The electrochemistry of 1-butyl-3-methyl-1H-imidazolium tetrafluoroborate (BmimBF 4 ) ionic liquid was investigated by cyclic voltammetry and Osteryoung square wave voltammetry. Impurity chloride was identified, its concentration was determined and a way to eliminate it was demonstrated. Constant current electrolysis of BmimBF 4 was performed and products were analyzed by 1 H, 13 C, and 19 F-NMR and gas chromatography-mass spectrometry. BF 3 and fluorocarbons are produced at the anode while Bmim ϩ undergoes dimerization and dealkylation reactions at the cathode after reduction to a carbene.
The strong interactions between microperoxidase (MP-11) and Tb-mesoMOF were identified via Raman spectroscopic studies, which revealed that MP-11 molecules interact with the framework of Tb-mesoMOF through π···π interactions between the heme of MP-11 and the conjugated triazine and benzene rings in the organic ligand of Tb-mesoMOF. The strong interactions facilitate the retention of MP-11 molecules within the metal-organic framework (MOF) pores, which is in striking contrast with the severe leaching of MP-11 from MCM-41 due to the lack of specific interactions between enzyme molecules and the mesoporous silica material.
NiSe@NiOOH core-shell hyacinth-like nanostructures supported on nickel foam (NF) have been successfully synthesized by a facile solvothermal selenization and subsequent in situ electrochemical oxidation (ISEO). First, the unique NiSe/NF nanopillar arrays were prepared in N,N-dimethylformamide (DMF) as a precursor template that can provide a large surface area, excellent conductivity, and robust support. Next, amorphous NiOOH covering the surface of NiSe nanopillars was fabricated by ISEO, as confirmed by XPS andEDX spectroscopy. SEM images revealed the hyacinth-like morphology of NiSe@NiOOH/NF with NiOOH as the shell and NiSe as the core. The electrochemical performance of NiSe@NiOOH/NF for the oxygen evolution reaction (OER) was investigated. NiSe@NiOOH/NF demonstrates an obviously enhanced OER activity with much lower overpotential of 332 mV at 50 mA cm(-2) compared to other Ni-based electrocatalysts. The low charge-transfer resistance (Rct), large electrochemical double-layer capacitance (Cdl) of electrochemically active surface areas (ECSAs), and excellent long-term stability of NiSe@NiOOH/NF confirm the enhancement of its electrochemical performance for the OER, which can be ascribed to the large amount of active sites derived from the amorphous NiOOH shell and the good conductivity and stability derived from the NiSe core. In addition, the synergistic effect between the NiSe core and NiOOH shell could serve for a highly efficient OER electrocatalyst.
Gold nanoparticles have been used as effective surface-enhanced Raman spectroscopy (SERS) substrates for decades. However, the origin of the enhancement and the effect of the size of nanoparticles still need clarification. Here, gold nanoparticles with different sizes from 17 to 80 nm were synthesized and characterized, and their SERS enhancement toward both 4-aminothiophenol and 4-nitrothiophenol was examined. For the same number of nanoparticles, the enhancement factor generated from the gold nanoparticles increases as the size of nanoparticles increases. Interestingly, when the concentration of gold or the total surface area of gold nanoparticles was kept the same, the optimal size of gold nanoparticles was found out to be around 50 nm when the enhancement factor reached a maximum. The same size effect was observed for both 4-aminothiophenol and 4-nitrothiophenol, which suggests that the conclusions drawn in this study might also be applicable to other adsorbates during SERS measurements.
A facile two-step method has been used to synthesize binary Ni–Fe sulfides supported on nickel foam (NF) as electrocatalysts for the oxygen evolution reaction (OER).
This paper reports an electrochemical microfluidic paper-based analytical device (EμPAD) for glucose detection, featuring a highly sensitive working electrode (WE) decorated with zinc oxide nanowires (ZnO NWs). In addition to the common features of μPADs, such as their low costs, high portability/disposability, and ease of operation, the reported EμPAD has three further advantages. (i) It provides higher sensitivity and a lower limit of detection (LOD) than previously reported μPADs because of the high surface-to-volume ratio and high enzyme-capturing efficiency of the ZnO NWs. (ii) It does not need any light-sensitive electron mediator (as is usually required in enzymatic glucose sensing), which leads to enhanced biosensing stability. (iii) The ZnO NWs are directly synthesized on the paper substrate via low-temperature hydrothermal growth, representing a simple, low-cost, consistent, and mass-producible process. To achieve superior analytical performance, the on-chip stored enzyme (glucose oxidase) dose and the assay incubation time are tuned. More importantly, the critical design parameters of the EμPAD, including the WE area and the ZnO-NW growth level, are adjusted to yield tunable ranges for the assay sensitivity and LOD. The highest sensitivity that we have achieved is 8.24 μA·mM, with a corresponding LOD of 59.5 μM. By choosing the right combination of design parameters, we constructed EμPADs that cover the range of clinically relevant glucose concentrations (0−15 mM) and fully calibrated these devices using spiked phosphate-buffered saline and human serum. We believe that the reported approach for integrating ZnO NWs on EμPADs could be well utilized in many other designs of EμPADs and provides a facile and inexpensive paradigm for further enhancing the device performance.
Hydrogen peroxide electroreduction on both catalytically active Pt and inactive Au surfaces are studied by using both surface-enhanced Raman spectroscopy (SERS) and density functional theory (DFT) calculations. SERS measurements on Pt show the presence of Pt-OH at negative potentials, which suggests that hydroxide is formed as an intermediate during the electroreduction process. Additionally, the O-O stretch mode of H(2)O(2) is observed on Pt, which shifts to lower energy as potential is swept negatively, indicating that the O-O bond is elongated. For comparison, there is no variation in the energy of the same O-O mode on Au surfaces, and there is no observation of Au-OH. DFT calculations show that H(2)O(2) adsorption on Pt(110) results in the dissociation of O-O bond and the formation of Pt-OH bond. On Au, O-O bond elongation is calculated to occur only on the (110) face. However, the magnitude of the elongation is much smaller than that found on Pt(110).
In situ cathodic activation (ISCA) of V-incorporated NiS nanowires supported on nickel foam (VS/NiS/NF) can be realized in an alkaline hydrogen evolution reaction (HER) process, which provides not only clearly enhanced activity but also ultrahigh stability for HER. The ISCA process is continuous linear sweep voltammetry (LSV) on VS/NiS/NF as a cathodic electrode with gradually enhanced HER activity. The activated VS/NiS/NF (A-VS/NiS/NF) demonstrates enhanced HER activity with an overpotential of 125 mV to drive 10 mA cm, which is much lower than that of other samples. It may be predicted that the ISCA-derived amorphous VOOH film covering on A-VS/NiS/NF accelerates the HER process, and NiOOH may protect active sites from decaying, leading to excellent activity and structural stability. However, for single metal sulfides, the ISCA process of nickel or vanadium sulfides is not available, implying that the synergistic effect between Ni and V of VS/NiS/NF may be the key to drive ISCA in alkaline HER. In addition, its ultra-high stability confirms that the stable active sites and nanostructures of A-VS/NiS/NF are derived from ISCA. Therefore, the ISCA of V-incorporated transition metal sulfides in the alkaline HER process may be a facile and promising method to obtain efficient electrocatalysts.
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