropolished in a 1M NaOH solution (Figure S1), then the polished Cu foil (Figure S2) was put inside a horizontal quartz tube for sulfurization. XRD pattern in Figure 1b proves that crystalline Cu2S was synthesized successfully. The two intensive peaks at 43.4 and 50.5 were generated from the Cu foil (111) and (200) facets, respectively. Figure 1c shows SEM (scanning electron Table 1
An overview of sulfur modified Cu-based catalysts showing high selectivity of conversion CO2 to formate.
Catalysts Electrolyte Potential JHCOO−
(mA cm−2)
FE (%) Reference
Cu2S 0.1 M KHCO3 -0.71 VRHE
-7.63 75.4 This work Cu2S-
derived Cu
0.5 M BmimBF4
[a] in MeCN [b] -2.0 VAg/
Ag+ -5.3 85 Zhu et al.
[42]
S-modified
Cu 0.1 M KHCO3 -0.80
VRHE
~-7.3 ~80 Shinagawa et al. [38]
CuS- derived Cu
0.1 M KHCO3 -0.80 VRHE
-2.5 ~60 Phillips et al.
[12]
S-doped Cu 0.1 M KHCO3 -0.80 VRHE
-10.7 74 Huang et al.
[41]
CuSx 0.1 M KHCO3 -0.90 VRHE
-9.0 75 Deng et al.
[39]
[a] Bmim =1-butyl-3-methylimidazolium. [b] MeCN =acetonitrile.
S. Cai et al.
Figure 1. a) Schematic illustration of synthetic procedure for Cu2S catalysts. b) XRD pattern of as prepared Cu2S catalysts. c) SEM image of Cu2S catalysts, lots of grain boundaries are generated. Insert of (c) shows the nanoarray structure.
Figure 2.TEM images of the as prepared Cu2S nanoarrays at different resolutions (a, b, c, d), EDS elemental mapping images (e, f, g).
Chemical Engineering Journal Advances 12 (2022) 100383
4 microscope) images of synthesized Cu2S, at different resolutions, illus- trating a lot of domains (at the size of a few micrometers) formed on Cu surface. The insert of Figure 1c shows Cu2S nanoarrays structures (small grey dots) uniformly deposited on the surface of Cu foil.
TEM (Figure 2) was used to investigate the morphology and intrinsic structure of the Cu2S nanoarrays. Figure 2a, b, c and d show TEM im- ages of Cu2S nanoarray at different resolution. The TEM images clearly show a nanorod with length of a few hundreds nanometers and the diameter around 75 nm. The spacing of the lattice fringes from a high- resolution TEM (HRTEM) image (Figure 2c) is ~3.2 Å, which corre- sponds to the (222) plane of low-chalcocite Cu2S [44]. The selected-area electron diffraction (SAED) pattern (the inset of Figure 2c) further confirms that Cu2S nanoarray is single-crystalline. The EDS elemental mapping images of the nanoarrays (Figure 2e and 2f) show that Cu and S are uniformly dispersed throughout the nanoarray. EDS image (Figure 2g) shows the presence of copper and sulphur in the sample, a small amount of oxygen is also detected.
XPS (Figure 3) was further conducted to confirm the surface chemical state and composition of the as-prepared Cu2S catalysts. As shown in Figure 3a, Cu, O, S, and C elements were found in the survey scan spectrum. The atomic percentage of Cu and S was calculated to be 45.1% and 23.8%, respectively. A small Na signal was found, which may be introduced during handling. The S 2p can be divided into two peaks of 2p3/2 and 2p1/2 at the position of 161.3 and 162.5 eV, respectively (Figure 3b) [45]. The S 2p spectrum also shows a little bit oxidation of the sulfide to sulfate (binding energy 167.1 eV) [46]. The Cu 2p3/2, shows a single peak at 931.9 eV (Figure 3c), can be assigned to the Cu+/Cu state [45]. The fitting peak from Cu 2p1/2 at about 951.8 eV and Cu LMM Auger electrons from X-ray-induced Auger electron
spectroscopy (XAES) at around 917 eV shown in Figure 3d coincide well with that of cuprous cation [47]. These results clearly demonstrate that the as-prepared nanoarrays on Cu foil surfaces are cuprous sulfide.
Electrocatalytic CO2 reduction by Cu2S (Figure 4a, b, c) and elec- tropolished Cu foil (Figure 4d, e, f) was evaluated in CO2-saturated 0.1 M KHCO3 aqueous solutions. Figure 4a shows the total current density of Cu2S at various potentials range from -0.32 VRHE to -0.89 VRHE, cur- rent density increased with more negative potential applied. Products distributions was shown in Figure 4b, hydrogen (H2), carbon monoxide (CO), and formate (HCOO−) were detected. The selectivity of CO increased with more negative potentials applied, but never exceeded 0.6%, which suggests Cu2S do not favor the production of CO. The FE of H2 decreased from 80.8% to 24.1% as the potentials increased from -0.32 VRHE to -0.71 VRHE, whereas the FE of HCOO− increase from 2.6%
to 75.4%. With more negative potentials applied, the FE of both H2 and HCOO− did not change significantly. The above results suggest that Cu2S can act as an efficient CO2RR electrocatalyst for the conversion of CO2 to formate with high activity and selectivity over a broad potential win- dow. We also noticed that formate start to appear at very low potential (only -0.32 VRHE), the standard equilibrium potential for the reduction of CO2 to formic acid is -0.20 VRHE [41], corresponding to an over- potential of 120 mV. The maximum FEformate (75.4%) was achieved at -0.71 VRHE, with an overpotential of ~ 0.5 V, which is much lower than most of other formate-selective electrocatalysts (Pb, Cd, Hg, In, Sn, and Bi), where an overpotential of ~ 1 V is usually required. The partial current density of formate was increased with potential also, and rea- ches -7.6 mA cm−2 and -16.1 mA cm−2 at -0.71 VRHE and -0.89 VRHE, respectively (Figure 4c). As a comparison, CO2RR performance of electropolished Cu foil was also evaluated at similar potential range. The
Figure 3. XPS spectra of the as prepared Cu2S nanoarrays: (a) survey spectrum, Cu and S ratio is around 2:1, (b) S 2p, (c) Cu 2p, and (d) Cu LMM.
S. Cai et al.
total current density (Figure 4d) is much lower than that of Cu2S nanoarrays. It shows almost no CO2RR activity with H2 as a dominant product, only very small amount of HCOO− and CO were produced at potentials more negative than -0.76 VRHE (Figure 4e). Thus, a low partial current density of formate was expected, which is lower than 0.1 mA cm−2 at -0.92 VRHE (Figure 4f). The above results indicate that upon sulfurization the selectivity and activity of CO2 conversion into formate was greatly improved.
Cu2S catalysts were also characterized after 1h’s CO2 reduction re- action (CO2RR) at -0.74 VRHE. After CO2RR, Cu2S catalysts were removed from 0.1 M KHCO3 electrolyte and flushed with large amount of deionized water, subsequently dried in a vacuum storage box. After dried overnight, XRD, XPS and SEM were applied to study the crystalline structure, surface chemical states and morphology of Cu2S after CO2RR.
From the XRD pattern (Figure S3) of Cu2S after CO2RR (vacuum dried), the presence of characteristic peaks of Cu2S suggesting Cu2S is stable under our CO2RR conditions. The stability of Cu2S in 0.1 M KHCO3 electrolyte under Ar at -0.8 VRHE was also tested (Figure S4a). The characteristic peaks of Cu2S in XRD pattern (Figure S4b) of catalysts after electrolysis (vacuum dried) further supported the argument that Cu2S is stable under our CO2RR experiment conditions. We also observed Cu2O peaks, which may be introduced by the oxidation of Cu foil during the drying process. To verify this hypothesis, we also examined the XRD of a Cu2S sample after CO2RR in an open circuit (under CO2RR conditions but without applying any potential), the characteristic crystalline peaks of Cu2O were observed (Figure S5), which further supports the argument that Cu2O was introduced during drying, coincided with previous report [44]. The XPS spectra of Cu2S after CO2RR as shown in Figure S6 also confirm the presence of Cu2S at Cu foil surface. The above XRD together with the XPS results demon- strate that Cu2S is stable under our CO2RR condition, which is also in line with previous reports [38,40]. Furthermore, we performed in-situ Raman experiments (Figure S7) on Cu2S catalysts under CO2 reduction conditions at -0.8 VRHE for 1 hour. The characteristic Raman features for Cu2S were observed (Figure 6d) during electrochemical CO2 reduction
reaction (sharp peak at 472 cm−1) [48,49], which provides direct evi- dence for that Cu2S is stable under our CO2RR condition. From the SEM images after CO2RR (Figure S8), the morphology of Cu2S nanoarrays changed significantly, which is common for Cu-based catalysts [6]. We further evaluated the catalytic performance of the above mentioned vacuum-dried catalysts. The results in Figure S9 clearly shown that vacuum dried catalysts maintain the high selectivity of formate, which is similar to the as-prepared Cu2S catalysts, indicating that the morphology of Cu2S catalysts does not play an important role in CO2RR.
The duribility (stability) of Cu2S catalysts were also tested. The test were conducted at -0.81VRHE in CO2-saturated 0.1 M KHCO3 electrolyte.
The test were run for 15 cycles (1h per cycle), after each cycle, the electrolyte was collected for NMR analysis to find out the formate for- mation rate and FE, and the electrolyte was re-freshed for another cy- cle’s test. As shown in Figure 5a, during the 15 cycles’ tests, the total current density was stabled at around -12 mA cm−2. The FE of formate was also stable during the test, which is fluctuated around 70%
(Figure 5b, Table S1). Subsequntly, a stable formate formation rate of
~ 4.3*10−5 mol s−1 cm−2 was achieved (Figure 5b). These results prove that Cu2S catalysts are very stable for CO2RR, after running for 15h, there is no significant change in their activity and selectivity.
It’s also very critical to find out whether the sulfurization duration during Cu2S preparation process will affect the formate selectivity or not. Apart from previous tested 16h’s sulfurization, we tried both shorter (1h and 4h) and longer (64h) sulfurization durations. Their CO2RR performance at -0.71 VRHE was shown in Figure 5c. It is obvious that high formate selectivity were achieved in all four cases, and the FEformate of 4h and 16h duration is slightly higher than that of 1h and 64h, which indicates that sulfurization duration has little effect on formate formation selectivity of Cu2S catalysts.
DFT calculation was applied to explore the selectivity of Cu2S cata- lysts at -0.90 VRHE. The Gibbs free energies of the formate production pathway via HCOO* intermediate and CO production pathway via COOH* intermediate on Cu2S (111) surfaces are presented in Figure 6.
At -0.90 VRHE, an energy barrier of 0.23 eV was observed when CO2 Figure 4. CO2RR performance of Cu2S catalysts (a, b, c) and electropolished Cu foil (d, e, f): (a, d) Current density under various potentials, (b, e) Faradiac efficiency, (c, f) Partial current density of formate and Tafel slop.
Chemical Engineering Journal Advances 12 (2022) 100383
6
protonated to COOH*, while the HCOO* formation step is exergonic.
Hence, the first protonation determines the high formate selectivity with respect to CO production.
4. Conclusions
In summary, we have successfully developed cuprous sulfide nano- arrays catalysts via a vapor sulfurization process. Cu2S catalysts are capable to selectively and efficiently reduce CO2 to HCOO− at low overpotentials, with high current density (over -20 mA/cm2 at -0.89 VRHE), and good Faradaic efficiency (>75%) over a broad potential window. Our study demonstrates a simple vapor-assisted approach for the development of copper chalcogenide CO2RR catalysts.
Funding Information
This work was supported primarily by National Key Research and Development Program of China (2020YFA0710303). The authors thank the support from National Natural Science Foundation of China (No.
U1905215, 51672046, 51672047 and 22109025), Natural Science Foundation of Fujian Province, China (2021J01230192), Scientific Research Foundation of Fuzhou University (510936) and King Abdullah University of Science and Technology.
Figure 5.(a) Current density of the 15 cycles’ durability test at -0.81 VRHE, (b) Faradaic efficiency and yield of formate during the durability test, (c) Sulfurization duration effect, (d) In-situ Raman Spectroscopy of Cu2S catalysts during electrochemical CO2 reduction at -0.8VRHE.
Figure 6. Free energy diagrams for the competition between CO2RR producing formate and CO at -0.90 VRHE.
S. Cai et al.
Declaration of Competing Interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgements
This work was supported primarily by National Key Research and Development Program of China (2020YFA0710303). The authors thank the support from National Natural Science Foundation of China (No.
U1905215, 51672046, 51672047 and 22109025), Natural Science Foundation of Fujian Province, China (2021J01230192), Scientific Research Foundation of Fuzhou University (510936) and King Abdullah University of Science and Technology.
Supplementary materials
Supplementary material associated with this article can be found, in the online version, at doi:10.1016/j.ceja.2022.100383.
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