Highly effective electrochemical water oxidation by copper oxide film generated in situ from Cu(II) tricine complex

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1 Chinese Journal of Catalysis 39 (218) 催化学报 218 年第 39 卷第 3 期 available at journal homepage: Article (Special Issue of Photocatalysis for Solar Fuels) Highly effective electrochemical water oxidation by copper oxide film generated in situ from Cu(II) tricine complex Yan Gao *, Hu Chen, Lu Ye, Zhongkai Lu, Yanan Yao, Yu Wei, Xuyang Chen State Key Laboratory of Fine Chemicals, Institute of Artificial Photosynthesis, DUT KTH Joint Education and Research Center on Molecular Devices, Dalian University of Technology (DUT), Dalian 11624, Liaoning, China A R T I C L E I N F O A B S T R A C T Article history: Received 28 October 217 Accepted 2 November 217 Published 5 March 218 Keywords: Water oxidation Oxygen evolution reaction Electrodeposition Copper oxide film Electrocatalyst Developing highly efficient and stable water oxidation catalysts based on abundant metallic elements is a challenge that must be met to fulfill the promise of water splitting for clean energy production. In this work, we developed an oxygen evolution reaction catalyst consisting of a nanostructured film electrodeposited from a phosphate buffer solution (.2 mol/l, ph = 12.) containing Cu tricine complex. A Tafel plot showed that the required overpotential for a current density of 1. ma/cm 2 was only 395 mv and the Tafel slope was 46.7 mv/decade. In addition, the Cu tricine film maintained a stable current density of 7.5 ma/cm 2 for the oxygen evolution reaction in phosphate buffer solution for 1 h, and a Faradaic efficiency of 99% was obtained. 218, Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved. 1. Introduction Increasing energy consumption and environmental pollution caused by burning of traditional fossil fuels have stimulated global efforts to develop clean energy alternatives to fossil fuels [1,2]. Water splitting, involving the cathodic hydrogen evolution reaction and anodic oxygen evolution reaction (OER), is considered to be a highly efficient method for producing renewable and clean hydrogen energy [3 7]. However, because of its intrinsically sluggish reaction kinetics and the requirement for a high overpotential, the OER is the limiting step in water splitting reactions [8,9]. The development of electrocatalysts with high OER activities is therefore needed to improve the reaction rate and reduce the overpotential. At present, complexes and oxides based on iridium and ruthenium are the best performing OER catalysts [1 16]. However, the scarcity and high cost of these noble metals greatly limits their large scale practical applications. It is therefore important to identify new efficient and cheap electrocatalysts for the OER. Recently, water oxidation catalysts based on non precious metals, such as cobalt [17 23], nickel [24 28], copper [29 4], iron [41 43], and manganese [44,45] have been reported. Because of their good redox properties and low cost, copper based electrocatalysts show great potential in various catalytic applications. Several Cu(II) based homogeneous catalysts for the OER have been reported in various buffered solutions with different phs, including Cu(II) bipyridyl [46,47] and Cu(II) polypeptide [48] complexes. Highly efficient, stable copper based heterogeneous electrocatalysts for the OER have also been reported and are listed in Table 1. In 214, Du s group [29] reported that heterogeneous copper oxide electrodeposited from copper tris(2 pyridylmethyl)amine was an active catalyst for the OER, with an overpotential of 6 mv (1. ma/cm 2 ). Du s group [31] also reported the use of an electro * Corresponding author. Tel: ; Fax: ; E mail: This work was supported by the National Basic Research Program of China (973 Program, 214CB23942), the National Natural Science Foundation of China ( ), and the Basic Research Project of Key Laboratory of Liaoning (LZ21515). DOI: 1.116/S (17) Chin. J. Catal., Vol. 39, No. 3, March 218

2 48 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) Table 1 Comparison of copper based heterogeneous electrocatalysts for water oxidation. Catalyst Electrolyte ph η (mv vs. 1. ma/cm 2 ) Tafel slope (mv/decade) Ref. CuO from Cu TPA Borate buffer.1 mol/l [29] Cu bifunctional Borate buffer.1 mol/l [31] CuO from Cu TEOA Acetate electrolyte.1 mol/l [39] Cu Bi Borate buffer.1 mol/l [32] CuO from Cu en PBS.2 mol/l [36] Annealed CuO KOH electrolyte 1. mol/l [4] Cu(OH)2 Borate buffer.1 mol/l [3] CuO from Cu Gly PBS.2 mol/l [33] CuO from Cu Tricine PBS.2 mol/l This work Note: Overpotential (η) values at 1. ma/cm 2 are determined from Tafel plots. deposited copper based film as a bifunctional catalyst; the catalytic overpotential was 749 mv (1. ma/cm 2 ) for the OER. In 215, Sun s group reported a robust copper oxide film[32], prepared by a simple electrodeposition of Cu 2+ from a borate buffer solution, which featured a current density of 1. ma/cm 2 at an overpotential of 53 mv in the OER. More recently, Chen s group [33,36] reported that CuO films electrodeposited from Cu en and Cu Gly complexes gave overpotentials of 55 and 45 mv, respectively, at a catalytic current density of 1. ma/cm 2 in.2 mol/l phosphate buffer solution (PBS, ph = 12.). 2. Experimental 2.1. Materials All chemical reagents used in this study, including CuSO4 5H2O, Na2HPO4 2H2O, NaOH, N [tris(hydroxymethyl) methyl] glycine (tricine), and Amberlite IRC 748 were purchased from commercial suppliers. The chemicals were of analytical reagent grade and used without further purification. Indium tin oxide (ITO ) coated glass slides were purchased from Zhuhai Kaivo Optoelectronic Technology Co., Ltd. (thickness ~1.6 mm, transmittance > 7%, resistance < 15 mω/cm 2 ). All aqueous solutions were prepared with Milli Q ultrapure water (>18 MΩ cm) unless stated otherwise. The ITO coated glass was washed by ultrasonication in aqueous detergent solution, acetone, ethanol, and deionized water for 3 min each, and then dried in an oven for future use Preparation of buffer solution The PBS (.2 mol/l, ph = 12.) was prepared by dissolving Na2HPO4 (.2 mol/l) in deionized water and the ph value of the solution was adjusted to 12. by addition of NaOH (solid). To rule out the influence of other metal impurity ions on the experiment, the PBS solution was washed with Amberlite IRC 748. The washing procedure for the electrolyte was as follows. First, the Amberlite resin was stirred for 45 min in ultrapure water and then filtered to remove any unbound iminodiacetic acid. After drying in air, 5. g of the cleaned Amberlite resin was added to 4 ml of electrolyte and the mixture was stirred for 5 min. In this time, the resin was removed by filtration and the electrolyte was reserved for further use Formation of Cu tricine complex The copper complex was formed in situ by adding an aqueous solution of ligand (1. ml of.3 mol/l tricine) to an aqueous solution of CuSO4 (1. ml,.3 mol/l) in molar ratio corresponding to the Cu/ligand stoichiometry of the final complex. The formation of the copper(ii) complex was confirmed by UV/Vis spectrophotometry. Immediately, prior to deposition, the solutions were diluted in PBS (.2 mol/l, ph = 12.) to form a 1. mmol/l Cu tricine complex in.2 mol/l PBS UV/Vis spectra Solution UV/Vis spectra of the Cu tricine complex were measured on a Varian 3 UV/Vis spectrophotometer in 1. cm cuvettes. The copper(ii) complex was diluted in PBS (.2 mol/l, ph = 12.) for analysis Preparation of Cu tricine catalyst films The electrodeposition of the Cu tricine films was performed in a two compartment electrochemical cell with a glass frit junction to separate the two compartments. In the auxiliary chamber, the counter electrode was immersed in 3. ml PBS (.2 mol/l, ph = 12.). In the working electrode compartment, an ITO coated glass electrode, with a 1. cm 2 electroactive area, was immersed in 3 ml PBS (.2 mol/l, ph = 12.) containing 1. mmol/l Cu tricine complex. An Ag/AgCl reference electrode was also immersed in the working electrode compartment. After controlled potential electrolysis for 6. h at 1.15 V (vs. normal hydrogen electrode (NHE)), without ir compensation or stirring, a layer of the catalyst film was formed on the ITO substrate Material characterization The morphology of the prepared Cu tricine films was observed with FEI Nova Nano SEM 45 instrument equipped with an energy dispersive X ray (EDX) analysis detector. Scanning electron microscope (SEM) images were obtained at an acceleration voltage of 3 5 kv and EDX spectra were obtained at accelerating voltages between 15 and 2 kv. Transmission electron microscopy (TEM) and high resolution TEM (HRTEM)

3 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) images were obtained with FEI TF3 equipment. The sample used for this measurement was carefully scraped off with the use of a doctor blade. The combined material was dispersed in absolute ethanol by ultrasonication, and a drop of the mixture was dried on a carbon coated copper grid for analysis. X ray diffraction (XRD) results were collected with a D/max 24 diffractometer. The measurements were performed from 1 to 9 at a scan rate of 8 /min. X ray photoelectron spectroscopy (XPS) was performed on a Thermo VG ESCALAB 25X. The results were obtained with the use of an aluminum anode (Al Kα = ev) operating at 15 W and a spot size of 5 µm. Typically, the hydrocarbon C 1s line at ev from adventitious carbon was used for energy referencing. Survey scans were measured at a constant pass energy of 5. ev Electrochemical studies All electrochemical experiments were performed at room temperature (25 ± 2 C) with a CH Instruments (model CHI 66E Electrochemical Analyzer). The electrochemical measurements were performed in aqueous solution (35. ml) with a conventional three electrode configuration: with the ITO (1. cm 2 ) and catalyst film as the working electrode, saturated Ag/AgCl (.2 V vs. NHE) as the reference electrode, and a Pt mesh as the auxiliary electrode. The reference electrode was calibrated against Ru(bpy)3 (1.26 V vs. NHE) before use. Cyclic voltammetry (CV) was performed in static PBS (.2 mol/l, ph = 12.) between.2 and 1.5 V vs. NHE (without ir compensation). The scan rate was 5 mv/s. Long term controlled potential electrolysis (CPE) was recorded in 35. ml PBS (.2 mol/l, ph = 12.) at 1.15 V vs. NHE in a fritted cell with gentle stirring. The Tafel plot of the Cu Tris film was constructed by measuring the steady state current density (after 12 s of electrolysis) with ir compensation in 25. ml PBS (.2 mol/l, ph = 12.) as a function of the applied overpotential. The solution was gently stirred during this experiment. The working electrode was prepared by depositing the Cu tricine film on 1. cm 2 ITO via CPE for 6 h at 1.15 V vs. NHE. The experimental setup was a single gas tight cell equipped with copper coated ITO (1. cm 2 active area) as the working electrode, Ag/AgCl as the reference electrode, and Pt mesh as the counter electrode in PBS (.2 mol/l, ph = 12.). First, the PBS was degassed by bubbling Ar for 1. h. Then electrolysis was performed at 6. ma/cm 2 without ir compensation in PBS (.2 mol/l, ph = 12.) for 3. h. The amount of oxygen evolved in the headspace was measured by a gas chromatograph (GC 789T instrument equipped Abs (a) 1 mmol/l Cu 2+ Cu 2+ /Tricine = 1/1 Cu 2+ /Tricine = 1/2 Cu 2+ /Tricine = 1/ (b) 1 mmol/l Cu 2+ Cu 2+ /Tricine = 1/1 Cu 2+ /Tricine = 1/2 Cu 2+ /Tricine = 1/ Wavelength (nm) 2.5 (c) 1 mmol/l Cu 2+ Cu 2+ /Tricine = 1/1 Cu 2+ /Tricine = 1/2 Cu 2+ /Tricine = 1/ Voltage (V vs. NHE) Voltage (V vs. NHE) (d) Bare ITO 1 mmol/l Cu 2+ 1 mmol/l Tricine Cu 2+ /Tricine = 1/ Voltage (V vs. NHE) Fig. 1. (a) UV vis spectra of Cu 2+ and tricine with different ratios in PBS (.2 mol/l, ph = 12.); (b) CV curves and (c) enlarged anodic polarization curves at an ITO electrode with the addition of an increasing amount of tricine into a PBS solution of 1. mmol/l Cu 2+ (.2 mol/l, ph = 12.); (d) CV curves measured at a bare ITO electrode, with 1. mmol/l Cu 2+, with 1. mmol/l tricine, and with Cu 2+ /tricine = 1/1 in PBS (.2 mol/l, ph = 12.) at 5 mv/s.

4 482 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) Fig. 4. TEM ((a), (b)) and HRTEM ((c), (d)) images of the Cu tricine film sample scraped from the ITO electrode. Fig. 2. SEM images of the electrodeposited Cu tricine based electrocatalyst film on an ITO substrate with different magnifications. Inset in (a) shows a photograph of the Cu tricine catalyst film on the ITO substrate. with a thermal conductive detector) to be μmol and the charge passed was 64.8 C (namely, μmol of oxygen gas) during electrolysis. The Faradic efficiency (%) was calculated as O2(actual)/O2(theoretical) Results and discussion In this study, a Cu tricine complex, formed in situ, was used as the precursor for electrodepositing a nanostructured catalyst film (i.e., a Cu tricine film), which featured a high OER activity in.2 mol/l PBS. Fig. 1 (a), (b), and (c) show the ultraviolet visible spectra and electrochemical CV curves measured for various Cu 2+ /tricine ligand ratios in PBS. The results show that the optimum concentrations were 1. mmol/l Cu 2+ and 1. mmol/l tricine. These values were used to electrodeposit the catalyst film in subsequent experiments. Fig. 1 (d) shows that a low background current density was measured in the absence of Cu 2+ and/or the tricine ligand. When Cu 2+ ions alone were added to PBS, Cu(OH)2 and Cu3(PO4)2 precipitates formed, which were not active towards water oxidation. Similarly, the addition of tricine alone did not enhance the OER activity. Water oxidation reactivity was clearly observed in the CV curve when both tricine and Cu 2+ were added to PBS. A copper derived electrocatalyst film was formed in PBS (.2 mol/l, ph = 12.) containing 1. mmol/l Cu 2+ and 1. mmol/l tricine within 6. h, while a working electrode potential of 1.15 V vs. NHE was maintained in the controlled potential experiments. Photographs (the inset in Fig. 2 (a)) show the black catalyst film that was electrodeposited on the ITO substrate. The morphology of the prepared Cu tricine catalyst film was examined by SEM and the images are shown in Fig. 2. A dense nanostructure can be clearly observed on the ITO substrate. A cross sectional image of the film, shown in Fig. 3, indicated that the average thickness of the catalyst film was approximately 1.4 μm. TEM and high resolution TEM images (Fig. 4) of the Cu tricine film scraped from the ITO substrate showed that the catalyst film was amorphous. The amorphous nature of the electrodeposited film was confirmed by XRD. Fig. 5 shows that the XRD pattern of the prepared film contained no peaks indicative of crystalline phases other than the peaks associated with the ITO substrate. Intensity Bare ITO Cu-Tricine film Fig. 3. Cross sectional SEM image of the electrodeposited Cu tricine film on an ITO substrate /( ) Fig. 5. XRD patterns of the bare ITO and the electrodeposited Cu tricine film on an ITO substrate.

5 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) The composition of the prepared Cu tricine film was determined by EDX and XPS measurements. The EDX data for the catalyst film (Fig. 6) showed that the film deposited in PBS contained mainly the elements Cu, O, and In. The Cu and O peaks likely derived from decomposition of the Cu complex, and In derived from the ITO substrate. The peaks in the XPS survey in Fig. 7 (a) were all accounted for by the elements detected by EDX. Fig. 7 (b) shows a high resolution spectrum of the Cu 2p. Peaks from 2p3/2 and 2p1/2 occurred at and ev, respectively, with additional intense satellite peaks from Cu(II). The binding energies of these Cu 2p peaks were intermediate between those of CuO and Cu(OH)2 and the signals could be attributed to a mixture of CuO/Cu(OH)2. The C signal in the XPS survey data (Fig. 7 (c)) can presumably be attributed to surface contamination of the sample by air. The two sub peaks at and ev in the high resolution O 1s spectrum (Fig. 7 (d)) were assigned to oxygen atoms of oxide and hydroxide, respectively. This result confirms that the electrodeposited Cu based catalyst film was a mixture of CuO and Cu(OH)2. The activity of the Cu tricine catalyst film for the OER was evaluated by CV. Fig. 8 (a) shows that the catalyst film exhibits excellent performance for electrocatalytic water oxidation. The catalytic current density grew rapidly and reached >15. ma/cm 2 at 1.4 V vs NHE. A bare ITO electrode, which had no Fig. 6. EDX spectrum of the electrodeposited Cu tricine film on an ITO substrate. appreciable catalytic activity from.2 to 1.5 V vs NHE, was used for a control experiment. The long term performance and stability of the Cu tricine electrocatalyst film were investigated by performing controlled potential water electrolysis in PBS (.2 mol/l). Under an applied potential of 1.15 V vs NHE, a stable catalytic current density for water oxidation of approximately 7.5 ma/cm 2 was achieved (Fig. 8 (b)). No obvious OER catalytic activity was observed with the use of a bare ITO plate as the working electrode during electrolysis under the same conditions (Fig. 8 (b)). These results clearly show that the electrodeposited Cu tricine film performed as a highly efficient and stable water oxidation catalyst in PBS. 5 4 (a) Survey O 1s Cu 2p 21 (b) Cu 2p Intensity (/1 3 ) Cu 3p C 1s Cu 3s Intensity (/1 3 ) Binding energy (ev) 12 (c) C 1s Binding energy (ev) (d) O 1s Intensity (/1 3 ) Intensity (/1 3 ) Binding energy (ev) Binding energy (ev) Fig. 7. (a) XPS spectrum of an electrodeposited Cu Tricine film on an ITO glass; Enlarged views of the XPS for Cu 2p (b), C 1s (c) and O 1s (d) present in the electrodeposited Cu tricine film.

6 484 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) (a) Bare ITO Cu-tricine film (b) Voltage (V vs. NHE) Cu-tricine film Bare ITO Time (h) Fig. 8. (a) CV curves of bare ITO and the electrodeposited Cu tricine electrocatalyst in PBS (.2 mol/l, ph = 12.); (b) Long term CPE of water in PBS (.2 mol/l, ph = 12.) with a bare ITO and a freshly electrodeposited Cu tricine electrocatalyst film. Gas bubbles were clearly observed on the surface of the Cu tricine film electrode during electrolysis. The electrolysis products were further explored by calculating the Faradaic efficiency, based on the catalytic performance of the Cu tricine film catalyst at 6. ma/cm 2 in a gas tight electrochemical cell in PBS (.2 mol/l). Gas chromatography showed that the amount of oxygen evolved during the OER during electrolysis for 3 h was μmol. The theoretical amount of oxygen evolution at a current density of 6. ma/cm 2 was calculated to be μmol, assuming that the total charge arose from 4e oxidation of water, based on Faraday s law. Thus, the amount of oxygen produced matched the theoretical amount well, and corresponded to a Faradaic efficiency of 99% (Fig. 9). This result shows that the catalytic current density was mainly consumed by water oxidation leading to oxygen production. The kinetics of the reaction catalyzed by the Cu tricine film were explored based on a Tafel plot for the electrocatalyst in PBS (.2 mol/l), with 1% ir compensation, under stirring. The steady state current densities (i) obtained by electrolysis for 12 s at various potentials were evaluated as a function of the overpotential (η) as η = Vappl ir EpH, where Vappl is the applied potential, i is the steady state current, R is the uncompensated resistance, and EpH is the thermodynamic potential for water oxidation at this ph (EpH = 1.23 V.59 ph V vs. NHE). Fig. 1 shows that a current density of 1. ma/cm 2 required η = 395 mv. A nearly linear relationship, with a slope of 46.7 mv/decade, was observed from.315 to.395 V, indicating that the water oxidation catalyst featured efficient kinetics. Thus, the catalytic activities and Tafel slopes of the reported Cu based catalysts (Table 1) indicate that the Cu tricine catalyst films exhibited efficient activity for water oxidation. 4. Conclusions A Cu tricine complex formed in situ served as a precursor for electrodepositing a nanostructured amorphous catalyst film for water oxidation. The results show that Cu tricine is a good and robust catalyst in PBS (.2 mol/l, ph 12.), giving a catalytic current density of 1. ma/cm 2 at an overpotential of 395 mv. A Faradaic efficiency of 99% for water oxidation was achieved with the use of the Cu tricine film as the working electrode at a current density of 6. ma/cm 2. A Tafel plot at ph O2 ( mol) 8 Measured value Theoretical value Overpotential (V) y = x Time (h) Fig. 9. Determination of the Faradic efficiency of the Cu tricine film for electrolysis of water at 6. ma/cm 2 in PBS (.2 mol/l, ph = 12.) log j /A/cm 2 Fig. 1. Tafel plot of Cu tricine film in phosphate solution buffer (.2 mol/l, ph = 12.) under stirring with 1% ir compensation.

7 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) Graphical Abstract Chin. J. Catal., 218, 39: doi: 1.116/S (17) Highly effective electrochemical water oxidation by copper oxide film generated in situ from Cu(II) tricine complex Yan Gao *, Hu Chen, Lu Ye, Zhongkai Lu, Yanan Yao, Yu Wei, Xuyang Chen Dalian University of Technology H + H 2 HER H 2 O O 2 A dense Cu tricine film was electrodeposited on ITO from phosphate buffer solution (.2 mol/l) containing Cu 2+ and tricine ligand. The as prepared anode showed efficient electrocatalytic water oxidation performance with good stability. OER 12. was constructed with a slope of 46.7 mv/decade. The use of metal complexes as precursors for electrodeposition can avoid metal salt precipitation in buffer solution and enable deposition of highly efficient and stable catalyst films. References [1] S. Chu, A. Majumdar, Nature, 212, 488, [2] D. G. Nocera, Acc. Chem. Res., 212, 45, [3] Y. Jiao, Y. Zheng, M. Jaroniec, S. Z. Qiao, Chem. Soc. Rev., 215, 44, [4] D. S. Kong, J. J. Cha, H. T. Wang, H. R. Lee, Y. Cui, Energy Environ. Sci., 213, 6, [5] X. M. Li, X. G. Hao, A. Abudula, G. Q. Guan, J. Mater. Chem. A, 216, 4, [6] X. Liu, S. Inagaki, J. L. Gong, Angew. Chem. Int. Ed., 216, 55, [7] G. Zhang, G. Liu, L. Z. Wang, J. T. S. Irvine, Chem. Soc. Rev., 216, 45, [8] M. T. M. Koper, J. Electroanal. Chem., 211, 66, [9] M. Gong, H. J. Dai, Nano Res., 215, 8, [1] H. Over, Chem. Rev., 212, 112, [11] Y. Lee, J. Suntivich, K. J. May, E. E. Perry, S. H. Yang, J. Phys. Chem. Lett., 212, 3, [12] Z. Liu, Y. Gao, Z. Yu, M. Zhang, J. H. Liu, Chin. J. Catal., 215, 36, [13] Y. Jiang, F. Li, F. Huang, B. B. Zhang, L. C. Sun, Chin. J. Catal., 213, 34, [14] J. J. Concepcion, J. W. Jurss, M. K. Brennaman, P. G. Hoertz, A. O. T. Patrocinio, N. Y. M. Iha, J. L. Templeton, T. J. Meyer, Acc. Chem. Res., 29, 42, [15] N. D. McDaniel, F. J. Coughlin, L. L. Tinker, S. Bernhard, J. Am. Chem. Soc., 28, 13, [16] Y. Lattach, J. F. Rivera, T. Bamine, A. Deronzier, J. C. Moutet, ACS Appl. Mater. Interfaces, 214, 6, [17] K. S. Joya, K. Takanabe, H. J. M. de Groot, Adv. Energy Mater., 214, 4, [18] H. Chen, Y. Gao, L. C. Sun, ChemCatChem, 216, 8, [19] S. A. Bonke, M. Wiechen, R. K. Hocking, X. Y. Fang, D. W. Lupton, D. R. MacFarlane, L. Spiccia, ChemSusChem, 215, 8, [2] H. Y. Chen, Z. J. Sun, X. Liu, A. L. Han, P. W. Du, J. Phys. Chem. C, 215, 119, [21] A. L. Han, H. T. Wu, Z. J. Sun, H. X. Jia, Z. P. Yan, H. Ma, X. Liu, P. W. Du, ACS Appl. Mater. Interfaces, 214, 6, [22] M. W. Kanan, D. G. Nocera, Science, 28, 321, [23] J. H. Wang, W. Cui, Q. Liu, Z. C. Xing, A. M. Asiri, X. P. Sun, Adv. Mater., 216, 28, [24] X. X Yu, T. Y. Hua, X. Liu, Z. P. Yan, P. Xu, P. W. Du, ACS Appl. Mater. Interfaces, 214, 6, [25] A. Singh, S. L. Y. Chang, R. K. Hocking, U. Bach, L. Spiccia, Energy Environ. Sci., 213, 6, [26] K. S. Joya, Y. F. Joya, H. J. M. de Groot, Adv. Energy Mater., 214, 4, [27] M. Dincă, Y. Surendranath, D. G. Nocera, Proc. Natl. Acad. Sci. USA, 21, 17, [28] C. Y. He, X. L. Wu, Z. Q. He, J. Phys. Chem. C, 214, 118, [29] X. Liu, H. X. Jia, Z. J. Sun, H. Y. Chen, P. Xu, P. W. Du, Electrochem. Commun., 214, 46, 1 4. [3] S. S. Cui, X. Liu, Z. J. Sun, P. W. Du, ACS Sustainable Chem. Eng., 216, 4, [31] X. Liu, H. F. Zheng, Z. J. Sun, A. L. Han, P. W. Du, ACS Catal., 215, 5, [32] F. S. Yu, F. Li, B. B. Zhang, H. Li, L. C. Sun, ACS Catal., 215, 5, [33] C. Lu, J. Y. Wang, Z. F. Chen, ChemCatChem, 216, 8, [34] K. S. Joya, H. J. M. de Groot, ACS Catal., 216, 6, [35] J. L. Du, Z. F. Chen, S. R. Ye, B. J. Wiley, T. J. Meyer, Angew. Chem. Int. Ed., 215, 54, [36] C. Lu, J. L. Du, X. J. Su, M. T. Zhang, X. X. Xu, T. J. Meyer, Z. Chen, ACS Catal., 216, 6, [37] H. Chen, Y. Gao, Z. K. Lu, L. Ye, L. C. Sun, Electrochim. Acta, 217, 23, [38] X. Q. Du, J. W. Huang, Y. Y. Feng, Y. Ding, Chin. J. Catal., 216, 37, [39] T. T. Li, S. Cao, C. Yang, Y. Chen, X. J. Lü, W. F. Fu, Inorg. Chem., 215, 54, [4] X. Liu, S. S. Cui, Z. J. Sun, Y. Ren, X. Y. Zhang, P. W. Du, J. Phys. Chem. C, 216, 12, [41] Y. Z. Wu, M. X. Chen, Y. Z. Han, H. X. Luo, X. J. Su, M. T. Zhang, X. H. Lin, J. L. Sun, L. Wang, L. Deng, W. Zhang, R. Cao, Angew. Chem. Int. Ed., 215, 54, [42] F. Li, L. C. Bai, H. Li, Y. Wang, F. S. Yu, L. C. Sun, Chem. Commun., 216, 52,

8 486 Yan Gao et al. / Chinese Journal of Catalysis 39 (218) [43] D. R. Chowdhury, L. Spiccia, S. S. Amritphale, A. Paul, A. Singh, J. Mater. Chem. A, 216, 4, [44] M. Khan, J. Xiao, F. L. Zhou, M. Yablonskikh, D. R. MacFarlane, L. Spiccia, E. F. Aziz, ChemSusChem, 215, 8, [45] M. Huynh, D. K. Bediako, D. G. Nocera, J. Am. Chem. Soc., 214, 136, [46] S. M. Barnett, K. I. Goldberg, J. M. Mayer, Nature Chem., 212, 4, [47] T. Zhang, C. Wang, S. B. Liu, J. L. Wang, W. B. Lin, J. Am. Chem. Soc., 214, 136, [48] M. T. Zhang, Z. F. Chen, P. Kang, T. J. Meyer, J. Am. Chem. Soc., 213, 135, 基于 Cu(II) Tricine 配合物制备氧化铜薄膜及其电催化水氧化活性 高岩 *, 陈虎, 叶璐, 路忠凯, 姚亚男, 魏宇, 陈旭阳大连理工大学精细化工国家重点实验室, 人工光作用研究所, 大连理工大学 - 瑞典皇家工学院分子器件联合中心, 辽宁大连 摘要 : 众所周知, 传统化石燃料的大量使用不仅导致严重的环境污染和温室效应, 而且化石能源本身也面临着枯竭的危机. 所以, 探索全新的 环境友善的 可持续发展的能源载体一直备受国内外科研工作者的关注. 氢能是一种清洁的可再生能源, 是有潜力的化石能源替代品. 水分解是一种有效的 理想的产氢途径, 然而水氧化反应是多质子多电子传递的过程, 是制约整个水分解过程的瓶颈. 目前, 基于贵金属 ( 铱和钌 ) 分子和氧化物的电催化剂已经被报道很多, 并且可以保持很好的催化活性 ; 但是, 这一类催化剂差的稳定性 昂贵的价格和少的地壳含量等因素严重制约了其大规模实际应用. 因此, 开发基于非贵金属 ( 钴 镍 铁 铜 锰 ) 的新型电催化剂材料是解决该问题的唯一出路, 但要保证电催化剂的高活性和好的稳定性仍面临着诸多挑战. 在众多的非贵金属中, 铜是一种来源广泛的金属, 而且铜对生物体毒性较小. 由于铜具有良好的配位化学和多重的氧化还原特性, 近年来, 很多基于铜的水氧化电催化剂被开发和研究. 我们在含有 1. mmol/l Cu 2+ 和 2. mmol/l Tris 配体的磷酸缓冲溶液 (.2 mol/l, ph = 12.) 中, 采用 1.15 V vs. NHE 恒电位电沉积的方法, 在 ITO 导电玻璃上制备出基于铜的水氧化催化剂薄膜 (Cu-tricine). 对得到的催化剂薄膜进行扫描电镜 (SEM) 测试, 该催化剂均匀负载在 ITO 表面, 厚度大约是 1.4 μm. 为了更加深入研究 Cu-Tricine 催化剂薄膜, 采用透射电子显微镜 (TEM) 和 X 射线衍射 (XRD) 对 Cu-tricine 催化剂进行表征, 结果表明, 该催化剂薄膜是一种结晶度较差的无定形材料. 同时, 为了研究催化剂薄膜的元素组成及其所处状态, 对催化剂进行了能量散射 X 射线能谱 (EDX) 和 X 射线光电子能谱 (XPS) 测试, 结果表明, 该催化剂由铜和氧元素组成, 并且铜是以正二价存在. 由高分辨 O 1s XPS 谱图分析结果可以推测, Cu-Tricine 催化剂可能是由氧化铜和氢氧化铜组成. Cu-tricine 催化剂的水氧化活性是在.2 mol/l 的磷酸缓冲溶液 (ph = 12.) 中进行测试, 从塔菲尔曲线中可以得出, 该催化剂达到 1. ma/cm 2 的催化电流密度所需的过电位是 395 mv, 塔菲尔斜率为 46.7 mv/decade. 此外, 在 1.15 V vs. NHE 的电位下, 在 1 h 的电解过程中, Cu-tricine 催化剂薄膜可以将催化电流密度一直保持在 7.5 ma/cm 2, 并且得到的法拉第效率为 99%. 关键词 : 水氧化 ; 析氧反应 ; 电沉积 ; 氧化铜薄膜 ; 电催化剂 收稿日期 : 接受日期 : 出版日期 : * 通讯联系人. 电话 : (411) ; 传真 : (411) ; 电子信箱 : 基金来源 : 国家重点基础研究发展计划 (973 计划, 214CB23942); 国家自然科学基金 ( ); 辽宁省重点实验室基础研究项目 (LZ21515). 本文的英文电子版由 Elsevier 出版社在 ScienceDirect 上出版 (

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