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3 protocols using ultrapure water

1

Synthesis and Characterization of Metal Compounds

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Sodium tungstate dihydrate (Na2WO4·2H2O) was purchased from Alfa Aesar India, and tin (II) chloride hydrate (SnCl2·2H2O) was purchased from Alfa Aesar United States. Hydrochloric acid (HCl, ~35% v/v) and ammonium sulfate ((NH4)2SO4) were purchased from Duksan. Carbon cloth (WOS1009) was obtained from CeTech Co., Ltd., and sodium sulfate (Na2SO4, anhydrous, ≥99%) was from Honeywell/Fluka. Potassium ferricyanide (K3Fe(CN)6, 99%) was purchased from Acros Organics. All of these chemicals were used without further purification. Aqueous solutions were freshly prepared with ultrapure water (resistivity of 18.2 MΩcm; Yamato, Japan) throughout the experiments. Characterization was performed over the range 2θ = 10° to 60° at room temperature with an X-ray diffractometer (XRD, Bruker, D2 phaser Karlsruhe, German) using a copper radiation source (λ = 0.154 nm), operating at 40 kV and 30 mA, with a step size of 0.05 and step time of 5 sec.; X-ray photoelectron spectroscopy (XPS, VG scientific ESCALAB 250, Birmingham, UK); and field emission scanning electron microscopy (FE-SEM, at 15 kV acceleration voltage) equipped with an energy-dispersive X-ray spectroscopy (EDS) analyzer (JSM-6500F, JEOL, Tokyo, Japan).
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2

Synthesis and Characterization of Transition Metal Oxides

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Titanium(iv) isopropoxide (TTIP, ACROS ORGANICS, CHINA), isopropanol (≥99.8% (GC), Honeywell|Riedel-de Haën™, France), sodium tungstate oxide dihydrate (Na2WO4·2H2O, 99.0–101.0%, Thermo Fisher Scientific.), ethanol (≥99.9%, Honeywell|Fluka™, Germany), nitric acid (65% w/w), hydrochloric acid (37%, reagent grade), ethylene glycol (99.5%, ACROS ORGANICS), methylene blue (ACROS ORGANICS, INDIA), and methyl orange (ACROS ORGANICS, INDIA) were used without further purification. Para-benzoquinone (p-BQ) and ethylenediaminetetraacetic acid disodium salt (Na2-EDTA) were purchased from Sigma-Aldrich and Fisher Chemical, respectively. Ultrapure water (resistivity of 18.2 mΩ cm, Yamato, Japan) was used throughout the experiments.
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3

Nickel Foam Electrode Preparation

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The reagents nickel(II)
nitrate hexahydrate (Ni(NO3)2·6H2O, Alfa), cobalt(II) nitrate hexahydrate (Co(NO3)2·6H2O, Acros), manganese(II) nitrate tetrahydrate
(Mn(NO3)2·4H2O, Alfa Aesar),
sodium nitrate (NaNO3, Acros), and potassium hydroxide
(KOH, Fisher Chemical) were of analytic grade and were used as received
without further purification. Nickel foam (110 PPI, approximately
1.7 mm × 1 cm × 3 cm, Fucell CO., Ltd.) was washed with
6 M hydrochloric acid solution (HCl, Fisher Chemical) in an ultrasonic
bath for 30 min to remove the NiO layer on the surface and then subsequently
rinsed with deionized water and isopropanol (Acros Organics) for 10
min in an ultrasonic bath and dried at room temperature. The Ni foam
was covered with a Kapton film with adhesive to control the surface
area to be exposed to the electrolyte solution. Throughout the experiments,
ultrapure water with a resistivity of 18.2 MΩ·cm (Yamato,
Japan) was used.
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