Silver nanoparticles/polymethacrylic acid (AgNPs/PMA) hybrid nanocomposites-modified electrodes for the electrochemical detection of nitrate ions

AgNPs/PMA hybrid nanocomposite materials with different Ag loadings have been synthesized using a simple chemical route assisted by UV irradiation. The hybrid composites were characterized by means of SEM and TEM, UV–vis spectroscopy and XPS. The as synthesized hybrid samples, composed of small Ag nanoparticles (AgNPs) embedded within the PMA (poly-methacrylic-acid) matrix, have been used to modify the working electrode of disposable screen printed carbon electrodes (SPCEs). It has been observed that hybrid composite with the lowest Ag loading forms dendritic silver structures on the surface of working electrode, whereas at higher loadings massive structures were formed. The electrocatalytic properties of the AgNPs/PMA/SPCEs were investigated toward the reduction of nitrate at neutral pH. Based on these modified electrodes, both voltammetric and amperometric sensors were developed for the electrochemical sensing of nitrate. Voltammetric sensor showed a wide linear range (0–20 mM) and high sensitivity (130 μA mM⁻¹ cm⁻²).     

Preparation,characterization, electrical conductivity and dielectric studies of Na2SO4 and V2O5 composite solid electrolytes

Composite solid electrolytes (1 − x) Na₂SO₄–(x) V₂O₅ were prepared and characterized by various techniques such as XRD, FT-IR, DTA and SEM. AC impedance spectroscopy revealed that the contribution of grain is strong enough over the grain boundary. Arrhenius plot of the Na₂SO₄ shows a sharp increase in conductivity at 523 K due to the structural phase transition (phase V → I). Composites show the enhanced ionic conductivity than the pristine Na₂SO₄ over the entire temperature range. The maximum conductivity σ = 0.003 S cm⁻¹ at 773 K with the lowest activation energy of 0.28 eV was observed for the x = 0.4 sample. The enhanced value of dielectric constant and dielectric loss in the case of composites was obtained because of increase of conductivity, resulted from the increase of space charge polarization and charge motion.     

Extremely low coefficient of friction of diamond sliding against Ag thin films on Si(1 1 1) surface under ultrahigh vacuum condition

The tribological properties of a diamond (1 1 1) pin slid on subnanometer thick Ag films, which were deposited on a cleaned Si(1 1 1) substrate, were studied using a pin-on-plate tribometer. The preparation of Ag ultrathin films and frictional experiments were performed in an ultrahigh vacuum (UHV) chamber at a pressure of 10⁻⁸ Pa. The frictional experiments were carried out at a sliding speed of 0.1 mm/s and at a normal load of 250 mN. An extremely low coefficient of friction, less than 0.01, was obtained when the pin was slid on Ag films, whose thicknesses were 1 and 2.6 monolayer (ML) under reciprocal motion. The minimum coefficient of friction was less than 0.004 for Ag 1 ML film. After the extremely low coefficient of friction was obtained, Ag remained on the worn track without any transfer to the diamond pin, as confirmed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).The mechanisms of extremely low coefficients of friction are discussed in terms of the chemical bonding force between atoms of the topmost layers, and Ag coverage on the Si surface.     

Plasmonic effect of silver nanoparticles on the upconversion emissions of Sm3+-doped sodium-borosilicate glass

The effect of the localized surface plasmon resonance (SPR) on optical absorption and photoluminescence of Sm³⁺-doped sodium borosilicate glass containing reduced silver nanoparticles (NPs) is reported (Ag⁺ → Ag⁰). The interaction of ultraviolet light by metallic NPs and its effect on the optical properties of samarium in proposed glass were investigated by absorption and photoluminescence spectra analysis. The existence of the NPs was pursued by transmission electron microscopy technique, revealing the existence of Ag NPs with average size of ∼8–14 nm. The largest enhancement was achieved for emission at 561 nm. Such improvements were attributed and discussed by enhanced electric field around metallic NPs and energy transfer (ET) between Sm³⁺ ions and silver NPs.     

Multi-range sensors for the measurement of liquid film thickness distributions based on electrical conductance

The paper presents an approach toward an enhancement of the measuring range of high-speed sensors for the measurement of liquid film thickness distributions based on electrical conductance. This type of sensors consists of electrodes mounted flush to the wall. The sampling of the current generated between a pair of neighboring electrode is used as a measure of the film thickness. Such sensors have a limited measuring range, which is proportional to the lateral distance between the electrodes. The range is therefore coupled to the spatial resolution. The proposed new design allows an extension of the film thickness range by combining electrode matrices of different resolution in one and the same sensor. In this way, a high spatial resolution is reached with a small thickness range, whereas a film thickness that exceeds the range of the high resolution measurement can still be acquired even though on the costs of a lower spatial resolution. A simultaneous signal acquisition with a sampling frequency of 3.2 kHz combines three measuring ranges for the characterization of a two-dimensional film thickness distribution: (1) thickness range 0–600 µm, lateral resolution 2×2 mm², (2) thickness range 400–1300 µm, lateral resolution 4×4 mm², and (3) thickness range 1000–3500 µm, lateral resolution 12×12 mm². The functionality of this concept sensor is demonstrated by tests in a horizontal wavy stratified air–water flow at ambient conditions. Using flexible printed circuit board technology to manufacture the sensor makes it possible to place the sensor at the inner surface of a circular pipe.     

Tribological properties of surface-modified Pd nanoparticles for electrical contacts

A fully comprehensive study of the tribological behavior of palladium nanoparticles (Pd NPs) capped by tetrabutylammonium chains using a ball-on-disk tribometer under different conditions of applied load, concentration, tribometer motion, linear speed and nature of the counterface is revised. A low concentration of NPs (2 wt%) in tetrabutylammonium acetate was found sufficient to improve the tribological properties due to the formation of a protective transfer film (TF) comprised of metallic Pd. The increase of the applied load (up to 20 N, 1.82 GPa of contact pressure) confirmed the excellent extreme-pressure behavior avoiding the counterfaces from severe wear. After a running-in period whose duration depends on the operating conditions, the TF build-up allows to maintain a low contact electrical resistance through the contact (<0.1 kΩ) during the entire test. When the Pd NPs are used with ceramic counterfaces, the nanoparticles increase the load-bearing capabilities and performance of the base without forming TF, likely by mixed or boundary lubrication and healing effects. Finally, the Pd NPs are demonstrated to be useful as a thin solid lubricant film in reciprocating motion yielding a comparable tribological behavior. Hence, the presented surface Pd NPs can be very helpful to extend life of sliding components due to their high strength resistance providing a gateway to electrical conduction as well.     

Low wear metal sliding electrical contacts at high current density

Operation of a low wear (2 × 10^?5 mm³/(N-m)), low contact resistance copper sliding electrical contact was demonstrated. The wear rate of a lightly loaded copper–beryllium metal fiber sliding on a polished copper counterface was insensitive to (DC) current density values as great as 440 A/cm² (in a brush positive or anodic configuration). Low wear and relatively low friction (μ ～ 0.2 to 0.3) was achieved by operating the contact immersed in a liquid medium consisting of a hydrofluoroether with helium cover gas, inhibitingoxidationand providing cooling of the contact. Similar experiments performed in liquid mediums of ultrapure water and dilute (3%) hydrogen peroxide show an order of magnitude increase in wear rate and provide further insight on the role of electrochemically enhanced oxidation and the degraded contact resistance and tribological behavior of non-noble sliding electrical contacts in general. In contrast to high current density slidingin hydrofluoroether, an order of magnitude greater wear rate was observed for similar sliding conditionsin hydrogen peroxide or water without the aid of externally supplied electric potential. A conceptual model is proposed correlatingthe rate of brush wear to fatigue strength and electrochemically enhanced oxidation as a result of high current density transport through the contact. A mathematical expression was derived to calculate the approximate wear volume of a single fiber laterally contacting a slip-ring, based on direct measurement of the wear scar geometry.     

Improved dielectric constant of thermoplastic blend as a function of alumina loading

Polycarbonate (PC) and Poly (methyl methacrylate) blends were prepared by incorporating Al₂O₃ into the polymer matrix using solution blending. The modified blends were characterized by X-ray diffraction, Thermogravimetric analysis, and Scanning electron microscopy. The crystalline to amorphous phase variation was confirmed by XRD with increase in the interplanar distance (d). TGA results indicate that the thermal stability of the modified blend was significantly improved as a function of alumina loading which may be due to interfacial interaction between the alumina particles and the polymers. Scanning electron microscopy studies reveal the presence of alumina particles resulting in plane surface morphology. The modified blends show very high dielectric constant value (10⁵–10⁷) as a function of frequency (in the range 50 Hz–35 MHz) and temperature in the range (40–150 °C). The modified polymer blend demonstrate consistent polarization across the frequency band 50 Hz–10 kHz. The neutral aggregates formation due to higher concentration of alumina loading demonstrated an influence on AC conductivity. This investigation can be feasible for electronic and electrical engineering application as the dielectric medium.     

Effect of electrical current on tribological behavior of copper-impregnated metallized carbon against a Cu–Cr–Zr alloy

A block-on-slip ring-type wear tester was used to investigate the tribological behavior of copper-impregnated metallized carbon against a Cu–Cr–Zr alloy under 2 to 6 N applied load and 0 to 20 A electrical current. The sliding speed was maintained at 25 km/h. The wear loss of copper-impregnated metallized carbon increased with greater electrical current. Under a certain applied load, the wear loss with electrical current was minimized. The tribo-layer had an apparent effect on the friction coefficient. The wear mechanisms were complex, consisting of adhesive wear, abrasive wear and arc erosion.     

An investigation into the effect of film thickness on nanowear with amorphous carbon-based coatings

A sample oscillation module linked to a nanoindentation unit was used to perform nano-scale wear testing on a series of sputtered Cr doped amorphous C films deposited over a range of thicknesses (10, 20, 50, 150, and 2000 nm) under conditions relevant to MEMS and micro-scale engineering devices. A ruby sphere was used as the counter-body. Specific wear rates (defined as volume of worn material per unit applied load per unit of slid distance) were quantified and the effect of film thickness, applied load and test duration was investigated. Specific wear rate reduced exponentially with decreasing film thickness over the range of 10–2000 nm. The lowest wear rates were in the range of 0.1–6.1 × 10^?17 m³ N^?1 m^?1. Specific wear rate reduced with increased applied load over the range of 0.1–10 mN. The data scatter of replicated testing reduced along with the reduction of wear rate. A rapid reduction of specific wear rate was observed during the first 3000 oscillation cycles. This was analogous to the ‘running in’ process observed with macroscopic tribology systems.     

Determination of the thermal conductivity of composted material

The objective of this study was to develop a reliable method for the determination of the thermal conductivity of composted material using the TP08 probe. Study was set out to determine whether the selection of a signal fragment used to establish thermal conductivity (λ), has a significant influence on the results. Also minimum number of measurements was determined for every phase of the composting process. No significant differences were reported between results, but certain changes in the value of λ were noted. In successive stages of the process, thermal conductivity of composted material were: 0.31 ± 0.09, 0.45 ± 0.14, 0.27 ± 0.03 and 0.37 ± 0.17 W m⁻¹ K⁻¹.     

Modified nanoporous carbon as a novel sorbent before solvent-based de-emulsification dispersive liquid–liquid microextraction for ultra-trace detection of cadmium by flame atomic absorption spectrophotometry

Combination of different extraction methods is an interesting work in the field of sample pretreatment. In the current study, for the first time, solid phase extraction combined with solvent-based de-emulsification dispersive liquid–liquid microextraction (SPE-SD-DLLME) was developed for preconcentration and trace detection of cadmium in water samples using flame atomic absorption spectrophotometry (FAAS). The adsorbed cadmium ions on prepared SPE (75 mL of aqueous solution) were eluted by optimized elution solvent and introduced to the second microextraction step. The effective variables of SPE including the pH of sample, flow rates, type, concentration and volume of the eluent and the effect of potentially interfering ions of the separation of cadmium were evaluated and optimized. Also, several factors that influence the SD-DLLME step such as pH, neocuproine concentration (the cadmium binding ligand), type of dispersed/de-emulsifier solvent, volume of disperser/de-emulsifier solvent and type and volume of extraction solvents were investigated. SPE-SD-DLLME provides a preconcentration factor of 165 for cadmium ions. Calibration plot was linear in the range of 0.1–50 μg L⁻¹ with correlation of determination (r²) of 0.988. The precision and limit of detection of proposed method were 5.1% (RSD%, n = 8) and 0.03 μg L⁻¹, respectively.     

Study of TiAlSiN coatings post-treated with N and C + N ion implantations. Part 2: The tribological analysis

Ion implantation has found to be an effective approach to modify surface properties of materials. The present research investigates the effect of (1) nitrogen (N), and (2) carbon subsequently with nitrogen (C + N) implantations on the mechanical and tribological properties of the titanium–aluminium–silicon–nitride (Ti–Al–Si–N) coatings. Superhard TiAlSiN coatings produced by magnetron sputtering, of approximately 2.5 μm thickness, were post-treated by implantations of N or C + N at an energy level of 50 keV. The dose range was between 5 × 10¹⁶ and 1 × 10¹⁸ ions cm^?2. After implantation, the tribological performance of the coatings was investigated by a ball-on-disk tribometer against WC–6 wt.%Co ball under dry condition in ambient air. The wear performance of the samples was examined by a variety of characterization techniques, such as secondary electron microscopy (SEM), 3D profilometry, atomic force microscopy (AFM), and micro-Raman. The results showed that the wear performance of the samples depended strongly on the implanted elements and doses. There was slight improvement on the samples implanted with N whereas significant improvement was found on the C + N implantations. Particularly, the friction coefficient of the sample with 5 × 10¹⁷ C⁺ cm^?2 and 5 × 10¹⁷ N⁺ cm^?2 could reach 0.1. In addition, the specific wear rate of the sample was extremely low (0.85 × 10^?7 mm³/Nm), which was nearly two orders of magnitude below that of the un-implanted coating. The speculation of the mechanical and tribological analyses of the samples indicates that the improvement of the N implanted and C + N implanted TiAlSiN samples could be due to a combined effect of improved hardness, plus enhanced adhesive and cohesive strength. In addition, the improved performance of the C + N implanted samples could be explained by the formation of lubricating implanted-layer, which existed mostly in sp² C–C and C–N forms. The formation of such implanted layer could lead to a change of wear mode from strong abrasive wear to mostly adhesive wear, and result in a drop of friction coefficient and wear rate.     

AC conduction mechanism and battery discharge characteristics of (PVC/PEO) polyblend films complexed with potassium chloride

New K⁺ ion-conducting polymer blend electrolyte films based on amorphous polymer poly(vinyl chloride) (PVC) and semicrystalline polymer poly(ethylene oxide) (PEO) complexed with KCl salt were prepared using a solution-cast technique. The maximum value of ionic conductivity of a PVC/PEO:KCl (42.5:42.5:15) system is 8.29 × 10⁻⁶ S/cm at 303 K. The absorption edge was found at 4.30 eV for undoped film, while it was observed at 4.03 and 3.93 eV for 10 and 15 wt% KCl doped films, respectively. The direct band gaps for these pure and salt doped PVC/PEO films were found to 4.10, 3.86 and 3.74 eV, respectively, whereas the indirect band gaps were determined as 4.15, 3.72 and 3.64 eV. Transference number values showed that the charge transport in this electrolyte system is predominantly due to ions (t_ion = 0.97). The discharge capacity for PVC/PEO:KCl (42.5:42.5:15) polymer blend electrolyte system is 11 μA/h.     

Nanocomposite polymer electrolyte based on rice starch/ionic liquid/TiO2 nanoparticles for solar cell application

Nanocomposite polymer electrolyte (NCPE) was prepared using solution cast technique. Rice starch (RS), lithium iodide (LiI), 1-methyl-3-propylimidazolium iodide (MPII) as ionic liquid and TiO₂ nanopowder (RS:LiI:MPII:TiO₂) were introduced to prepare the sample. The conductivity of 3.63 × 10⁻⁴ S/cm was achieved by introducing 30 wt.% of 1-methyl-3-propylimidazolium iodide (MPII) as ionic liquid and 2 wt.% of TiO₂. Temperature-dependent conductivity and dielectric behavior were analyzed in this work. Dye sensitized solar cell was fabricated using the nanocomposite film for this sample and analyzed.     

Thermal experimental verification on effects of nanoparticles for enhancing electric and dielectric performance of polyvinyl chloride

This paper presents investigation on the enhancement of dielectric constant characterization of polyvinyl chloride (PVC) by organic and inorganic nanoparticles under variant frequencies and thermal conditions. Dielectric spectroscopy has been experiment dielectric properties of polyvinyl chloride at various frequencies (0.01 Hz–1 MHz) and temperatures (20–80 °C); then, it has been specified the effective nanoparticles on dielectric constant performance compared with unfilled base matrix polymer. Therefore, it has been got optimum types and concentrations of nanoparticles that have been used for controlling and enhancing dielectric constant characterization of polyvinyl chloride.     

Study of unidirectional conductivity on the electrical discharge machining of semiconductor crystals

This paper investigates the unidirectional conductivity of semiconductor crystals machined by electrical discharge machining (EDM) by analyzing the properties of current–voltage (I–V) curves of the equivalent circuit. The simplified equivalent circuit of a semiconductor EDM consists of reverse-biased diodes and linear resistance. The I–V curve has three typical parameters, namely, conduction angle, breakdown angle, and breakdown point. The values of the conduction angle and the breakdown point are determined by the contact area of the reverse-biased diode, and the breakdown angle is determined by the value of linear resistance. Two diodes exist in the model with two metal electric feeders. To increase the current in this model, the diode with larger contact area should be reverse-biased. If the work piece is connected to anode in semiconductor EDM, the diode in the conduction side is reverse-biased and the avalanche voltage is only 42 V. If the work piece is connected to the cathode in semiconductor EDM, then the arc plasma, which is a termination with a small area, becomes reverse-biased. The temperature in the arc plasma side is high, causing the breakdown voltage to be much higher than the theoretical calculation value 88.5 V. As a result, when the work piece is connected to the cathode, spark production is difficult. Holes are bored on the P-type semiconductor crystals by positive and negative polarity, which could prove that machining with positive polarity is suitable for P-type semiconductor crystals during EDM. When the no-load voltage is set to 150 V, the penetration speed by positive polarity can reach 533 μm/min.     

Effect of humidity on electrical properties of micro/nano-polyaniline thin films with different D-CSA doping degree

In this paper, the influence on humidity sensitive characteristics of micro/nano-polyaniline (PANI) thin films with different doping degree of (1S)-(+)-10-camphorsulfonic acid (D-CSA) is investigated. The PANI is synthesized by an in situ chemical oxidative polymerization of aniline in the presence of ammonium peroxydisulfate (APS) acidic at ice–water bath for 10 h, and characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), respectively. Then, the composite films are formed between interdigital electrodes on a silicon (Si) substrate via self-assembly method. The humidity sensitive characteristics of the PANI films are measured. The experimental results show that the conductivity of PANI increases with increasing the molar ratios of [D-CSA]/[Ani]. Besides, the humidity sensitivity of the PANI films enhances with increasing the molar ratios of [D-CSA]/[Ani] and decreasing the layer number of PANI films, respectively. The PANI films with [D-CSA]/[Ani] molar ratio of 1.0 ([D-CSA]/[Ani] = 1:1) has higher sensitivity. The results indicate that the doping degree of D-CSA actually influences on the humidity sensitive characteristics of PANI thin films, and may be referencing significance for the fabrication of better humidity sensor.     

Potential step study of electrooxidation of methanol in 1-butyl-3-methylimidazolium tetrafluoroborate

A potential step method was used to characterize the electrooxidation of methanol on a chemically modified electrode in an ionic liquid solvent. Two major findings were reported from this study. Firstly, the oxidation was dominant 2.2 s after the potential step. Before that, the double layer charging and adsorption were dominant. Therefore, there should be a waiting time of a few seconds if a methanol sensor is developed with a potential step method. Secondly, the oxidation of methanol on the electrode was diffusion controlled. The concentration of methanol affected the diffusion. The diffusion constant D₀ was 8.37 × 10⁻¹⁷ m²/s when the concentration was lower than 0.5 M and was 2.66 × 10⁻¹³ m²/s when the concentration was higher than 1.0 M. This suggests that the methanol concentration should be kept higher than a threshold in an ionic liquid based fuel cell.     

Polymethacrylate optodes: A potential for chemical digital color analysis

The paper describes results of implementing a new kind of optical analytical method, digital color analysis (DCA), in which colorimetric polymethacrylate sensors (optodes) are used. The optodes are made of optically transparent polymethacrylate matrix with physically immobilized analytical reagent which is responsible for the extraction of the analyte into the sensing material and changing its color. The developed optodes can be used in determination of various analytes using both solid-phase spectrophotometer and naked eye. In order to improve accuracy and sensitivity of the naked-eye determination, it is possible to measure visible color changes using digital imaging of the polymethacrylate optode. The digital images then can be represented as basic color (e.g. RGB) data. The DCA determinations of Cu (II), Ag (I) and Co (II) have indicated that the developed optodes are linear in concentration ranges 0.02–0.30; 0.02–0.20 and 0.05–0.25 mg L⁻¹ appropriately with corresponding practical detection limits of 0.01; 0.02 and 0.07 mg L⁻¹.