Preparation of copper oxide modified boron-doped

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Preparation of copper oxide modified boron-doped diamond electrodes and its preliminary study for CO2 reduction

This content has been downloaded from IOPscience. Please scroll down to see the full text. 2017 IOP Conf. Ser.: Mater. Sci. Eng. 188 012011 (http://iopscience.iop.org/1757-899X/188/1/012011) View the table of contents for this issue, or go to the journal homepage for more Download details: IP Address: 181.215.130.199 This content was downloaded on 03/05/2017 at 08:43 Please note that terms and conditions apply.

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International Conference in Physics 2016 (ICRTP2016) IOP Publishing Symposiumon onRecent CurrentTrends Progress in Functional Materials Journal of Physics: Conference Seriesand 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001 IOP Conf. Series: Materials Science Engineering 188 (2017) 012011 doi:10.1088/1757-899X/188/1/012011 1234567890

Preparation of copper oxide modified boron-doped diamond electrodes and its preliminary study for CO2 reduction N Y Yetri, T A Ivandini and J Gunlazuardi Department of Chemistry, Faculty of Mathematics and Natural Sciences Universitas Indonesia, Kampus UI Depok, Depok 16424, Indonesia Corresponding author's e-mail: [email protected] Abstract. Preparation of boron-doped diamond (BDD) modified with Cu2O (Cu2O-BDD) electrodes was conducted to study the electrochemical reduction of CO2. The electrodes were prepared by electrochemical reduction using a solution containing 1mM Cu(CH3COO)2 and 0.1 M CH3COONa (1: 1) at pH 5.7 for 60 s. The electrodeposition of Cu2O at BDD surface was performed by chronoamperometry technique at -0.4 V (vs Ag/AgCl). SEM-EDS and XPS were utilized to characterize the electrodes. At Cu2O-BDD electrodes, cyclic voltammetry of dissolved CO2 in 0.1 M NaCl solution exhibited a reduction peak at around -1.3 V (vs Ag/AgCl), indicated the possibility for application in electrochemical reduction of CO2.

Keywords: Copper oxide, boron-doped diamond, carbon dioxide, electrochemical reduction 1. Introduction Carbon dioxide is one of main components contained in the atmosphere and is known as one of the greenhouse gas that causes global warming. Since the 19th century, emission of carbon dioxide gas increases dramatically with the rate of around 2 ppm every year. Pletcher [1] has stated that the current content of CO2 gas has reached around 400 ppm. This phenomenon has attracted the interest of researchers to reduce the emission of CO2 converting it to more useful compounds. In order to achieve this purpose, some electrochemists have applied certain types of electrodes, including Sn, Pb, Cu, and their related oxides [2, 3] to study the electrochemical reduction of CO2. It was reported that electrode surface contained copper oxide and can increase the formation of hydrocarbons [4]. The use of copper as a catalyst in CO2 electroreduction by coating the electrode with Cu2O was also reported to efficiently produce hydrocarbons in ambient temperature [5]. On the other hand, boron-doped diamond (BDD) electrodes are reported to have various advantages, such as high stability, wide working potential, as well as very low background current [6, 7]. Nakata et al. [8] reported that the electrochemical reduction of CO2 by using BDD electrodes can be performed in NaCl or sea water as the electrolyte. Further, Panglipur et al. [9] have employed copper-modified BDD electrodes for the electroreduction of CO2. In this work, we modify BDD with copper oxide. It is expected that by applying this electrode the percent yield of useful products can be increased. 2. Materials and methods The materials used were CO2, N2, Cu(CH3COO)2, CH3COONa, CH3COOH, H2SO4, NaCl, 2-propanol, HClO4, phosphate buffer, and acetonitrile. Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI. Published under licence by IOP Publishing Ltd 1

International Symposium on Current Progress in Functional Materials IOP Publishing IOP Conf. Series: Materials Science and Engineering 188 (2017) 012011 doi:10.1088/1757-899X/188/1/012011 1234567890

Prior to copper deposition, cyclic voltammetry of a solution containing 1 mM Cu (CH3COO)2 and 0.1 M CH3COONa with a ratio of 1: 1 at pH 5.7 was performed using BDD as the working electrode in the potential range of -0.2 V to -1.0 V (vs. Ag/AgCl). Chronoamperometry technique with a deposition time of 60 s was then applied at the peak potential attributed to the Cu(I) formation. The characterization of the modified was performed using SEM-EDS and XPS. Electrochemical reduction of CO2 was performed in a cell with three-electrode system with 0.1 M NaCl as the electrolyte. Cu2O-BDD was employed as the working electrode, while Ag/AgCl and Pt foil were used as the reference and the counter electrodes, respectively. In order to remove other gas in the solution, N2 was bubbled to the solution for 30 min. Further, CO2 was bubbled followed by performing the cyclic voltammetry of the solution at the potential range of 0.0 to -2.0 V. The solution produced was characterized using HPLC. 3. Results and discussion Cyclic voltammograms of the solution containing 1 mM Cu(CH3COO)2 and 0.1 M CH3COONa (1:1) pH 5.7 (figure 1a) shows that two reduction peaks of copper were observed. The first peak at -0.40 V was attributed to the formation Cu(I), while the second peak at -0.60 V indicated the formation of Cu(0). Accordingly, Cu2O-BDD was prepared by electrochemical reduction of the same solution at the potential of -0.40 V. Calculation based on the amperogram (figure 1b) indicated that 1.72 μg Cu2O could be deposited at the surface of BDD. SEM image of the electrode surface (figure 2 a) showed that copper particles could be deposited at the surface of the electrode with the average size of ~1 μm. EDS result showed the surface contained copper with the percent yields of 25.71% as well as oxygen with the percent yields of 10.67%. Meanwhile, the XPS spectrum shows that besides the peaks of C 1s at 285 eV and of O 1s at 530.5 eV, which characterized the surface of BDD [10], a couple peaks of Cu 2p3/2 and 2p1/2 at 952.8 eV and 933 eV, respectively (figure 2b) were also observed. The results confirmed the existence of bonds associated with Cu+ in Cu2O [11]. The cyclic voltammogram (figure 3) of the solution showed that the longer the time of CO2 bubbling, the higher the current which starting at about -1.2 V, suggested that onset of electrochemical reduction of CO2 was around the potential. Chronoamperometry technique at this potential was then required to investigate the products of electrochemical reduction of CO2 in NaCl solution.

Current (mA)

-0.02

-0.04

-0.06 (a) -0.08 -1

-0.8 -0.6 -0.4 Poten al (V) vs Ag/AgCl

-0.2

(a)

(b)

Figure 1. (a) Cyclic voltammogram and (b) chronoamperogram of the solution containing 1 mM Cu(CH3COO)2 and 0.1 M CH3COONa (1:1) pH 5.7. Scan rate of 100 mV/s was applied with BDD electrode as the working electrode.

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(a)

(a)

(b)

Figure 2. The characterization of the prepared Cu2O-BDD electrodes shown by (a) SEM image and (b) XPS spectrum with the magnification of Cu 2p peaks shown in the inset.

Figure 3. Cyclic voltammograms of 0.1 M NaCl solution containing N2 (solid line) and CO2 (dashed lines) at Cu2O- BDD 4. Conclusions Cu2O-modified boron-doped diamond electrodes have been successfully prepared. The electrodes showed the onset of CO2 reduction in 0.1 M NaCl solution at the potential around -1.3 V (vs. Ag/AgCl), indicated that the electrode is promising for application in CO2 reduction. More experiments will be conducted to investigate this possibility. Acknowledgements This work was funded by Hibah Desentralisasi PUPT Universitas Indonesia, Contract No. 1127/UN2.R12/HKP.05.00/2016. References [1] Pletcher D 2015 Electrochemistry Communications 61 97-101 [2] Chang T Y, Liang R M, Wu P W, Chen J Y and Hsieh Y C 2009 Materials Letters 63 1001-3 [3] Albo J, Alvarez-Guerra M, Castano P and Irabien A 2015 Green Chemistry 17 2304-24 [4] Ohya S, Kaneco S, Katsumata H, Suzuki T and Ohta K 2009 Catalysis Today 148 329-34

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