Chemistry Commons^™

Investigation Of The Ideal Composition Of Metal Hexacyanocobaltates With High Water Oxidation Catalytic Activity, Ferdi̇ Karadaş

Turkish Journal of Chemistry

The electrocatalytic activities of Prussian blue analogues (PBAs) have recently received much attention due to their robustness and efficiency. Considering that PBAs with hexacyanocobaltate building block stand forward among other PBAs, a systematic study on a family of metal hexacyanocobaltates is presented in this study. Metal hexacyanocobaltates (M $=$ Co, Mn, Ni, and Fe) were prepared, characterized, and electrochemical studies were performed. A series of mixed-metal cobalt-iron hexacyanocobaltates has also been studied to determine the ideal composition of a metal hexacyanocobaltate for electrocatalytic water oxidation process. The overall study clearly indicates that cobalt hexacyanocobaltate exhibits the highest electrocatalytic activity among …

Palladium Adatoms On Gold Nanoparticles As Electrocatalysts For Ethanol Electro-Oxidation In Alkaline Solutions, Hui-Mei Chen, Shang-Qian Zhu, Jia-Le Huang, Min-Hua Shao

Journal of Electrochemistry

Palladium (Pd) is a good catalyst for ethanol electro-oxidation in alkaline solutions. The activity of Pd is further improved in this study by modifying the gold (Au) nanoparticles with Pd adatoms using a simple spontaneous deposition process. The Pd overlayer on the Au core (Au@Pd) is un-uniform with some Au atoms exposed to the electrolyte. The activity of Au@Pd/C toward ethanol oxidation reaction (EOR) is much higher than that of Pd/C in an alkaline solution. The peak current density of Au@Pd/C is 4.6 times higher than that of Pd/C with a 100 mV lower onset potential. The enhanced activity may …

Recent Advances In Non-Noble Metal Nanomaterials For Oxygen Evolution Electrocatalysis, Dan-Dan Zhao, Nan Zhang, Ling-Zheng Bu, Qi Shao, Xiao-Qing Huang

Journal of Electrochemistry

Hydrogen is a kind of renewable energies with the merits of environmentally friendly, abundance and high weight energy density, which can replace the fossil energy. The electrolysis of water is regarded as the most effective way to generate hydrogen. Owing to the sluggish kinetics and large overpotential of the anode oxygen evolution reaction (OER), the efficiency of the cathode hydrogen evolution reaction is greatly limited. Therefore, it is highly desirable to explore efficient, stable and low cost electrocatalysts to reduce the overpotential of OER and improve the efficiency of hydrogen evolution. Based on the natural characteristics of non-noble metal catalysts …

Highly Crystalline Nickel Borate Nanorods As Oxygen Evolution Reaction Electrocatalysts, Xi Xu, Juan Liu, Hua-Zong Wu, Wen-Jie Jiang

Journal of Electrochemistry

Hydrogen energy, a kind of clean and renewable energy, is considered to be the solution to the problems of energy crisis and environmental deterioration. Electrochemical water splitting is an efficient and promising technology for the production of high-purity hydrogen. However, oxygen evolution reaction (OER) at the anode of water electrolyzer limits the efficiency of water splitting due to the high overpotential. Therefore, the challenges still remain for the exploration of highly active, stable and low-cost catalysts with superior activity for OER. Herein, nickel borate nanorods with high crystallinity were prepared via high-temperature calcination. The as-obtained nickel borate nanorods with 2 …

Preparation Of Ni(Dpim)2Cl2 Complex For The Electrocatalytic Reduction Of Co2, Li-Pu Zhang, Dong-Fang Niu, Xin-Sheng Zhang

Journal of Electrochemistry

A new Ni(dpim)₂Cl₂complex using 2-(diphenylphosphino)-1-methylimidazole (dpim) as ligand was prepared and served as a catalyst for the electrochemical reduction of CO₂. The electrochemical redox behavior of Ni(dpim)₂Cl₂ in CH₃CN/TPABF₄ solution under nitrogen atmosphere showed the two-electron irreversible reduction at -0.7 V and one-electron quasi-reversible reduction at -1.3 V. After bubbling CO₂ into the electrolyte, the reduction peak appeared at -1.3 V became irreversible and the peak current increased from 0.48 mA·cm^-2 to 0.55 mA·cm^-2. Moreover, the peak current at -1.3 V could further increase …

Fabrication Of Cuox-Pd Nanocatalyst Supported On A Glassy Carbon Electrode For Enhanced Formic Acid Electro-Oxidation, Islam M. Al-Akraa Dr., Ahmad M. Mohammad Prof, Mohamed S. El-Deab Prof, Bahgat E. El-Anadouli Prof

Chemical Engineering

Formic acid (FA) electro-oxidation (FAO) was investigated at a binary catalyst composed of palladium nanoparticles (PdNPs) and copper oxide nanowires (CuOxNWs) and assembled onto a glassy carbon (GC) electrode. /e deposition sequence of PdNPs and CuOxNWs was properly adjusted in such a way that could improve the electrocatalytic activity and stability of the electrode toward FAO. Several techniques including cyclic voltammetry, chronoamperometry, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction were all combined to report the catalyst’s activity and to evaluate its morphology, composition, and structure. /e highest catalytic activity and stability were obtained at the CuOx/Pd/GC …

Carbon Quantum Dots: Bridging The Gap Between Chemical Structure And Material Properties, Timothy J. Pillar-Little Jr.

Theses and Dissertations--Chemistry

Carbon quantum dots (CQDs) are the latest generation of carbon nanomaterials in applications where fullerenes, carbon nanotubes, and graphene are abundantly used. With several attractive properties such as tunable optical property, edge-functionalization, and defect-rich chemical structure, CQDs have the potential to revolutionize optoelectronics, electro- and photocatalysis, and biomedical applications. Chemical modifications through the addition of heteroatoms, chemical reduction, and surface passivation are found to alter the band gap, spectral position, and emission pathways of CQDs. Despite extensive studies, fundamental understanding of structure-property relationship remains unclear due to the inhomogeneity in chemical structure and a complex emission mechanism for CQDs.

This …

Cobalt-Based Nitrogen-Doped Carbon Non-Noble Metal Catalysts For Oxygen Reduction Reaction, Meng-Xiu Jiang, Jing Zhang, Yue-Hua Li, Rong Zhang

Journal of Electrochemistry

Transition metal-nitrogen co-doped carbon catalysts have attracted significant attention because of their reasonable activity and remarkable selectivity toward oxygen reduction reaction (ORR) as cathodic reaction in fuel cells. However, the role of transition metal in the active sites of the catalysts still is uncertain. In this work, the Co_x-N_y/C-T catalysts were prepared with BP2000 as a carbon source, urea (Ur) as a nitrogen source and Co(OAc)₂•4H₂O as a metal precursor by a simple chemical method. Meanwhile, in order to optimize the ORR activity, the catalysts were synthesized with different amounts of Co …

Core-Shell Pd@Pt Ultrathin Nanowires As Durable Oxygen Reduction Electrocatalysts, Xin Wang, Yun-Jie Xiong, Liang-Liang Zou, Qing-Hong Huang, Zhi-Qing Zou, Hui Yang

Journal of Electrochemistry

This paper describes a simple CO-assisted reduction approach for the controllable synthesis of ultrathin Pd nanowires along the one-dimensional (1D) direction. Ultrathin Pt films from one to several atomic layers were successfully decorated onto ultrathin Pd nanowires by utilizing Cu UPD deposition, and followed by in-situ redox replacement reaction of UPD Cu by Pt. The core–shell structure and composition of the Pd@Pt ultrathin nanowires have been verified using transmission electron microscopy and energy dispersive X-ray spectrometry. The core–shell Pd@Pt ultrathin nanowires exhibited comparative electrocatalytic activity and improved durability for the oxygen reduction reaction in comparison with commercial Pt black. The …

Metal-Organic Frameworks And Mof-Derived Carbon Materials For Fuel Cell Applications, Kia Williams

USF Tampa Graduate Theses and Dissertations

Rapid industrial globalization and technological development and energy consumption across the globe has significantly increased in response to mounting energy needs. The necessity for alternative and sustainable energy conversion devices has become apparent with the growth of energy utilization. In recent years, many research efforts have been made in the development of low-cost, efficient, environmentally friendly energy conversion devices. One type of energy conversion device, polymer electrolyte membrane fuel cells (PEMFCs), uses hydrogen oxidation at the anode and oxygen reduction at the cathode, with a solid-state proton conducting membrane between to generate energy with water as a by-product. PEMFCs use …

Electrocatalysis Of Nanotin Dioxide In The Battery Reaction Of Zinc-Nitrobenzene, Xu-Guo Tu, Xiang-Yu Ma, Rui-Nan He, Xiao-Juan Wang, Chen Ling, Yun-Xia Sun, Song Chen

Journal of Electrochemistry

The tin dioxide (SnO₂) nanoparticles were synthesized by using a simple hydrothermal route in the presence of tetrapropyl ammonium bromide (TPAB) as a surfactant. Accordingly, the titanium mesh based SnO₂ catalyst electrode was prepared. The morphologies and structures of SnO₂ nanostructures were characterized by scanning electron microscopy and X-ray diffraction spectrometry. The influences of reactant concentration, reaction temperature and time on the morphology of the products were investigated in detail. The electrocatalytic performance of SnO₂ for the reduction of nitrobenzene with zinc was studied. Possible formation process and growth mechanism for such hierarchical SnO_{2 …}

Homogeneous Ligand-Centered Hydrogen Evolution And Hydrogen Oxidation : Exploiting Redox Non-Innocence To Drive Catalysis., Andrew Z. Haddad

Electronic Theses and Dissertations

Hydrogen is a promising carbon-free fuel / energy carrier and is an essential building block for many industrial and agricultural processes. Rising energy demands have ignited interest in the development of carbon-free and carbon neutral energy sources. In this context, hydrogen is an attractive candidate—being energy-dense, carbon-free—and easily accessible through a two-electron reduction of water. Accordingly, many electrochemical homogeneous catalyst systems have been studied, with a focus on understanding the mechanism of hydrogen evolution proceeding through metal-hydride intermediates. However, there has been a renaissance in hydrogen evolution reaction (HER) catalyst design, with many groups implicating ligand redox non-innocence as a …

Green Electrochemical Ozone Production Via Water Splitting: Mechanism Studies, Gregory Gibson, Wenfeng Lin

Journal of Electrochemistry

The green and energy-efficient water splitting reaction using electrocatalysis for O₃ formation provides a very attractive alternative to the conventional energy-intensive cold corona discharge (CCD) method. Among a large number of electrocatalysts explored for the electrochemical ozone production, β-PbO₂ and SnO₂-based catalysts have proven to be the most efficient ones at room temperature. In this study Density Functional Theory (DFT) calculations have been employed to investigate the possible mechanisms of ozone formation over these two types of catalysts. For both the β-PbO₂ and Ni/Sb-SnO₂ (nickel and antimony doped tin oxide) catalysts the (110) facet …

Electrochemical Nanoprobes For Electron Transfer Kinetics And Electrocatalysis Study, Yun Yu

Dissertations, Theses, and Capstone Projects

The studies of electrochemical processes on the nanoscale have led to a significant progress in understanding of electrochemical mechanisms and characterization of nanomaterials in the fields of energy, catalysis, and biological research. Electrochemical experiments at nanoscale require the fabrication and characterization of nanometer-sized electrochemical probes. The main advantages of the nanoprobes include very fast mass-transfer rate, high signal-to-noise ratio and extremely fine spatial resolution of electrochemical imaging. In the course of my Ph.D. research, different types of electrochemical probes were developed for measuring electron-transfer kinetics, probing single catalytic nanoparticles and sampling ultra-small volume of liquids.

We developed methodologies to fabricate …

Preparation Parameters Optimization And Electrocatalytic Properties Of Supported Au Nanoparticles, Rui Yao, Yu-Jiang Song, Huan-Qiao Li, Jia Li, Jian-Guo Liu

Journal of Electrochemistry

Due to interesting size effect, physical and chemical properties, nano-scale gold materials have been commonly used to catalytic reactions. However, the application of gold nanomaterials in the field of electrocatalysis is limited. Herein, we report the synthesis of gold nanparticles supported on carbon through chemical reduction of HAuCl₄ by NaBH₄ under mild conditions in the presence of surfactants as soft templates, carbon black or graphene as a support. We investigated a series of key reaction parameters, including reagent concentration, temperature, the types of carbon supports and surfactants. With the optimum synthetic parameters, we successfully obtained supported 1 ~ …

Recent Progresses In Molybdenum-Based Electrocatalysts For The Hydrogen Evolution Reaction, Ze-Xing Wu, Jie Wang, Jun-Po Guo, Jing Zhu, De-Li Wang

Journal of Electrochemistry

Electrochemical catalytic production of hydrogen has been considered as a promising and sustainable strategy for clean and renewable energy technologies. Molybdenum-based non noble metal catalysts for the hydrogen evolution reaction have attracted extensive attention due to its effective catalytic performance. In this review, the recent progresses in molybdenum-carbide, phosphide, nitride and sulfide electrocatalysts are presented. In addition, the strategies to improve the catalytic performance are analyzed and the prospects for the future development trends are expected.

Robust Nickel Catalysts Supported By Biaryl-Bridged Pyridyl-N-Heterocyclic Carbenes For Carbon Dioxide Reduction To Value-Added Products, Hunter Allen Dulaney

Electronic Theses and Dissertations

Carbon dioxide is a greenhouse gas, but also represents a readily accessible C1 feedstock for conversion to solar fuels and value-added chemicals. However, CO2 is relatively inert and very negative voltages or strong chemical reductants are comfor its conversion. An additional challenge lies in achieving these reactions in water where aqueous protons are utilized selectively for CO2 reduction rather than hydrogen generation. Our strategy for CO2 reduction involves the design of new homogeneous catalysts with tunable geometries and polyaromatic frameworks with increased delocalization to lower overpotentials for catalysis. We report a family of biaryl-bridged pyridyl-N-heterocyclic carbene-based ligands and their corresponding …

Synthesis Of Palladium And Palladium-Copper Nanostructures As Electrocatalysts, Haibin Wu

Graduate Theses and Dissertations

Pd and its alloys are alternatives of Pt as promising catalysts and electrocatalysts for many reactions. Size controlled synthesis of nanoparticles remains a major research subject, since smaller size particles show better catalytic performance. In this work, we developed a modified chemical wet method to prepare Pd and Pd-Cu nanostructures with uniform small size. Different sizes and shapes of Pd nanostructures were successfully synthesized by using the two reducing agents (i.e., L-ascorbyl-6-palmitate or phenylphosphinic acid). The reducing agents play a role to control the final morphologies and sizes of particles. The use of L-ascorbyl-6-palmitate favors to form irregular branch shapes …

Kinetic Study Of The Oxygen Reduction Reaction On Α-Ni(Oh)2 And Α-Ni(Oh)2 Supported On Graphene Oxide, Elaheh Farjami, L. Jay Deiner

Publications and Research

The kinetics of the oxygen reduction reaction on α-Ni(OH)2 and α-Ni(OH)2 supported on graphene oxide (α-Ni(OH)2/GO) were investigated using rotating disk linear sweep voltammetry in alkaline solutions of varying oxygen and hydroxyl concentrations. Over the full hydroxyl concentration range (0.05 M to 0.5M), α-Ni(OH)2/GO displayed higher activity than unsupported α-Ni(OH)2. The electron transfer numbers were 2.9 ± 0.2 for α-Ni(OH)2, 3.4 ± 0.1 for α-Ni(OH)2/GO at low [OH−], and 3.8–3.9 for α-Ni(OH)2/GO at high [OH−]. Compared to α-Ni(OH)2, α-Ni(OH)2/GO displayed higher chemical reaction rate constants and higher electron transfer rate constants. These differences suggest that the synergy between the α-Ni(OH)2 …

On The Catalytic Activity Of Palladium Nanoparticles-Based Anodes Towards Formic Acid Electro-Oxidation: Effect Of Electrodeposition Potential, Islam M. Al-Akraa Dr., Ahmad M. Mohammad Prof, Mohamed S. El-Deab Prof, Bahgat E. El-Anadouli Prof

Chemical Engineering

In this investigation, the catalytic activity of palladium nanoparticles (PdNPs)-modified glassy carbon (GC) (simply noted as PdNPs/GC) electrodes towards the formic acid electro-oxidation (FAO) was investigated. The deposition of PdNPs on the GC substrate was carried out by a potentiostatic technique at different potentials and the corresponding influence on the particles size and crystal structure of PdNPs as well as the catalytic activity towards FAO was studied. Scanning electron microscopy (SEM) demonstrated the deposition of PdNPs in spherical shapes and the average particle size of PdNPs deposited at a potential of 0 V vs. Ag/AgCl/KCl(sat.) was the smallest (ca. 8 …

Investigation Of New Ligand Architechtures Towards Proton And Water Reduction Catalysis By Cobalt Complexes, Debashis Basu

Wayne State University Dissertations

We designed several redox-active ligand architectures to optimize and understand the redox, electronic, and catalytic properties of their respective cobalt complexes. Ligand design was varied from pentadentate donor phenolate to tetradentate acceptor oxime in order to reduce the overpotential of hydrogen generation in organic solvents. We altered the substitution, axial ligands and axial ligand substitutions to vary electronic and catalytic properties for such tetra- or pentadentate ligand systems. Knowledge of the nature of the active species for catalysis enabled us to design the pentadentate oxime ligand which exhibited rich reaction chemistry along with suitable catalytic property in organic solvent. Presence …

Electrochemical And Spectroscopic Studies Of Ethanol Oxidation On Nano-Cubic Pt Modified By Tin Adatoms, Lu Rao, Bin-Wei Zhang, Yan-Yan Li, Yan-Xia Jiang, Shi-Gang Sun

Journal of Electrochemistry

The nano-cubic Pt modified by tin (Sn) was synthesized and used to investigate the role of this adatom played in the ethanol oxidation. The onset potential of ethanol oxidation was significantly shifted negatively which can be forward about 300 mV when the coverage of Sn (θSn)was 0.9. The electrtochemical in situ FTIR result demonstrated that the amount of CO₂ increased first, and then decreased with θSn increased, and reached the maximun when θSn was 0.38. Furthermore, the formation of acetic acid could be observed at very low potential (-0.05 V) after modifying Sn adatom, and the amount of acetic …

Synthesis Of Platinum Nanocrystallites And Possible Electrocatalytic Properties For Methanol, Lei-Lei Lu, Bao-Zhong Du, Sha Sun, Jin-Fen Niu, Jie Zhao

Journal of Electrochemistry

Platinum nanocrystallites were synthesized by the colloidal method using oxamide as the stabilizer. The morphologies and electrocatalytic performances for methanol of platinum nanocrystallites prepared at different pH values and with different reactant ratios of precursor and stabilizer were investigated. It was found that the platinum nanocrystallites synthesized at pH=5 and with the reactant ratio of 1:20 showed the best electrocatalytic activity for methanol. The peak current density reached up to 1709 μA·cm^-2. Furthermore, the electrocatalytic activity of platinum nanocrystallites for methanol reduced significantly although the cyclic voltammograms in the blank solution were not obviously changed after exposing in …

Pulse Electrodeposition Of Pd-Ni Alloy Nanoparticles For Electrocatalytic Oxidation Of Formic Acid, Fang-Zu Yang, Jun-Pei Yue, Zhong-Qun Tian, Shao-Min Zhou

Journal of Electrochemistry

The Pd-Ni alloy nanoparticles with nickel atomic contents of 12.0%, 16.4% and 22.6% were successfully electrodeposited from a Pd-Ni alloy electrolyte by square wave pulse plating. The alloy nanoparticles were in the spherical shape with a diameter of 50 ~ 80 nm. As the growth potential of the alloy was negatively shifted, the nickel content of the alloy was increased, and the size of the nanoparticles was almost the same, whereas the number, the degree of crosslinking and the real active area of the nanoparticles were increased. As the nickel content of the alloy nanoparticles increased, the peak current for …

Synthesis And Electrocatalysis Of Pdcu Alloy Nanocrystals, Hai-Bin Wu, Rui-Zhong Zhang, Wei Chen

Journal of Electrochemistry

Monodispersed PdCu alloy nanoparticles were synthesized by co-reduction of Cu(acac)2 and Pd(acac)2 with 1, 2-hexadecanediol. The spherical and popcorn-like shapes of PdCu alloy nanoparticles were obtained by changing the ratios of mixed surface protecting ligands of 1-octadecene, and oleylamine or oleic acid. TEM and XRD measurements showed that both PdCu nanoparticles are alloy nanocrystals dominated with (111) planes and the average sizes are 12.7 ± 0.18 and 20.4 ± 0.31 nm for he spherical and popcorn-like PdCu nanoparticles, respectively. The electrocatalytic activities of the PdCu nanocrystals for formic acid oxidation were evaluated by electrochemical cyclic voltammetry (CV). The result showed …

Preparation And Catalytic Properties Of Feco Alloy Nanocatalyst, Ming-Xuan Li, Jie-Lian Ou, Sheng-Pei Chen, Peng Wang, Bin-Bin Xu, Shi-Gang Sun

Journal of Electrochemistry

The FeCo alloy nanoparticles were electrodeposited on glassy carbon electrode by chronoamperometry and were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The results showed that the shapes of FeCo nanoparticles were cubes with an average size of 65 nm. The atom ratio of Fe and Co is 1:1. As indicated from the pattern of selected area electron diffraction (SAED), the FeCo cubic nanoparticles were single crystal which belonged to body-centered cubic with an interval of 0.201 nm referring to the (110) facets of FeCo alloy. The FeCo cubic nanoparticles exhibited the enhanced electrocatalytic …

An In Situ Ftir Spectroelectrochemical Study On Methanol Oxidation At Pt-Mo2C/Gc Catalyst, Hai-Ping Huang, Xi-Yu Yao, Pei-Kang Shen

Journal of Electrochemistry

A 40% Pt on Mo₂C/GC catalyst has been prepared by ion exchange method. The mechanism of methanol electrooxidation on Pt-Mo₂C/GC and commercial Pt/C catalysts in acidic media was studied by cyclic voltammetry, XRD measurements and in-situ Fourier transform infrared spectroelectrochemistry. The results revealed that the Pt nanoparticles were uniformly dispersed on Mo₂C/GC with an average particle size of 3 nm. The cyclic voltammetric and chronopotentiometric experiments indicated that Pt-Mo₂C/GC catalyst exhibited a better performance for methanol oxidation than that of Pt/C in acid solution. A negative shift over 90 mV of the …

Model Pt- And Pd-Based Electrocatalysts For Low Temperature Fuel Cells Applications, Selasi Ofoe Blavo

USF Tampa Graduate Theses and Dissertations

In the search for alternative energy technologies, low temperature fuel cells continue to feature as technologies with the most promise for mass commercialization. Among the low temperature fuel cells, alkaline and proton exchange membrane fuel cells are the most popular. Alkaline fuel cells have typically been used for water generation as well as auxiliary power for space shuttles. Their bulkiness however makes them undesirable for other applications, especially in automobiles, where there is a great demand for alternative technologies to internal combustion engines. Proton exchange membrane fuel cells on the other hand possess numerous qualities including their compact size, high …

Electrocatalytic Oxidation Of Formic Acid On Pd/Ni Heterostructured Catalyst, Mingjun Ren, Liangliang Zou, Ju Chen, Ting Yuan, Qinghong Huang, Haifeng Zhang, Hui Yang, Songlin Feng

Journal of Electrochemistry

A Pd/Ni bimetallic nanostructured electrocatalyst was fabricated via a two-step reduction route. Owing to an epitaxial growth of Pd atoms on the surface of Ni nanoparticles, heterostructured Pd/Ni nanocomposites were formed and verified by high resolution transmission electron microscopy combined with energy-dispersion X-ray spectroscopy. X-ray diffraction confirmed that the as-prepared Pd/Ni nanocomposites possessed a single face-centered-cubic (fcc) Pd structure, probably due to a weaker diffraction intensity of metallic Ni and/or overlapping by that of Pd. The intrinsic catalytic activity on the Pd/Ni is higher than that on the Pd. Moreover, the durability of formic acid oxidation on the Pd/Ni was …

Electrochemical Properties Of The Keggin-Type Lacunary Heteropolysilicate Anion And Its Eectrocatalysis For H2O2 Reduction, Xi-Long Liu, Chun-Yan Wu, Fang Zhou, Hong-Sheng Liu, Ying-Jie Hua, Chong-Tai Wang, Xiao-Yang Liu

Journal of Electrochemistry

Electrochemical properties of the Keggin-type lacunary heteropolysilicate anion SiW₁₁O₃₉^8- (SiW₁₁) and its indirect electrocatalysis for H₂O₂ reduction in the supporting electrolyte containing 0.1 mol·L^-1 NaHSO₄ and Na₂SO₄ solutions were investigated using cyclic voltammetry, square wave voltammetry and alternating current impedance spectroscopy. Experimental results indicated that SiW₁₁ showed two pairs of reversible redox waves on the glassy carbon (GC) electrode in an acidic solution. The electron transfer number corresponding to the two pairs of waves was one, and the proton transfer number involved was two during …