An immunochromatographic strip (ICS) using urchin-like gold nanoparticles (UGNs) for sensitive detection of fumonisin B1 (FB1) was developed to meet the requirement for rapidly monitoring FB1 in grain samples. The sensitivity of the ICS was 5.0 ng/mL, which represents a fourfold increase in sensitivity over conventional strip preparation using colloidal gold as the antibody-labeled probe. Analysis of FB1 in grain samples showed that data obtained from the strip tests were in a good agreement with those obtained from HPLC and enzyme-linked immunosorbent assays (ELISAs). This qualitative test did not require any specialized equipment, and the detection time was less than 5 min, which is suitable for on-site testing of FB1 in grain samples. Overall, to our knowledge, this is the first report of using a UGN as the antibody-labeled probe for sensitive detection of FB1 in grains using an ICS.
LiNi1-x-yCoxMnyO2 (NCM) with excessive lithium is known to exhibit high rate capability and charge–discharge cycling durability. However, the practical usage of NCM is difficult, because the positive electrode slurry is unstable and battery cells swell due to the alkaline residual lithium compound generated on the surface of NCM particles. To reduce the residual lithium compound, ammonium metatungstate (AMT) added to NCM is studied, and the effect is investigated by scanning electron microscopy, aberration-corrected scanning transmission electron microscopy, X-ray diffractometry, synchrotron X-ray diffractometry, and several electrochemical measurements. It is found that the AMT modification reduces the amount of alkaline residual lithium compound and improves the rate capability due to the ~1-nm-thick W-rich layer generated on the NCM surface.
Herein, porous Li3V2(PO4)3/C microspheres made of nanoparticles are obtained by a combination of sol spray-drying and subsequent-sintering process. Beta-cyclodextrin serves as a special chelating agent and carbon source to obtain carbon-coated Li3V2(PO4)3 grains with the size of ca. 30–50?nm. The unique porous structure and continuous carbon skeleton facilitate the fast transport of lithium ion and electron. The Li3V2(PO4)3/C microspheres offer an outstanding electrochemical performance, which present a discharge capacity of 122?mAh?g?1 at 2?C with capacity retention of 96% at the end of 1000 cycles and a high-rate capacity of 113?mAh?g?1 at 20?C in the voltage window of 3.0–4.3?V. Moreover, the Li3V2(PO4)3/C microspheres also give considerable cycling stability and high-rate reversible capacity at a higher end-of-charge voltage of 4.8?V.
The authors report on the fabrication of Co(OH)2-enfolded Cu2O nanocubes on reduced graphene oxide (rGO), and the use of this material in an electrochemical caffeine sensor. The rGO/Cu2O/Co(OH)2 composite was characterized by X-ray powder diffraction pattern analysis, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy and Raman spectroscopy. A rotating disc glassy carbon electrode covered with the nanocomposite displays enhanced electrocatalytic activity towards the electro-oxidation of caffeine. The peak oxidation potential is at 1.4 V (vs. Ag/AgCl) and hence is strongly shifted to the negative side when compared to other modified electrodes. The calibration plot is linear in the 0.83 to 1200 μM concentration range, with a 0.4 μM detection limit (at a signal-to-noise ratio of 3). The modified electrode is sensitive, selective and stable. It was successfully applied to the determination of caffeine in (spiked) caffeine-containing beverages and coffee powder and gave recoveries that ranged from 95.7 to 98.3 %.
Sulfonated polyvinylchloride (SPVC) cation-exchange membranes were coated using chitosan solutions comprising different amounts of Fe3O4 nanoparticles. Influence of chitosan immobilization as well as nanofiller concentration on the electrochemical performance of the membranes was investigated. Electrochemical properties of the membranes including permselectivity, ionic permeability, and areal resistance were studied using an equipped electrodialysis setup and NaCl solution as model electrolyte. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were employed for membrane characterization. Electrochemical performance of the SPVC membranes was improved by coating chitosan polymer. In addition, ionic permeability and permselectivity of the membranes were initially raised by increasing nanoparticles concentration from nil to 2 wt% and then decreased by further insertion of the nanofiller. The areal resistance of the plain SPVC membrane was decreased from 9.4 to 2.9 (ohm) by coating of chitosan solution including optimum value of nano-Fe3O4 due to electrical potential field enhancement across the membrane.
Bismuth ferrite (BiFeO3) nanopowder have been successfully synthesized for the first time via a microwave-assisted sol-gel combustion method by using citric acid as fuel. The resulting nanopowder was characterized using FT-IR, TG-DTA, XRD, EDX, VSM, SEM, and UV-Vis DRS. A ferromagnetic hysteresis loop with a saturation magnetization (MS) of 0.66?emu?g?1 has been observed at room temperature in the sample. The optical properties of the nanosized BiFeO3 showed its small band gap (=2.08?eV) indicates a possibility of utilizing much visible light for photocatalysis.
Co2(OH)3Cl xerogel interconnected mesoporous structures have been prepared by a facile one pot sol-gel process and heat treated at 200 and 400 °C. All samples are studied for their morphology, structure, and electrochemical stability upon cycling. The specific capacitance of the as-prepared Co2(OH)3Cl from single electrode study is 450 F/g, when the electrodes are cycled in 3 M KOH at a specific current 2 A/g. Interestingly, capacity retention after 500 and 1000 cycles is about 92 and 75 %, respectively. Sample heated at 200 °C exhibits 308 F/g at 2 A/g and that heated at 400 °C shows only 32 F/g at 0.2 A/g. With an increase in preparation temperature, amorphous Co2(OH)3Cl is converted to crystalline Co3O4 phases with lower electrochemical performance. In full cell study, as-prepared Co2(OH)3Cl showed a capacity of about 49 F/g as asymmetric capacitor and 32 F/g as symmetric capacitor at 2 A/g current density. Co2(OH)3Cl being a novel porous material with merits of homogeneous porosity, high surface area, and an interconnected three dimensional (3D) structure exhibits considerably high capacitance. With a significant specific capacity and electrochemical stability, the synthesized material is a novel potential candidate for supercapacitors.
Generally adopted strategies to improve capacitance of the electrode materials are tuning various properties of the electrode material or increasing the cell voltage. While tuning the properties of the electrode material is tedious, increasing the cell voltage is restricted by the stability of the electrolyte. Herein, we report a facile approach to improve the capacitance of MnCO3 by the influence of SiOx nanofluid in the electrolyte. The capacitance properties of MnCO3 are studied in 0.1 M Mg(ClO4)2 electrolyte in the presence and in the absence of SiOx nanofluid. The presence of small amount of SiOx nanofluid in the electrolyte provides higher diffusivity and more conductive percolation paths for ions and thus decreases internal resistance and increases ionic conductivity of the electrolyte. As a result, 60% enhancement in the capacitance is witnessed for MnCO3. Further, nanofluid containing electrolyte is found to be stable over a month.
Magnesium hydroxide and magnesium oxide nanostructures have been prepared by microwave/hydrothermal technique using magnesium metal in hydrogen peroxide (H2O2). The applied power of the microwave was 700?W for 10?min at 145?°C. The method produced Mg(OH)2 powder as a base material for MgO by calcinations at 550?°C for 2?h. X-ray diffraction data confirms the microwave production of Mg(OH)2 and (MgO) through the agreement with the standard JCDPS cards. Scanning electron microscopy shows nanoplates morphology for Mg(OH)2 and large-scale nanoplates with a hexagonal shape for MgO. The fundamental direct optical band gap of Mg(OH)2 equals 5.8?eV while for MgO equals 5.2?eV from the analysis of diffused reflectance data. MgO has higher dielectric constant than Mg(OH)2 at the higher frequencies. AC electrical conductivity increases with increasing the applied frequency for both materials. The microwave-hydrothermal technique shows a promising method for production of magnesium compounds from magnesium metal which can be used in different aspects such as catalysis, wastewater treatment, pharmaceutical and coated materials.
A novel photoelectrochemical (PEC) aptasensor with graphitic-phase carbon nitride quantum dots (g-C3N4; QDs) and reduced graphene oxide (rGO) was fabricated. The g-C3N4 QDs possess enhanced emission quantum yield (with an emission peak at 450 nm), improved charge separation ability and effective optical absorption, while rGO has excellent electron transfer capability. Altogether, this results in improved PEC performance. The method is making use of an aptamer against sulfadimethoxine (SDM) that was immobilized on electrode through π stacking interaction. Changes of the photocurrent occur because SDM as a photogenerated hole acceptor can further accelerate the separation of photoexcited carriers. Under optimized conditions and at an applied potential of +0.2 V, the aptasensor has a linear response in the 0.5 nM to 80 nM SDM concentration range, with a 0.1 nM detection limit (at S/N =?3). The method was successfully applied to the analysis of SDM in tap, lake and waste water samples.
Graphical abstract Graphitic-phase carbon nitride (g-C3N4) quantum dots (QDs) and reduced graphene oxide (rGO) were used to modify fluorine-doped SnO2 (FTO) electrodes for use in a photoelectrochemical (PEC) aptasensor. SDM oxidized by the hole on valance band (VB) of g-C3N4 QDs promote the separation of electron in the conductive band (CB), which made the changes of photocurrent signal.
A photoelectrochemical wire microelectrode was constructed based on the use of a TiO2 nanotube array with electrochemically deposited CdSe semiconductor. A strongly amplified photocurrent is generated on the sensor surface. The microsensor has a response in the 0.05–20 μM dopamine (DA) concentration range and a 16.7 μM detection limit at a signal-to-noise ratio of 3. Sensitivity, recovery and reproducibility of the sensor were validated by detecting DA in spiked human urine, and satisfactory results were obtained.
Graphical abstract Schematic of a sensitive photoelectrochemical microsensor based on CdSe modified TiO2 nanotube array. The photoelectrochemical microsensor was successfully applied to the determination of dopamine in urine samples.
The authors describe double-shell magnetic nanoparticles functionalized with 2-mercaptobenzothiazole (MBT) to give nanospheres of the type MBT-Fe3O4@SiO2@C). These are shown to be viable and acid-resistant adsorbents for magnetic separation of the heavy metal ions Ni(II), Cu(II) and Pb(II). MBT act as a binding reagent, and the carbon shell and the silica shell protect the magnetic core. Following 12 min incubation, the loaded nanospheres are magnetically separated, the ions are eluted with 2 M nitric acid and then determined by inductively coupled plasma-mass spectroscopy. The limits of detection of this method are 2, 82 and 103 ng L￣1 for Ni(II), Cu(II), and Pb(II) ions, respectively, and the relative standard deviations (for n = 7) are 6, 7.8, and 7.4 %. The protocol is successfully applied to the quantitation of these ions in tap water and food samples (mint, cabbage, potato, peas). Recoveries from spiked water samples ranged from 97 to 100 %.
Graphical abstract Mercaptobenzothiazole-functionalized magnetic carbon nanospheres of type Fe3O4@SiO2@C were synthesized. Then applied for magnetic solid phase extraction of Ni(II), Cu(II) and Pb(II) from water and food samples with LOD of 0.002, 0.082 and 0.103 μg L?1 respectively.
The three-dimensional porous Li3V2(PO4)3/nitrogen-doped reduced graphene oxide (LVP/N-RGO) composite was prepared by a facile one-pot hydrothermal method and evaluated as cathode material for lithium-ion batteries. It is clearly seen that the novel porous structure of the as-prepared LVP/N-RGO significantly facilitates electron transfer and lithium-ion diffusion, as well as markedly restrains the agglomeration of Li3V2(PO4)3 (LVP) nanoparticles. The introduction of N atom also has positive influence on the conductivity of RGO, which improves the kinetics of electrochemical reaction during the charge and discharge cycles. It can be found that the resultant LVP/N-RGO composite exhibits superior rate properties (92 mA h g?1 at 30 C) and outstanding cycle performance (122 mA h g?1 after 300 cycles at 5 C), indicating that nitrogen-doped RGO could be used to improve the electrochemical properties of LVP cathodes for high-power lithium-ion battery application.
Graphical abstract The three-dimensional porous Li3V2(PO4)3/nitrogen-doped reduced graphene oxide composite with significantly accelerating electron transfer and lithium-ion diffusion exhibits superior rate property and outstanding cycle performance.
The authors describe magnetic nanoparticles consisting of an Fe3O4 core and a poly(methacrylic acid) coating for dispersive solid phase extraction (DSPE) of arsenic prior to its determination by hydride-generation microwave plasma AES (HG-MP-AES). The particles have an average size of 25 nm, can be prepared at low costs, and provide improved operational safety in combination with plasma generation. The methods allows arsenic to be determined with detection limits (at 3σ/m) of 3.0 ng?L?1 for As(III) and of 10.0 ng?L?1 of As(V). Recoveries of (spiked) samples range from 99.0 to 102%. This is the first report on the use of HG-MP-AES for speciation and preconcentration of arsenic using DSPE. The method displays detection limits that come close to those of ICP-OES and ICP-MS.
Graphical abstract A core/shell Fe3O4@poly(methacrylic acid) coated sorbent was synthesised and employed to the speciation of arsenic prior to its determination by hydride-generation microwave plasma atomic emission spectrometry.
CdSe is an important semiconductor for photoelectrochemistry. Here, we propose a two-step method for preparing thin films of aggregated CdSe nanoparticles on Cd electrodes. We first anodized the Cd electrode in an aqueous solution of 0.2 M KNO3 at ?0.9 V (vs. Hg|Hg2SO4(s)|K2SO4 (saturated)) into a porous and layered structure covered with Cd(OH)2 precipitation, and then selenized the Cd(OH)2 deposited on the Cd anode in an aqueous solution of 0.2 M Na2SeSO3. The resulting CdSe nanoparticles self-assembled into strawberry-like nanoaggregates. The anodization time and selenization time were optimized separately. Under our experimental conditions, the optimized anodization time was 80 s, whereas the optimized selenization time ranged from 15 to 60 min, corresponding to the partial or complete conversion of the deposited Cd(OH)2 into smaller and larger strawberry-like CdSe nanoaggregates, respectively. The optimized partially and completely selenized films showed photocurrent responses that were enhanced in different ways but demonstrated comparable performances. They presented an anodic photocurrent density as high as 3.2 mA cm?2 at ?0.3 V with good stability under visible light illumination of 100 mW cm?2 in a solution containing a sacrificial reagent of ascorbic acid.
Graphical Abstract Strawberry-like CdSe nanoaggregates were prepared by selenizing the anodization film of Cd(OH)2 on Cd electrode and they demonstrated enhanced photoelectrochemical performance.
Hetero-dimeric magnetic nanoparticles of the type Au-Fe3O4 have been synthesised from separately prepared, differently shaped (spheres and cubes), monodisperse nanoparticles. This synthesis was achieved by the following steps: (a) Mono-functionalising each type of nanoparticles with aldehyde functional groups through a solid support approach, where nanoparticle decorated silica nanoparticles were fabricated as an intermediate step; (b) Derivatising the functional faces with complementary functionalities (e.g. amines and carboxylic acids); (c) Dimerising the two types of particles via amide bond formation. The resulting hetero-dimers were characterised by high-resolution TEM, Fourier transform IR spectroscopy and other appropriate methods.
Graphical Abstract Nano-LEGO: Assembling two types of separately prepared nanoparticles into a hetero-dimer is the first step towards complex nano-architectures. This study shows a solid support approach to combine a gold and a magnetite nanocrystal.
A method is described for the fluorometric determination of hypochlorite. It is making use of molybdenum disulfide quantum dots (MoS2 QDs) as a fluorescent probe. The QDs are prepared by hydrothermal reaction of sodium molybdate with glutathione. They possess diameters typically ranging from 1.4 to 3.8 nm, excellent stability in water, and blue photoluminescence (with excitation/emission peaks located at 315/412 nm and a quantum yield of 3.7%). The fluorescence of the QDs is statically quenched by hypochlorite, and the Stern-Volmer plot is linear. Hypochlorite can be detected in the 5–500 μM concentration range with a 0.5 μM detection limit. The method has been successfully applied to the determination of hypochlorite in spiked samples of tap water, lake water, and commercial disinfectants.
Graphical abstract Schematic of a method for the fluorometric determination of hypochlorite using MoS2 quantum dots as a fluorescent probe. It has been applied to hypochlorite assay in spiked samples of tap water, lake water, and commercial disinfectants.
A porous, hollow, microspherical composite of Li2MnO3 and LiMn1/3Co1/3Ni1/3O2 (composition: Li1.2Mn0.53Ni0.13Co0.13O2) was prepared using hollow MnO2 as the sacrificial template. The resulting composite was found to be mesoporous; its pores were about 20 nm in diameter. It also delivered a reversible discharge capacity value of 220 mAh g?1 at a specific current of 25 mA g?1 with excellent cycling stability and a high rate capability. A discharge capacity of 100 mAh g?1 was obtained for this composite at a specific current of 1000 mA g?1. The high rate capability of this hollow microspherical composite can be attributed to its porous nature.
CaMn7O12 precursor sol was prepared by using Ca(NO3)2·4H2O and Mn(CH3COO)4·4H2O as the raw materials, acetylacetone (AcAcH) as the chelating agent, and methyl alcohol (MeOH) as the solvent. The CaMn7O12 crystalline film was obtained via dip-coating and annealing treatment on the LaAlO3 (001) single-crystal substrate. XRD θ-2θ scan indicated that the as-prepared CaMn7O12 film had strong preferred orientation along the c-axis. In addition, the results of the ω and ? scans demonstrated that the film exhibited outstanding out-of-plane and in-plane texture characteristics. The SEM characterization showed that the CaMn7O12 film was dense and free of cracks. The grain size was uniform with an average size of ~180?nm. Vibrating sample magnetometer (VSM) test results indicated the CaMn7O12 film was antiferromagnetic and had a saturation magnetization of 114.2?emu/cm3 at 50?K.
The structural and electrochemical effects of electrospun V2O5 with selected redox-inactive dopants (namely Na+, Ba2+ and Al3+) have been studied. The electrospun materials have been characterised via a range of analytical methods including X-ray diffraction, X-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area measurements and scanning and transmission electron microscopy. The incorporation of dopants in V2O5 was further studied with computational modelling. Structural analysis suggested that the dopants had been incorporated into the V2O5 structure with changes in crystal orientation and particle size, and variations in the V4+ concentration. Electrochemical investigations using potentiodynamic, galvanostatic and impedance spectroscopy analysis showed that electrochemical performance might be dependent on V4+ concentration, which influenced electronic conductivity. Na+- or Ba2+-doped V2O5 offered improved conductivities and lithium ion diffusion properties, whilst Al3+ doping was shown to be detrimental to these properties. The energetics of dopant incorporation, calculated using atomistic simulations, indicated that Na+ and Ba2+ occupy interstitial positions in the interlayer space, whilst Al3+ is incorporated in V sites and replaces a vanadyl-like (VO)3+ group. Overall, the mode of incorporation of the dopants affects the concentration of oxygen vacancies and V4+ ions in the compounds, and in turn their electrochemical performance.
