Solid-state synthesis of nitrogen-doped graphitic nanotubes with outstanding electrochemical properties

Synthesis of new anodes is crucial for commercialization of rechargeable potassium-ion batteries (PIBs). In this work, the nitrogen-doped graphitic nanotubes (NGTs) were synthesized by solid-state reaction method. The microstructural characterization of synthesized NGTs revealed the presence of many active sites (provided by N-doping i.e. N_p and N_g) and tubular channels for the K⁺ ion transport. The NGTs electrode was tested against potassium metal in the presence of carbonate based electrolytes. The NGTs revealed the maximum reversible capacity of 220 mA h g^?1 at 20 mA g^?1 current density. Furthermore, the cycle stability of NGTs was confirmed by cycling it for 200 times at the current density of 100 mA g^?1, where specific capacity of 81.2 mA h g^?1 was retained. The excellent electrochemical properties (rate capability) and fast synthesis of NGTs highlights its possibility to be used against post-lithium metal anodes in near future.     

Mechanisms of electrochemical nitrogen gas reduction to ammonia under ambient conditions: a focused review

Journal of Solid State Electrochemistry - Electrocatalytic nitrogen reduction reaction (E-NRR) to ammonia is becoming a major topic of interest in the field of large-scale energy storage from...     

Zn nanosheets:An earth-abundant metallic catalyst for efficient electrochemical ammonia synthesis

Ammonia(NH₃),a critical raw material for various industrial chemicals,is also recognized as a clean and efficient energy carrier for the future energy economy[1].However,the industrial-scale production of NH₃ strongly relies on the Haber-Bosch process,which involves massive fuel consumption and enormous greenhouse gas emissions[2].Therefore,there is an urgent need to develop sustainable and energy-saving alternative routes for artificial NH3 production.     

Solid-state synthesis of a ladder polymer

Solid-state synthesis of a cyclically bound ladder polymer from a cyclic tetradiyne (cyclodotriaconta-1,3,9,11,17,19,25,27-octayne) is described. Irradiation of the colorless, needlelike monomer crystals with interstitially incorporated chloroform with 50 Mrad of ⁶⁰Co γ-ray radiation results in red-brown polymer fibers in nearly quantitative yield. Infrared, Raman, and x-ray diffraction analyses of the polymer are consistent with polymerization by a 1,4-addition reaction at each diacetylene linkage to produce four fully conjugated chains joined together in pairs by a total of four ? (CH₂)₄? interchain linkages per 4.8-Å polymer repeat unit. Conformationally, it appears that the cyclic tetradiyne monomer polymerizes via a chair form. The results of the mechanical and thermal analyses indicate the presence of unreacted diacetylene functionality in the ladder polymer crystals.     

Low-overpotential electrochemical ammonia synthesis using BiOCl-modified 2D titanium carbide MXene

Electrochemical synthesis of ammonia has the advantages of low energy consumption and promising environmental protection, as compared to the traditional Haber-Bosch process. However, the commercial utilization of this novel system is limited by the low Faradaic efficiency, poor ammonia yield and high overpotential due to the strong N≡N bond and the dominant competing reaction of hydrogen evolution reaction（HER）. Herein, a BiOCl-modified two-dimensional（2D） titanium carbide MXenes nanocomposite（B...     

Low-overpotential electrochemical ammonia synthesis using BiOCl-modified 2D titanium carbide MXene

Electrochemical synthesis of ammonia has the advantages of low energy consumption and promising environmental protection, as compared to the traditional Haber-Bosch process. However, the commercial utilization of this novel system is limited by the low Faradaic efficiency, poor ammonia yield and high overpotential due to the strong N≡N bond and the dominant competing reaction of hydrogen evolution reaction（HER）. Herein, a BiOCl-modified two-dimensional（2D） titanium carbide MXenes nanocomposite（B...     

Solid-state NMR study of Li-assisted dehydrogenation of ammonia borane

The mechanism of thermochemical dehydrogenation of the 1:3 mixture of Li(3)AlH(6) and NH(3)BH(3) (AB) has been studied by the extensive use of solid-state NMR spectroscopy and theoretical calculations. The activation energy for the dehydrogenation is estimated to be 110 kJ mol(-1), which is lower than for pristine AB (184 kJ mol(-1)). The major hydrogen release from the mixture occurs at 60 and 72 °C, which compares favorably with pristine AB and related hydrogen storage materials, such as lithium amidoborane (LiNH(2)BH(3), LiAB). The NMR studies suggest that Li(3)AlH(6) improves the dehydrogenation kinetics of AB by forming an intermediate compound (LiAB)(x)(AB)(1-x). A part of AB in the mixture transforms into LiAB to form this intermediate, which accelerates the subsequent formation of branched polyaminoborane species and further release of hydrogen. The detailed reaction mechanism, in particular the role of lithium, revealed in the present study highlights new opportunities for using ammonia borane and its derivatives as hydrogen storage materials.     

Solid-state mechanochemical synthesis of ferrocene

Solid-state mechanochemical reactions of iron(II) chloride with cyclopentadienides of alkaline metals or thallium, which lead to the formation of ferrocene, were studied. The dependence of the yield of the product on the parameters of mechanical loading for the reaction with cyclopentadienylthallium was determined.     

Solid-state assisted synthesis of oligobenzoates

The solid-state assisted synthesis opens an easy access to oligobenzoates end-capped with gallic acid, protocatechuic acid or 4-hydroxybenzoic acid etherified with long flexible chains – which are important precursors for liquid crystalline materials. The latter may consist of aliphatic, oligoethyleneoxy and semiperfluorinated chains. The rapid preparation of oligoesters with different peripheries is demonstrated.     

Solid-state synthesis of Schiff bases

A new preparative method for the synthesis of Schiff bases by the solid-state interaction of crystalline organic and organometallic aldehydes and amines is suggested. The possibility of direct synthesis of aldimines in the solid state from amine salts without isolation of the free amines is demonstrated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2056–2059, November, 1997.     

Solid-state electrochemical behavior of Keggin-type borotungstic acid single crystal

We demonstrate the electrochemical characteristics of the, poorly described in the literature, mixed-valence proton conducting solid borotungstic acid single crystal, H₅BW₁₂O₄₀ xH₂O, in the absence of liquid electrolyte phase. We performed electrochemical measurements in an all-solid cell with a gold fiber ultramicrodisk (diameter 10, 25, and 40 μm) working electrode, a silver semi-reference disk electrode, and a glassy carbon ring counter electrode. Diagnostic experiments at different scan rates aimed at probing the model of mass transport and potential kinetic limitations. Such bulk parameters as the effective diffusion coefficient of charge propagation and the concentration of mixed-valence redox centers were determined by two methods. The first method is based on the analysis of both Cottrellian and steady-state currents (the mixed-regimes method), and the second method provides the true diffusion coefficient (transport coefficient free of the migration influence) for both the substrate and the product of the electrode reaction. Together, these methods constitute a double potential step chronoamperometry experiment. The data obtained with these electrochemical experiments (effective diffusion coefficients, concentration of mixed-valence redox centers, etc.) can support the results obtained with other techniques (XRD, FTIR, and TGA).     

Solid-state electrochemical detector for carbon monoxide at sub-ppm concentrations

Carbon monoxide reacts with iodine pentoxide at 42°C to produce iodine vapor, which is dtected by a solid-state electrochemical detector, essentially a Pt/AgI/Ag galvanic cell. The response begins to rise steeply 3.7 s after a 1.1-ml gas sample is introduce and reaches a maximum after a further 1.2 s. The response is linearly related to the concentration of carbon monoxide up to 2 ppm from the detection limit of 0.03 ppm. Interferences such as H₂S and C₂H₄ are removed by 5A molecuarl sieve; H₂ (1%), CH₄ (5%) and C₂H₄ (5%) are without effect.     

Solid-state tubular assemblies of thiolactones: synthesis and structural characterization

The synthesis of cyclic thiolactones, 2,5,8-trithiacyclododecane-1,9-dione (4), 2,5,8,14,17,20-hexathiacyclotetracosane-1,9,13,21-tetraone (5), 2,5,8-trithiacyclotetradecane-1,9-dione (6) and 2,5,8,16,19,22-hexathiacyclooctacosane-1,9,15,23-tetraone (7) was achieved by tin-template reaction of 2,2-dibutyl-2-stanna-1,3,6-trithiacyclooctane (1) with corresponding diacyl chlorides. The structures of 12-, 14-, 24- and 28-membered ring systems of 4, 6, 5, and 7, respectively, were investigated by X-ray structure analysis. These investigations revealed that, in the solid-state, thiolactones 4 and 7 form tubular assemblies. However, the crystal structure of 5 forms layered packing dominated by CH?O hydrogen bonds whereas 6 forms three-dimensional network via CH?O hydrogen bonds and van der Waals interactions.     

Microneedle-based electrochemical devices for transdermal biosensing: a review

Many research efforts over the last decade have been devoted to the development of microneedle-based diagnostic devices for minimally invasive transdermal biosensing and for long-term health monitoring. Transdermal biosensing via microneedle allows the development of minimally invasive easy-to-use point-of-care biodevices. The main objective of this short review is to provide a general overview of the most immediate and relevant progress in microneedle-based transdermal biosensing in the last five years. A critical analysis of the recent literature is finally presented.     

Solid-state gas sensors for breath analysis: A review

The analysis of volatile compounds is an efficient method to appraise information about the chemical composition of liquids and solids. This principle is applied to several practical applications, such as food analysis where many important features (e.g. freshness) can be directly inferred from the analysis of volatile compounds.     

Solid-state synthesis of luminescent silicon nitride nanocrystals

Silicon nitride nanocrystals (NCs) have been prepared via in situ nitridation of magnesium followed by a metathesis reaction with sol-gel derived silica particles. Highly luminescent, freestanding β-Si(3)N(4) NCs with complex surface chemistry dominated by Si-H and N-H moieties were isolated upon etching with hydrofluoric acid.     

Solid-state synthesis and properties of SmCoO3

In this paper, perovskite oxide SmCoO₃ was prepared by the solid-state reaction method using Co₂O₃ and Sm₂O₃ as raw materials. The structure and properties of the samples were investigated by XRD, Raman spectral techniques, and DC measurements and so on. The results of XRD and Raman spectra showed that the mixtures of Co₂O₃ and Sm₂O₃ can react to produce a single phase perovskite oxide SmCoO₃ around 1353 K. The single-phase SmCoO₃ changes from an insulator to a semi-conductor and transition occurs around 470 K. The thermal expansion coefficient (2.17 × 10⁻⁵ K⁻¹) of the single-phase SmCoO₃ is approximately equal to that of doped LaGaO₃, but much bigger than that of SDC(Ce_0.85Sm_0.15O₂) above 873 K.     

Solid-state synthesis of novel 3-substituted indoles

Poly(N-bromo-N-ethyl-benzene-1,3-disulfonamide) [PBBS] and N,N,N’,N’-tetrabromobenzene-1,3-disulfonamide [TBBDA] were used as efficient catalysts for the one-pot synthesis of 3-substituted indoles in good to high yields from indole, aldehydes, and arylamines under solid-state conditions at room temperature.     

Non-enzymatic electrochemical immunoassay using noble metal nanoparticles: a review

Electrochemical immunodetection has attracted considerable attention due to its high sensitivity, low cost and simplicity. Large efforts have recently made in order to design ultrasensitive assays. Noble metal nanoparticles (NM-NPs) offer advantages such as high conductivity and large surface-to-volume ratio. NM-NPs therefore are excellent candidates for developing electrochemical platforms for immunodetection and as signal tags. The use of biofunctionalized NM-NPs often results in amplified recognition via stronger loading of signal tags, and also in enhanced signal. This review (with 87 references) gives an overview on the current state in the use of NM-NPs in Non-enzymatic electrochemical immunosensing. We discuss the application of NM-NPs as electrode matrices and as electroactive labels (either as a carrier or as electrocatalytic labels), and compare the materials (mainly nanoparticles of gold, platinum, or of bimetallic materials) in terms of performance (for example by increasing sensitivity via label amplification or via high densities of capture molecules). A conclusion covers current challenges and gives an outlook. Rather than being exhaustive, the review focuses on representative examples that illustrate novel concepts and promising applications. NM-NPs based immunosensing opens a series of concepts for basic research and offers new tools for determination of trace amounts of protein-related analytes in environment and clinical applications.

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