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Electronic Supplementary Information Electrosynthesis, Functional, And Electronic Supplementary Material (ESI) for Energy & Environmental Science This journal is © The Royal Society of Chemistry 2012 Electronic Supplementary Information Electrosynthesis, Functional, and Structural Characterization of a Water-Oxidizing Manganese Oxide Ivelina Zaharieva,*a Petko Chernev, a Marcel Risch,a, c Katharina Klingan,a Mike Kohlhoff,a Anna Fischer,b and Holger Dau*a a Fachbereich Physik, Freie Universität Berlin, Arnimallee 14, 14195 Berlin, Germany. E-mail: [email protected]; [email protected]; Fax: +49 30 838 56299; Tel: +49 30 838 53581 b Institute of Chemistry, Technical University Berlin, Straße des 17. Juni, 10623 Berlin, Germany c present address: Electrochemical Energy Laboratory, MIT, 77 Massachusetts Ave, Cambridge, MA-02139, USA S1 Electronic Supplementary Material (ESI) for Energy & Environmental Science This journal is © The Royal Society of Chemistry 2012 S-1. Details of experimental procedures A. Electrodeposition. Reagents: (Mn(CH3COO)2·4H2O (Fluka, ≥99%), H2KPO4 (Roth, ≥99%), K2HPO4 (Roth, ≥99%), MgSO4·7H2O (AppliChem, ≥99.5%), Na(CH3COO) (Sigma-Aldrich, ≥99%), CH3COOH (AppliChem, 100%), MnCl2·4H2O (Roth, ≥98%), Mg(CH3COO)2·4H2O (Fluka, 99%), MnSO4·4H2O (Merck, p.A.), NaClO4 (Aldrich, 99.99% trace metal basis), II II Co (OH2)6(NO3)2 (Sigma Aldrich, ≥99.9%), Ni (OH2)6(NO3)2 (ChemPur, ≥99%), H3BO3 (Merck, p.A.), KOH (Sigma Aldrich, ≥86%). All reagents where used without further purification. Solutions were prepared with 18 MΩ·cm Milli-Q water. The electrochemical experiments were performed at room temperature using a potentiostat (SP-300, BioLogic Science Instruments) controlled by EC-Lab v10.20 software package. The Mn films were deposited in de- ionised water, in 0.1 M MgSO4 or in 0.1 M Na acetate buffer (pH 6.0). If not stated otherwise, Mn(II) acetate tetrahydrate in final concentration of 0.5 mM was added as a source of Mn2+ ions. The conditions for electrodeposition were kept as simple as possible. The solutions were not stirred during the experiments, and if not stated otherwise, also not dearated. A single- compartment three-electrode electrochemical cell was used with saturated Hg/Hg2SO4 electrode (RE-2C, BioLogic) as reference electrode and a platinum mesh as counter electrode. The working electrode was 2 cm2 (2 cm × 1 cm) indium-tin oxide (ITO) coated glass plate, 8-12 Ω/sq (purchased from Sigma-Aldrich). The volume of the solution was 100 mL. The pH was adjusted using 3 M NaOH only for the buffered systems (0.1 M phosphate or 0.1 M acetate buffer). The pH of the other solutions used for film deposition was typically between 6 and 6.5 (which did not affect the reproducibility) and was not adjusted. For comparison of the turnover frequency (TOF), catalytically active Co and Ni oxides were electrodeposited, The Co oxide was deposited at constant potential in 0.1 M phosphate buffer as described in ref.1, but using an anode potential of +1.05 V (vs. NHE) which is below onset of catalytic activity. The total charge during the electrodeposition was used to estimate the amount of deposited Co ions (assuming that Co2+ gets oxidized to Co3+ during the deposition). Oxygen evolution was measured as described in S-1C applying a constant potential of 1.35 V at pH 7 in Co-free 0.1 M phosphate buffer. The Ni oxide was deposited at constant potential in 0.1 M borate buffer at pH 9.2 as described in refs.2-3 At the deposition potential of 1.15 V the catalytic current was still small. The charge during the deposition was used to estimate the amount of the deposited Ni, assuming change of oxidation state of Ni from +2 in the solution to +3 in the deposited material. Oxygen evolution was measured in Ni-free borate buffer (0.1 M) at pH 9.2. B. UV-vis spectroscopy. UV-vis measurements were performed using Varian Cary 50 UV-vis spectrophotometer. To realize in situ measurements, a modified quartz cuvette (2.5 cm × 2.5 cm × 4 cm height) filled with 15 ml electrolyte was placed in the optical compartment of the spectrometer. The transparent working electrode was placed in front of the detector window and the Hg/Hg2SO4 reference electrode (5 mm diameter) and the platinum counter electrode were placed next to the walls of the cuvette in such a way that they were not hit be the measuring beam. The electrochemistry was controlled by a potentiostat (SP-300). For the spectrum of the inactive film shown in Fig 2, a slightly negative value was detected at the absorption minimum because of minor imprecision in the baseline determination. S2 Electronic Supplementary Material (ESI) for Energy & Environmental Science This journal is © The Royal Society of Chemistry 2012 C. Detection of O2 evolution. The oxygen evolution was measured with a Clark-type electrode, (liquid-phase oxygen electrode chamber DW1, Hansatech Instruments). The counter, working, and reference electrodes of the electrochemistry setup were inserted into the solution compartment of the oxygen electrode chamber. The counter electrode (platinum mesh) was wrapped around the glass tube of the reference Hg/Hg2SO4electrode. The working electrode was an ITO-coated glass plate (0.5 cm × 1 cm). The contact between the ITO surface and the potentiostat cable was secured by copper tape, which was isolated from the solution by parafilm. The cell was filled with 3 ml 0.1 M phosphate buffer (pH 7) and sealed with a rubber ring and parafilm, leaving no gas phase volume. To remove the O2 from the buffer solution, nitrogen gas was bubbled through the solution, for several minutes, before complete sealing of the Clark cell. The Clark cell was calibrated using O2-free water and O2-saturated water. The signal was recorded with a computer using a digital oscilloscope (Voltcraft® DSO-2090 USB). In control experiments, we verified that the Clark electrode for polarographic detection of dioxygen does not interfere with the electrochemical experiment. To ensure interference-free function, the electronics used for detection of the O2-reduction current and application of the polarization voltage (-0.7 V) to the platinum cathode and silver anode was completely galvanically insulated from the electrochemical set up. The two Clark-cell electrodes were covered with a KCl solution (3 M) and separated from the buffer solution by a diaphragm permeable only to dioxygen. Switching on and off the anodic potential (i.e. 1.35 V) on the potentiostat did not change the O2 signal (with bare ITO electrode). Also switching on and off the polarization voltage of the Clark cell did not change the (catalytic) current recorded when a constant potential of 1.35 V was applied to the MnCat in the Clark-cell. D. SEM images and elemental analysis. Scanning electron microscopy (SEM) and energy- dispersive X-ray analysis (EDX) were performed with a JEOL 7401F scanning electron microscope operated at 10 kV and equipped with a Bruker Quantax 400 EDX detector. Elemental analysis was done using the PicoFox Spectrometer (Bruker) for total reflection X-ray fluorescence (TXRF) measurements. The Mn oxide films that had been deposited on 1 cm2 ITO coated glass plate were dissolved in 500 µl of 30% HCl by exposing the films to the acid for several minutes. 100 µl of the resulting solution were mixed with 100 µl of a solution containing a Ga standard (Ga(NO3)3, concentration of 10 mg/l), and 5 µl of the mixture were deposited on a silicon-coated quartz glass sample plate. The acquisition time was 30 min per sample. E. XAS measurements and simulations. X-ray absorption spectroscopy at the K-edge of manganese was performed at the KMC-1 beamline at the BESSY synchrotron (Helmholtz- Zentrum Berlin, Germany) at 20 K in a liquid-helium cryostat as described elsewhere.4 Spectra were recorded in fluorescence mode using a 13-element Ge detector (Canberra). The extracted 3 spectrum was weighted by k and simulated in k-space (E0 = 6547 eV). All EXAFS simulations were performed using in-house software (SimX3) after calculation of the phase functions with the FEFF program5-6 (version 8.4, self-consistent field option activated). Atomic coordinates of the FEFF input files were generated for several reasonable structural models; the EXAFS phase functions did not depend strongly on the details of the used model. An amplitude reduction factor 2 -1 S0 of 0.7 was used. The data range used in the simulation was 20–1000 eV (3–16 Å ). The EXAFS simulation was optimized by a minimization of the error sum obtained by summation of the squared deviations between measured and simulated values (least-squares fit). The fit was performed using the Levenberg-Marquardt method with numerical derivatives. The error ranges S3 Electronic Supplementary Material (ESI) for Energy & Environmental Science This journal is © The Royal Society of Chemistry 2012 of the fit parameters were estimated from the covariance matrix of the fit, and indicate the 68 % confidence intervals of the corresponding fit parameters. The fit error was calculated as in ref.3 For XAS samples preparation, mostly 1.35 V was applied for 2 min in a Mn-free phosphate buffer (pH 7). After that the samples were quickly taken out of the solution, rinsed with de- ionized water and frozen in liquid nitrogen where they were kept until the XAS measurements. To verify that during rinsing and freezing of the sample there is no major change in the structure, we prepared samples according to a procedure detailed in the following which allows freezing of the MnCat in liquid nitrogen under applied potential. Therefore we deposited the MnCat not on ITO, but on 1.5 cm2 of glassy carbon of 100 µm thickness (HTW Hochtemperatur-Werkstoffe GmbH).
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