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8 protocols using chi660e potentiostat

1

Copper Oxide Photoanode Characterization

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All electrochemical experiments were conducted using a three-electrode system with a Cu2O|FTO plate working electrode, a platinum wire counter electrode, and an Ag/AgCl (saturated KCl, E = 0.197 V) reference electrode in 0.5 M sodium sulfate. A CHI 660-E potentiostat (CH Instruments Inc., USA) was used for all electrochemical tests. Photocurrent was analyzed under open circuit potential (OCP) by subjecting the working electrode to intermittent illumination in fifty second intervals using an 85 W Xe Sunworld HID light source. Mott–Schottky (MS) analysis was performed under a reverse bias from 0.1 to 0.6 V at 10 kHz, with a potential step of 0.05 V. The voltage range for MS and photocurrent tests was determined by cyclic voltammetry (CV). The potential range with no copper redox activity was used for MS analysis. AC impedance was carried out, without applied bias, under dark and illuminated conditions and in a frequency range of 10−2–105 Hz.
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2

Comprehensive Materials Characterization Protocol

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SEM, as well as corresponding elemental mapping, and EDX analysis were carried out with a Gemini 500 (Carl Zeiss) system. HRTEM was performed using a LIBRA 200 MC Cs scanning TEM (Carl Zeiss) operating at an accelerating voltage of 200 kV. XPS experiments were carried out on an AXIS Ultra DLD (Kratos) system using Al Kα radiation. XRD patterns were recorded on a PW1820 powder diffractometer (Phillips) using Cu-Kα radiation. The electrochemical tests were carried out on WaveDriver 20 (Pine Research Instrumentation) and CHI 660E Potentiostat (CH Instruments) systems.
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3

Comprehensive Characterization of Electrocatalysts

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X-ray diffraction (XRD) patterns of the materials were obtained using a Rigaku-Ultima IV fully automatic high-resolution X-ray diffractometer equipped with an X-ray generator operating at 40 kV and 40 mA. The measurements were performed in a step of 0.01° (2θ) at room temperature. The as-prepared electrocatalysts were characterized by FE-SEM (JEOL-Japan) equipped with an energy dispersive X-ray analysis (EDAX) attachment. High-resolution transmission electron microscopy (HR-TEM) was performed using a JEOL JEM 2100 instrument. Fourier transform infrared (FTIR) spectroscopy was recorded in the range of 4000–500 cm−1 on a PerkinElmer Spectrum-I spectrometer. Field emission scanning electron microscopy and Raman spectroscopy were performed using a Raman spectrometer with a microscope (Seki Technotron Corp., Tokyo) with a 532 nm laser. UV-visible spectroscopy of the samples was done using a Jasco V-750 spectrometer. X-ray photoelectron spectroscopy (XPS) was analyzed by a Thermo Fischer Scientific ESCALAB Xi+ instrument. All electrochemical studies were performed using a CHI-660E potentiostat (CH-instrument, USA) and a three-electrode cell comprising a saturated calomel (SCE) reference electrode, a Pt wire counter electrode, and a working electrode.
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4

Fabrication and Electrochemical Characterization of SAH Electrodes

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Fabrication of the working electrode consisted of physically mixing 40 mg of prepared SAH with 5 mg of carbon black. Separately, polyvinylidene difluoride (PVDF) binder was dissolved in N, N-dimethylacetamide (99% pure) (DMAC) using a 1:10 ratio forming a gel-like consistency to transform the mixed carbon materials into a paste. Once the electrode paste was procured, it was transferred into the tip of a borosilicate capillary (outer diameter of 1.0 mm and inner diameter of 0.58 mm) resulting in a mass loading of 0.18 mg. The weight of the capillary was recorded before and after packing to obtain the mass of the electrode material added. The electrical contact was established by inserting a silver wire into the capillary.
The electrochemical performance of SAHs was tested using a three-electrode configuration via cyclic voltammetry (CV) and galvanostatic charge–discharge (GCD) techniques using CHI 660E potentiostat (CH Instruments, Austin, TX, USA) in 6 M KOH. The counter electrode was platinum, and the reference electrode was a saturated calomel electrode. Specific capacitance can be calculated as presented below, where C is the specific capacitance (F/g), I is the current density (A), Δ t is the discharge time, m is the mass of the active material in the working electrode (g), and Δ V is the potential (V) within the discharge time excluding the IR drop.
C=I×Δtm×ΔV
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5

Electrochemical Capacitor Characterization

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The EC was tested by using a CHI 660E Potentiostat (CH Instruments Inc., China). For Cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) measurements, the electrochemical windows were controlled to be 0 − 1.5 V. EIS tests were performed in the frequency range of 105 to 1 Hz at an amplitude of 5 mV and bias voltage of 0 V. CV tests of connected ECs in series or in parallel were carried out by using a Keithley 2450. For the AC-line filtering test, all the input AC signals were supplied by an arbitrary function generator (33511B, Agilent Technologies Inc., Tektronix, USA). For the AC line filtering test of connected ECs, the input signals were enlarged by an ATA-2041 high-voltage amplifier (Agitek, China). All the outputs were recorded by a RTB2002 mixed domain oscilloscope (Rohde & Schwarz, Germany). The above tests were performed in ambient temperature of 25 °C.
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6

Electrode Preparation and Characterization

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Electrodes were 2 mm, 0.6 mm, or 25 μm diameter platinum disks (CH Instruments) or a cochlear implant with 22 half band, 0.3 mm2 nominal area platinum electrodes (donated by Cochlear, Ltd.). One electrode of each type was tested. The electrodes were freshly polished before every experiment ensuring reproducible starting conditions. Disk electrodes were polished with 0.3 μm alumina slurry on Microcloth polishing cloth (Buehler), rinsed in deionised water and gently dried (Kimwipe) before use; the cochlear implant was not mechanically polished before use and had not been used for any in vivo studies. Acid polishing was achieved by cycling the electrode potential from 1.2 to -0.2 V at 50 mV s-1 for 50 cycles in 0.5 M H2SO4. Electrodes were tested in a 3-electrode configuration on a CHI660E potentiostat (CH Instruments) using a Ag/AgCl (3 M KCl) as reference electrode and Pt wire as counter electrode. The electrodes were connected to the potentiostat via alligator clips and placed into a beaker of solution.
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7

Nanopipet Electrochemical Characterization

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All electrochemical experiments were conducted with CHI660E potentiostat (CH Instruments, TX, USA) in a three-electrode system using a lab-built Ag/AgCl electrode as the reference electrode and a Pt wire (Alfa Aesar, MA, USA) as the counter electrode. Each experiment was conducted with at least 4 nanopipets in triplicate (at least 12 runs in total).
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8

Electrochemical Characterization of Platinum Electrodes

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Hexaammineruthenium(III) chloride (Ru(NH 3 ) 6 Cl 3 ), phosphate buffered saline (PBS: 154 mM NaCl, 10 mM phosphate buffer, pH 7.4), sodium chloride, potassium chloride, sodium bicarbonate, calcium chloride, D-glucose (Sigma-Aldrich), magnesium chloride hexahydrate (Scharlau), monosodium phosphate (Biochemicals) and 98% sulfuric acid (RCI Labscan), were used as received. An artificial perilymph contained 125 mM NaCl, 3.5 mM KCl, 25 mM NaHCO 3 , 1.2 mM MgCl 2 , 1.3 mM CaCl 2 , 0.75 mM NaH 2 PO 4 and 5 mM glucose [18] . Electrodes were 2 mm, 0.6 mm or 25 µm diameter platinum discs (CH Instruments) or a cochlear implant with 22 half band, 0.3 mm 2 nominal area platinum electrodes (donated by Cochlear Ltd). One electrode of each type was tested. Disc electrodes were polished with 0.3 µm alumina slurry on Microcloth polishing cloth (Buehler), rinsed in deionised water and gently dried (Kimwipe) before use; the cochlear implant has not been used for in vivo studies and was not mechanically polished before use. Electrodes were tested in a 3 electrode configuration on a CHI660E potentiostat (CH Instruments) using a Ag/AgCl (3 M KCl) as reference electrode and Pt wire as counter electrode. The electrodes were connected to the potentiostat via alligator clips and placed into a beaker of solution. Unless indicated, test solutions were degassed with nitrogen for at least 10 min.
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