Investigation of Polyoxometalate-(Poly)pyrrole Heterogeneous Nanostructures as Cathodes for Rechargeable Magnesium-Ion Batteries

2018 ◽  
Author(s):  
Hakeem K. Henry ◽  
Sang Bok Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Active Material ◽  
Conductive Polymer ◽  
Current Collector ◽  
Constant Current ◽  
Anodized Aluminum ◽  
Transmission Electron ◽  
Pyrrole Monomer

The PMo<sub>12</sub>-PPy heterogeneous cathode was synthesized electrochemically. In doing so, the PMo<sub>12</sub> redox-active material was impregnated throughout the conductive polymer matrix of the poly(pyrrole) nanowires. All chemicals and reagents used were purchased from Sigma-Aldrich. Anodized aluminum oxide (AAO) purchased from Whatman served as the porous hard template for nanowire deposition. A thin layer of gold of approximately 200nm was sputtered onto the disordered side of the AAO membrane to serve as the current collector. Copper tape was connected to the sputtered gold for contact and the device was sealed in parafilm with heat with an exposed area of 0.32 cm<sup>2</sup> to serve as the electroactive area for deposition. All electrochemical synthesis and experiments were conducted using a Bio-Logic MPG2 potentiostat. The deposition was carried out using a 3-electrode beaker cell setup with a solution of acetonitrile containing 5mM and 14mM of the phosphomolybdic acid and pyrrole monomer, respectively. The synthesis was achieved using chronoamperometry to apply a constant voltage of 0.8V vs. Ag/AgCl (BASi) to oxidatively polymerize the pyrrole monomer to poly(pyrrole). To prevent the POM from chemically polymerizing the pyrrole, an injection method was used in which the pyrrole monomer was added to the POM solution only after the deposition voltage had already been applied. The deposition was well controlled by limiting the amount of charge transferred to 300mC. Following deposition, the AAO template was removed by soaking in 3M sodium hydroxide (NaOH) for 20 minutes and rinsed several times with water. After synthesis, all cathodes underwent electrochemical testing to determine their performance using cyclic voltammetry and constant current charge-discharge cycling in 0.1 M Mg(ClO<sub>4</sub>)<sub>2</sub>/PC electrolyte. The cathodes were further characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and x-ray photoelectron spectroscopy (XPS).

Investigation of Polyoxometalate-(Poly)pyrrole Heterogeneous Nanostructures as Cathodes for Rechargeable Magnesium-Ion Batteries

2018 ◽  
Author(s):  
Hakeem K. Henry ◽  
Sang Bok Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Active Material ◽  
Conductive Polymer ◽  
Current Collector ◽  
Constant Current ◽  
Anodized Aluminum ◽  
Transmission Electron ◽  
Pyrrole Monomer

The PMo<sub>12</sub>-PPy heterogeneous cathode was synthesized electrochemically. In doing so, the PMo<sub>12</sub> redox-active material was impregnated throughout the conductive polymer matrix of the poly(pyrrole) nanowires. All chemicals and reagents used were purchased from Sigma-Aldrich. Anodized aluminum oxide (AAO) purchased from Whatman served as the porous hard template for nanowire deposition. A thin layer of gold of approximately 200nm was sputtered onto the disordered side of the AAO membrane to serve as the current collector. Copper tape was connected to the sputtered gold for contact and the device was sealed in parafilm with heat with an exposed area of 0.32 cm<sup>2</sup> to serve as the electroactive area for deposition. All electrochemical synthesis and experiments were conducted using a Bio-Logic MPG2 potentiostat. The deposition was carried out using a 3-electrode beaker cell setup with a solution of acetonitrile containing 5mM and 14mM of the phosphomolybdic acid and pyrrole monomer, respectively. The synthesis was achieved using chronoamperometry to apply a constant voltage of 0.8V vs. Ag/AgCl (BASi) to oxidatively polymerize the pyrrole monomer to poly(pyrrole). To prevent the POM from chemically polymerizing the pyrrole, an injection method was used in which the pyrrole monomer was added to the POM solution only after the deposition voltage had already been applied. The deposition was well controlled by limiting the amount of charge transferred to 300mC. Following deposition, the AAO template was removed by soaking in 3M sodium hydroxide (NaOH) for 20 minutes and rinsed several times with water. After synthesis, all cathodes underwent electrochemical testing to determine their performance using cyclic voltammetry and constant current charge-discharge cycling in 0.1 M Mg(ClO<sub>4</sub>)<sub>2</sub>/PC electrolyte. The cathodes were further characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and x-ray photoelectron spectroscopy (XPS).

scholarly journals 3D Modeling of Silver Doped ZrO2 Coupled Graphene-Based Mesoporous Silica Quaternary Nanocomposite for a Nonenzymatic Glucose Sensing Effects

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 193
Author(s):  
Kamrun Nahar Fatema ◽  
Chang-Sung Lim ◽  
Yin Liu ◽  
Kwang-Youn Cho ◽  
Chong-Hun Jung ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Mesoporous Silica ◽  
Photoelectron Spectroscopy ◽  
Glucose Sensor ◽  
Diffuse Reflectance Spectroscopy ◽  
Active Material ◽  
Glucose Sensing ◽  
X Ray ◽  
Transmission Electron

We described the novel nanocomposite of silver doped ZrO2 combined graphene-based mesoporous silica (ZrO2-Ag-G-SiO2,) in bases of low-cost and self-assembly strategy. Synthesized ZrO2-Ag-G-SiO2 were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, Nitrogen adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS), and Diffuse Reflectance Spectroscopy (DRS). The ZrO2-Ag-G-SiO2 as an enzyme-free glucose sensor active material toward coordinate electro-oxidation of glucose was considered through cyclic voltammetry in significant electrolytes, such as phosphate buffer (PBS) at pH 7.4 and commercial urine. Utilizing ZrO2-Ag-G-SiO2, glucose detecting may well be finished with effective electrocatalytic performance toward organically important concentrations with the current reaction of 9.0 × 10−3 mAcm−2 and 0.05 mmol/L at the lowest potential of +0.2 V, thus fulfilling the elemental prerequisites for glucose detecting within the urine. Likewise, the ZrO2-Ag-G-SiO2 electrode can be worked for glucose detecting within the interferometer substances (e.g., ascorbic corrosive, lactose, fructose, and starch) in urine at proper pH conditions. Our results highlight the potential usages for qualitative and quantitative electrochemical investigation of glucose through the ZrO2-Ag-G-SiO2 sensor for glucose detecting within the urine concentration.

scholarly journals Novel 3D Structure of Silver Doped ZrO2 Combined Graphene-Based Mesopouros Silica Quaternary Nanocomposite for a Nonenzymatic Glucose Sensing Effects

2021 ◽  
Author(s):  
Won-Chun Oh ◽  
Kwang-Youn Cho ◽  
Saksit Chanthai ◽  
Kamrun Nahar Fatema
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Glucose Sensor ◽  
Diffuse Reflectance Spectroscopy ◽  
Active Material ◽  
3D Structure ◽  
Glucose Sensing ◽  
X Ray ◽  
Transmission Electron

Abstract We described the novel nanocomposite of silver doped ZrO2 combined graphene-based mesoporous silica (ZrO2-Ag-G-SiO2, ZAGS) in bases of low-cost and self-assembly strategy. Synthesized ZAGS were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDX), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, Nitrogen adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS), and Diffuse Reflectance Spectroscopy (DRS). The ZAGS as a enzyme-free glucose sensor active material toward coordinate electro-oxidation of glucose was considered through cyclic voltammetry in significant organic electrolytes, such as phosphate-buffer (PBS) at pH 7.4 and commercial urine. Utilizing ZAGS, glucose detecting may well be finished with effective electrocatalytic performance toward organically important concentrations with the current reaction of 9.0 × 10-3 mAcm-2 and discovery restrain of 0.05 mmol/L at the lowest potential of +0.2 V, thus fulfilling the elemental prerequisites for glucose detecting within the urine. Likewise, ZAGS cathodes can be worked for glucose detecting within the nearness of interferometer substances (e.g., ascorbic corrosive, lactose and starch) in urine at proper pH condition. Our results highlight the potential usages for subjective and quantitative electrochemical investigation of glucose through the ZAGS sensor for glucose detecting stage permitted within the urine concentration.

scholarly journals Amorphous Ni x Co y P-supported TiO2 nanotube arrays as an efficient hydrogen evolution reaction electrocatalyst in acidic solution

2019 ◽  
Vol 10 ◽  
pp. 62-70 ◽  
Author(s):  
Yong Li ◽  
Peng Yang ◽  
Bin Wang ◽  
Zhongqing Liu
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Hydrogen Evolution ◽  
Hydrogen Evolution Reaction ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Nanotube Arrays ◽  
Active Surface Area ◽  
X Ray ◽  
Transmission Electron

Bimetallic phosphides have been attracting increasing attention due to their synergistic effect for improving the hydrogen evolution reaction as compared to monometallic phosphides. In this work, NiCoP modified hybrid electrodes were fabricated by a one-step electrodeposition process with TiO2 nanotube arrays (TNAs) as a carrier. X-ray diffraction, transmission electron microscopy, UV–vis diffuse reflection spectroscopy, X-ray photoelectron spectroscopy and scanning transmission electron microscopy/energy-dispersive X-ray spectroscopy were used to characterize the physiochemical properties of the samples. The electrochemical performance was investigated by cyclic voltammetry, linear sweep voltammetry, and electrochemical impedance spectroscopy. We show that after incorporating Co into Ni–P, the resulting Ni x Co y P/TNAs present enhanced electrocatalytic activity due to the improved electron transfer and increased electrochemically active surface area (ECSA). In 0.5 mol L−1 H2SO4 electrolyte, the Ni x Co y P/TNAs (x = 3.84, y = 0.78) demonstrated an ECSA value of 52.1 mF cm−2, which is 3.8 times that of Ni–P/TNAs (13.7 mF cm−2). In a two-electrode system with a Pt sheet as the anode, the Ni x Co y P/TNAs presented a bath voltage of 1.92 V at 100 mA cm−2, which is an improvment of 79% over that of 1.07 V at 10 mA cm−2.

scholarly journals Synthesis of nickel/gallium nanoalloys using a dual-source approach in 1-alkyl-3-methylimidazole ionic liquids

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dual Source ◽  
Induced Decomposition

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.

Limitations to the use of Sb as a Surfactant During SiGe MBE

1998 ◽  
Vol 533 ◽  
Author(s):  
Glenn G. Jernigan ◽  
Conrad L. Silvestre ◽  
Mohammad Fatemi ◽  
Mark E. Twigg ◽  
Phillip E. Thompson
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Transmission Electron Microscopy ◽  
Quantum Well ◽  
Photoelectron Spectroscopy ◽  
Surface Coverage ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Alloy Concentration

AbstractThe use of Sb as a surfactant in suppressing Ge segregation during SiGe alloy growth was investigated as a function of Sb surface coverage, Ge alloy concentration, and alloy thickness using xray photoelectron spectroscopy, x-ray diffraction, and transmission electron microscopy. Unlike previous studies where Sb was found to completely quench Ge segregation into a Si capping layer, we find that Sb can not completely prevent Ge segregation while Si and Ge are being co-deposited. This results in the production of a non-square quantum well with missing Ge at the beginning and extra Ge at the end of the alloy. We also found that Sb does not relieve strain in thin films but does result in compositional or strain variations within thick alloy layers.

scholarly journals Biosynthesized Highly Stable Au/C Nanodots: Ideal Probes for the Selective and Sensitive Detection of Hg2+ Ions

Nanomaterials ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 245 ◽  
Author(s):  
Sada Venkateswarlu ◽  
Saravanan Govindaraju ◽  
Roopkumar Sangubotla ◽  
Jongsung Kim ◽  
Min-Ho Lee ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Metal Ions ◽  
Fluorescent Probe ◽  
Photoelectron Spectroscopy ◽  
Industrial Development ◽  
Carbon Nanodots ◽  
Detection Mechanism ◽  
X Ray ◽  
Transmission Electron

The enormous ongoing industrial development has caused serious water pollution which has become a major crisis, particularly in developing countries. Among the various water pollutants, non-biodegradable heavy metal ions are the most prevalent. Thus, trace-level detection of these metal ions using a simple technique is essential. To address this issue, we have developed a fluorescent probe of Au/C nanodots (GCNDs-gold carbon nanodots) using an eco-friendly method based on an extract from waste onion leaves (Allium cepa-red onions). The leaves are rich in many flavonoids, playing a vital role in the formation of GCNDs. Transmission electron microscopy (TEM) and Scanning transmission electron microscopy-Energy-dispersive X-ray spectroscopy (STEM-EDS) elemental mapping clearly indicated that the newly synthesized materials are approximately 2 nm in size. The resulting GCNDs exhibited a strong orange fluorescence with excitation at 380 nm and emission at 610 nm. The GCNDs were applied as a fluorescent probe for the detection of Hg2+ ions. They can detect ultra-trace concentrations of Hg2+ with a detection limit of 1.3 nM. The X-ray photoelectron spectroscopy results facilitated the identification of a clear detection mechanism. We also used the new probe on a real river water sample. The newly developed sensor is highly stable with a strong fluorescent property and can be used for various applications such as in catalysis and biomedicine.

scholarly journals Heterogeneous Fenton-like oxidation of p-hydroxybenzoic acid using Fe/CeO2-TiO2 catalyst

2019 ◽  
Vol 79 (7) ◽  
pp. 1276-1286 ◽  
Author(s):  
Tijani Hammedi ◽  
Mohamed Triki ◽  
Mayra G. Alvarez ◽  
Jordi Llorca ◽  
Abdelhamid Ghorbel ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Catalytic Properties ◽  
Molar Ratio ◽  
Hydroxybenzoic Acid ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Temperature Programmed

Abstract This paper is built on the Fenton-like oxidation of p-hydroxybenzoic acid (p–HBZ) in the presence of H2O2 and 3%Fe supported on CeO2-TiO2 aerogels under mild conditions. These catalysts were deeply characterized by X-ray diffraction (XRD), hydrogen temperature programmed reduction (H2-TPR), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and X-ray photoelectron spectroscopy (XPS). The effect of thermal treatment, pH (2–3, 5, 7), H2O2/p–HBZ molar ratio (5, 15, 20, 25) and reaction temperature (25 °C, 40 °C and 60 °C) on the catalytic properties of supported Fe catalysts are studied. Our results highlight the role of CeO2 and the calcination of the catalyst to obtain the highest catalytic properties after 10 min: 73% of p–HBZ conversion and 52% of total organic carbon (TOC) abatement.

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