Achieving High Electrocatalytic Efficiency on Copper: A Low-Cost Alternative to Platinum for Hydrogen Generation in Water

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1 Supporting Information Achieving High Electrocatalytic Efficiency on Copper: A Low-Cost Alternative to Platinum for Hydrogen Generation in Water Jian Zhao, a,b,c,d Phong D. Tran,* a,c Yang Chen, a,c Joachim Loo,* b,c James Barber, c,e and Zhichuan J. Xu* a,b,c,d a Energy Research Nanyang Technological University, Singapore; b School of Materials Science Engineering, Nanyang Technological University, Singapore; c Solar Fuel Laboratory, Nanyang Technological University, Singapore; d Singapore-Berkeley Research Initiative for Sustainable Energy, 1 Create Way, Singapore; e Department of Life Sciences, Imperial College London, London, UK. s: xuzc@ntu.edu.sg; joachimloo@ntu.edu.sg; dptran@ntu.edu.sg 1

2 Materials and Methods All chemical compounds were used as received without any further purification. Cu 2 O/Cu/Mo electrode preparation: Mo (approximately 1.0 m thickness) coated glass slides were prepared by thermal evaporation. Cu 2 O film was deposited on Mo-coated glass slide from deposition bath which consisted of CuSO 4 5H 2 O (4994 mg), lactic acid (15015 mg), DI water (28 ml) whose ph was adjusted to 12 by adding concentrated NaOH (20 M) solution. Conventional three electrodes configuration was employed. Reference electrode was Ag/AgCl/1M KCl while counter electrode was a Pt wire. Typically, Mo-coated glass (geometric area of 1cm 2 ) was held at -0.4 V vs. Ag/AgCl for 15 min. resulting in deposition of 1.5 m Cu 2 O film. The deposition bath was kept at 50 C during deposition process. Once the deposition was over, the resulting films were carefully washed with DI water and subsequently annealed at 100 C for 3h. The Cu 2 O electrode was then held at V vs. RHE, under 1 Sun illumination, in a degassed ph 7 phosphate buffer solution for 10 min. It was further equilibrated at V vs. RHE in the same electrolyte solution but under dark conditions for 30 min. Finally, the resulting Cu/Cu 2 O electrodes were carefully washed with DI water and air-dried prior to being used for characterization and assays of catalytic activities. Catalytic activities assessment Catalytic activities of prepared Cu/Cu 2 O electrodes were assayed in phosphate or carbonate buffer solution by recording steady currents at different cathodic potentials. The potential increment was mv per experimental point. Bulk electrolysis was conducted in a customized gas-tight closed two compartment cell. Possible gas products (H 2 and CO) were analysed by gas chromatography while formate was analysed by employing ion-exchange column chromatography. Characterizations: The morphology of films and mapping images was obtained from Field Emission Scanning Electron Microscopy (FESEM, JEOL JSM-7600F). XRD analysis was carried out on Shimadzu XRD-6000 X-ray diffractometer (Cu K source) with the 2 range from 10 to 80 at a scan rate of 2 o /min. Electrochemical measurements were conducted on Autolab PGSTAT-30 or a CHI workstation (CHI852c, CH Instruments). The applied potential vs. RHE was calibrated by HER/HOR (hydrogen evolution/oxidation reaction) on a Pt disk electrode in the hydrogen saturated electrolyte (the system was bubbled with hydrogen gas continuously during the calibration measurements). The determined E was 650 mv (as shown in the figure below, Figure S1). 2

3 Figure S1: RHE reference electrode calibration using HER/HOR on Pt electrode. Bulk electrolysis was conducted in a gas-tight closed, two compartment electrochemical cell. Gas in the head cap of the working compartment was manually sampled at given intervals and analyzed by gas chromatography (GC, Agilent 7890A) with TCD detector. Formate within electrolyte solution was analyzed employing a Metrohm ion chromatograph. Current to H 2 yield (Faradaic Efficiency, FE) was calculated according to equation: I- current during electrolysis t- electrolysis time

4 Figure S2: Cross-section of Cu 2 O film i) after treatment at V, hv, 10 min ii) and V, dark, 10 min iii). Figure S3: Calibration curve obtained by plotting the amount of H 2 in head space vs. total amount of H 2 calculated in head space and solution. The number of moles of dissolved H 2 in solution (nh 2(sol) ) was calculated using Henry s law as follows: nh 2(sol) = V sol P H2 kh,cp, where P H2 is the partial pressure and kh,cp is Henry s constant, mol/l atm. Assuming ideal gas behavior, the partial pressure of H 2 (P H2 ) can be expressed as: P H2 = [nh 2(HS) R T]/V HS, where V HS is the volume of the head space, T the room temperature and R the gas constant, L atm/k mol. Finally, total amount of H 2 produced was calculated as the sum of H 2 in head space and H 2 dissolved in solution. 4

5 Figure S4: XRD pattern and the cross-section SEM image with EDS mapping after 2 h bulk electrolysis at V vs. RHE using a Cu/Cu 2 O electrode (ii) in 0.1 M phosphate buffer ph 7. (Note: Pt was coated when conducting this SEM experiment for EDS mapping). Figure S5: Bulk electrolysis at -0.26V vs. RHE using a Cu/Cu 2 O electrode and polarization curves in 0.1 M phosphate buffer ph 7. 5

6 Figure S6: Polarization curves of stabilized Cu/Cu 2 O on carbon paper in ph 7 phosphate buffer solution (0.5 M), scan rate 2 mv/s. a is due to the double layer capacitance. The inset picture shows the Cu/Cu 2 O on carbon paper. Figure S7: Bulk electrolysis at V vs. RHE in 0.5 M phosphate buffer ph 7 employing a Cu/Cu 2 O electrode. 6

7 Figure S8. Polarization curves of our Cu/Cu 2 O electrode with a scan rate 2 mv/s and Pt disk with a rotating rate of 1000 rpm, in ph 7 phosphate buffer solution (0.5 M). a is due to the double layer capacitance. 7

8 Figure S9. The representative CVs of the four electrodes we measured for ESA. (a) Thick Cu foil annealed at 500 o C for 12 h (the same treatment method as Kanan group s work, Reference 2). It was then reduced using the same reduction method for our copper electrode. (b) Thin Cu foil electrochemically oxidized at V vs. SCE in 3 M NaOH for 30 min (the same treatment as the Reference 3). It was then reduced using the same reduction method for our copper electrode. (c) Thin Cu foil without the oxidation/reduction process. (d) Our Cu electrode. All the electrodes have the same geometric surface area of 1 cm 2. Figure S10. The catalytic performance of the four Cu electrodes using current density normalized by ESA. Figure S11. Reproduction of Figure 2a (in the manuscript) by normalizing current density using the ESA of the electrode. (a) Current-voltage (I-V) characteristic curves and (b) the corresponding log j versus over potential η curves. The points were obtained by recording the steady current at certain potentials for 15 min. 8

9 We measured the electrochemical surface area (ESA) of our Cu electrode in Ar-saturated 0.1 M KOH solution according to the established method (Energy Environment Science, 2013, 6, 1509, Ref. [1] below), as shown in Figure S9. In a typical measurement, the CV was recorded from V to V vs. RHE at a scan rate of 20 mv/s. The anodic peak between 0.5 V and 0.75 V corresponds to the formation of Cu 2 O with a charge density of 360 C/cm 2 Cu.[1] The calculated ESA and roughness factors can be found in Table S1.According to the ESA, we normalized the polarization curves of these four samples in 0.5 M phosphate solution (ph=7, scan rate 2 mv/s) by their ESA. Please see the Figure S10. As compared with the other high roughness copper electrode (a), clearly our copper electrode shows excellent performance (d). If we divide the I-V curve of Figure 2a (the figure in the manuscript) by the real surface area (ESA), the onset potential remains same with a Tafel slope of 65 mv/dec using the established method by Adzic s group (Figure S11). Therefore, we confirm that the excellent performance of our copper electrode is not due to the high surface area. Table S1. Parameters for the calculation of ESA and surface roughness corresponding to Figure S9. Sample Integrated Range (V) Integrated Area S (ma V) Q ( C) = S*1000/[0.02] Real surface area (cm 2 ) = Q/[360( C/cm 2 Cu)] (a) (b) (c) (d) Roughness factor References cited: [1] Sheng, W. C.; Myint M.; Chen, J. G.; Yan, Y. S. Energy Environ. Sci., 2013, 6, [2] Li, C. W.;Kanan, M. W. J. Am. Chem. Soc. 2012, 134, [3] Zhang, Z. H.; Wang, P. J. Mater. Chem. 2012, 22,

10 Figure S12: Morphology of Cu/Cu 2 O electrode after HER assays in a 0.1 M Na 2 SO 4 electrolyte solution. Figure S13: Morphology of Cu/Cu 2 O electrode after HER assays in a 0.1M NaClO 4 electrolyte solution. 10

11 Figure S14: Morphology of Cu/Cu 2 O electrode after HER assays in a 0.1M NaCl electrolyte solution. Figure S15: EDS of Cu 2 O/Cu electrode after treatment in ph 6.9 Na 2 SO 4 (0.1 M) solution. 11

12 Figure S16: Catalytic activities of Cu/Cu 2 O electrode in a 0.25 M Na 2 CO 3 solution saturated with CO 2 (0.5 M NaHCO 3 ). Figure S17: Dependence of catalytic activities on carbonate concentration for a Cu/Cu 2 O electrode. Carbonate solution was adjusted to ph

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