Polymer electrolytes based on polyacrylonitrile (PAN) containing inorganic salts; lithium triflate (LiCF3SO3) and sodium triflate (NaCF3SO3) and ethylene carbonate (EC) as plasticizer were prepared using solvent casting technique. In this study, five systems of plasticized and unplasticized polymer electrolyte films i.e. PAN-EC, PAN-LiCF3SO3, PAN-NaCF3SO3 PAN-EC-LiCF3SO3 and PAN-EC-NaCF3SO3 systems have been prepared. The structural and morphological properties of the films were studied using infrared spectroscopy and scanning electron microscopy (SEM) while the conductivity study was done by using impedance spectroscopy. The infrared results revealed that interaction had taken place between the nitrogen atoms of PAN and Li+ and Na+ ions from the salts. SEM micrographs showed that the plasticized film, PAN-EC-NaCF3SO3 has bigger pores than PAN-EC-LiCF3SO3 film resulting in the film containing NaCF3SO3 salt being more conductive. On addition of salts and plasticizer, the conductivity of pure PAN increases to three orders of magnitude. The plasticized film containing NaCF3SO3 salt has a higher conductivity compared to that containing LiCF3SO3 salt. This result showed that the interaction between Li+-ion and the nitrogen atom of PAN was stronger than that of Na+-ion. The conductivity-temperature dependence of the highest conducting film from each system follows Arrhenius equation in the temperature range of 303 to 353 K. The conductivity-pressure study in the range of 0.01 - 0.09 MPa showed that the conductivity decreased when pressure was increased. This can be explained in term of free volume model.
Solid polymer electrolytes comprised of various weight percent ratios of poly(ethyl methacrylate) (PEMA) and lithium perchlorate (LiClO4) salt were prepared via solution casting technique using N,N-dimethylformamide (DMF) as the solvent. The conductivity values of the electrolytes were determined via impedance spectroscopy. The conductivity of the PEMA-LiClO4 electrolytes increased with increasing salt concentration and the highest conductivity obtained was in the order of 10-6 S cm-1 at salt concentration of 20 wt%. The conductivity decreased for higher salt concentration. In order to understand the conductivity behavior, XRD and dielectric studies were done. The results showed that the conductivity was influenced by the fraction of amorphous region and number of charge carriers in the system. The transference number measurement was also performed on the highest conducting electrolyte systems. The result of the measurement indicated that the systems were ionic conductors.
In this study, two nickel based electrodes were prepared; nickel foil and nickel-polyvinylchloride (Ni-PVC), in order to study their electrochemical behavior using cyclic voltammetry, CV and chronocoulometry, CC. Ni electrode was prepared from Ni metal foil while Ni-PVC electrode was prepared by mixing a weighed portion of Ni powder and PVC in THF solvent, swirled until the suspension was homogeneous and drying the suspension in an oven at 50oC for 3 h. The dry sample was then placed in a 1 cm diameter stainless steel mould and pressed at 10 ton/cm2. From CV data, Ni-PVC electrode showed a better electrochemical behavior compared to Ni metal foil electrode. The use of Ni-PVC electrode at higher concentration of supporting electrolyte (1.0 M KOH) was better than at lower concentration of the same supporting electrolyte in electroxidation of ethanol. In addition to acetic acid, the oxidation of ethanol also produced ethyl acetate and acetaldehyde.
A simple micellar electrokinetic chromatography (MEKC) method for the simultaneous determination of 2-furfural (2-F), 3-furfural (3-F), 5-methylfurfural (5-MF), 5-hydroxymethylfurfural (5-HMF), 2-furoic acid (2-FA) and 3-furoic acid (3-FA) in honey and vegetable oils is described. Parameters affecting the separation such as pH, buffer and surfactant concentrations, applied voltage, capillary temperature, injection time and capillary length were studied and optimized. The separation was carried out in normal polarity mode at 20 °C, 22 kV and using hydrodynamic injection (17 s). The separation was achieved in a bare fused-silica capillary (46 cm × 50 μm i.d.) with a background electrolyte of 75 mM phosphoric acid (pH 7.3), containing 200 mM of sodium dodecyl sulphate (SDS). The detection wavelengths were at 200 nm (2-FA and 3-FA) and 280 nm (2-F, 3-F, 5-MF, 5-HMF). The furfurals were well separated in less than 20 min. The method was validated in terms of linearity, limit of detection and quantitation, precision and recoveries. Calibration curves of the six furfurals were well correlated (r(2)>0.991) within the range 1-25 μg mL(-1). Relative standard deviations of intra- and inter-day migration times and corrected peak areas ≤9.96% were achieved. The limit of detection (signal:noise, 3) was 0.33-0.70 μg mL(-1) whereas the limit of quantitation (signal:noise, 10) was 1.00-2.12 μg mL(-1). The method was applied to the determination of furanic compounds in honeys and vegetable oils (palm, walnut, grape seed and rapeseed). The effects of thermal treatment and gamma irradiation on the formation of the furanic compounds in honey were also investigated.
Thermoelectric nanostructures hold great promise for capturing and directly converting into electricity some vast amount of low-grade waste heats now being lost to the environment (e.g. from nuclear power plant, fossil fuel burning, automotives and household appliances). In this study, large-area vertically-aligned silicon nanowire (SiNW) arrays were synthesized in an aqueous solution containing AgN•i and HF on p-type Si (100) substrate by self-selective electroless etching process. The etching conditions were systematically varied in order to achieve different stages of nanowire formation. Diameters of the SiNWs obtained varied from approximately 50 to 200 nm and their lengths ranged from several to a few tens of um. Te/Bi2Tex.Si thermoelectric core-shell nanostructures were subsequently obtained via galvanic displacement of SiNWs in acidic HF electrolytes containing HTe02+ and 139' /HTe02+ ions. The reactions were basically a nano-electrochemical process due to the difference in redox potentials between the materials. The surface-modified SiNWs of core-shell structures had roughened surface morphologies and, therefore, higher surface-to-bulk ratios compared to unmodified SiNWs. They have potential applications in sensors, photovoltaic and thermoelectric nanodevices. Growth study on the SiNWs and core-shell nanostructures produced is presented using various microscopy, diffraction and probe-based techniques for microstructural, morphological and chemical characterizations.
Polymer electrolytes were developed by solution casting technique utilizing the materials of cellulose acetate (CA), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) and deep eutectic solvent (DES). The DES is synthesized from the mixture of choline chloride and urea of 1:2 ratios. The increasing DES content well plasticizes the CA:LiTFSI:DES matrix and gradually improves the ionic conductivity and chemical integrity. The highest conducting sample was identified for the composition of CA:LiTFSI:DES (28 wt.%:12 wt.%:60 wt.%), which has the greatest ability to retain the room temperature ionic conductivity over the entire 30 days of storage time. The changes in FTIR cage peaks upon varying the DES content in CA:LiTFSI:DES prove the complexation. This complexation results in the collapse of CA matrix crystallinity, observed from the reduced intensity of XRD diffraction peaks. The DES-plasticized sample is found to be more heat-stable compared to pure CA. Nevertheless, the addition of DES diminishes the CA:LiTFSI matrix's heat-resistivity but at the minimum addition the thermal stability is enhanced.
We report the crystallization of electrodeposited germanium (Ge) thin films on n-silicon (Si) (100) by rapid melting process. The electrodeposition was carried out in germanium (IV) chloride: propylene glycol (GeCl₄:C₃H₈O₂) electrolyte with constant current of 50 mA for 30 min. The measured Raman spectra and electron backscattering diffraction (EBSD) images show that the as-deposited Ge thin film was amorphous. The crystallization of deposited Ge was achieved by rapid thermal annealing (RTA) at 980 °C for 1 s. The EBSD images confirm that the orientations of the annealed Ge are similar to that of the Si substrate. The highly intense peak of Raman spectra at 300 cm(-1) corresponding to Ge-Ge vibration mode was observed, indicating good crystal quality of Ge. An additional sub peak near to 390 cm(-1) corresponding to the Si-Ge vibration mode was also observed, indicating the Ge-Si mixing at Ge/Si interface. Auger electron spectroscopy (AES) reveals that the intermixing depth was around 60 nm. The calculated Si fraction from Raman spectra was found to be in good agreement with the value estimated from Ge-Si equilibrium phase diagram. The proposed technique is expected to be an effective way to crystallize Ge films for various device applications as well as to create strain at the Ge-Si interface for enhancement of mobility.
In this work, epoxidized natural rubber 50 (ENR-50) has been used as a host polymer for the preparation of electrolyte system. Attenuated total reflection-fourier transform infrared spectroscopic analyses showed the presence of lithium saltENR interactions. The glass transition temperature displayed an increasing trend with the increase in salt concentration indicating that the ionic conductivity was not influenced by segmental motion of the ENR-50 chains. The increase in
glass transition temperature with the addition of salt was due to the formation of transient cross-linking between ENR-50 chains via the coordinated interaction between ENR-50 chains and salt. The highest room temperature ionic conductivity obtained was in the order of 10-5 S cm-1 for the film containing 50 wt% of lithium salt. The ionic conductivity of this electrolyte system increased with increasing temperature and obeyed the Vogel-Tamman-Fulcher behavior. The increase in ionic conductivity of the electrolyte system with salt concentration could also be correlated to the charge carriers concentration and/or migration rate of charge carriers.
Two different ionic liquid-based biopolymer electrolyte systems were prepared using a solution casting technique. Corn starch and lithium hexafluorophosphate (LiPF₆) were employed as polymer and salt, respectively. Additionally, two different counteranions of ionic liquids, viz. 1-butyl-3-methylimidazolium hexafluorophosphate (BmImPF₆) and 1-butyl-3-methylimidazolium trifluoromethanesulfonate (also known as 1-butyl-3-methylimidazolium triflate) (BmImTf) were used and studied in this present work. The maximum ionic conductivities of (1.47 ± 0.02) × 10(-4) and (3.21 ± 0.01) × 10(-4) S∙cm(-1) were achieved with adulteration of 50 wt% of BmImPF₆ and 80 wt% of BmImTf, respectively at ambient temperature. Activated carbon-based electrodes were prepared and used in supercapacitor fabrication. Supercapacitors were then assembled using the most conducting polymer electrolyte from each system. The electrochemical properties of the supercapacitors were then analyzed. The supercapacitor containing the triflate-based biopolymer electrolyte depicted a higher specific capacitance with a wider electrochemical stability window compared to that of the hexafluorophosphate system.
The accumulation of paralytic shellfish toxins (PSTs) in contaminated shellfish is a serious health risk making early detection important to improve shellfish safety and biotoxin management. Capillary electrophoresis (CE) has been proven as a high resolution separation technique compatible with miniaturization, making it an attractive choice in the development of portable instrumentation for early, on-site detection of PSTs. In this work, capillary zone electrophoresis (CZE) with capacitively coupled contactless conductivity detector (C(4)D) and UV detection were examined with counter-flow transient isotachophoresis (tITP) to improve the sensitivity and deal with the high conductivity sample matrix. The high sodium concentration in the sample was used as the leading ion while l-alanine was used as the terminating electrolyte (TE) and background electrolyte (BGE) in which the toxins were separated. Careful optimization of the injected sample volume and duration of the counter-flow resulted in limit of detections (LODs) ranging from 74.2 to 1020 ng/mL for tITP-CZE-C(4)D and 141 to 461 ng/mL for tITP-CZE-UV, an 8-97 fold reduction compared to conventional CZE. The LODs were adequate for the analysis of PSTs in shellfish samples close to the regulatory limit. Intra-day and inter-day repeatability values (percentage relative standard deviation, n=3) of tITP-CZE-C(4)D and tITP-CZE-UV methods for both migration time and peak height were in the range of 0.82-11% and 0.76-10%, respectively. The developed method was applied to the analysis of a contaminated mussel sample and validated against an Association of Official Analytical Chemists (AOAC)-approved method for PSTs analysis by high performance liquid chromatography (HPLC) with fluorescence detection (FLD) after pre-column oxidation of the sample. The method presented has potential for incorporation in to field-deployable devices for the early detection of PSTs on-site.
The aim of the study was to evaluate the effect of crude aqueous extract of Boswellia serrata Roxb. oleo gum on urinary electrolytes, pH and diuretic activity in normal albino rats. Moreover, acute toxicity of the gum extract was assessed using mice. Albino rats were divided into five groups. Control group received normal saline (10 mg/kg), reference group received furosemide (10 mg/kg) and test groups were given different doses of crude extract (10, 30 and 50 mg/kg) by intra-peritoneal route, respectively. The Graph Pad Prism was used for the statistical analysis and p < 0.05 was considered statistically significant. Significant diuretic, kaliuretic and natriuretic effects were observed in the treated groups in a dose dependent manner. Diuretic index showed good diuretic activity of the crude extract. Lipschitz values indicated that the crude extract, at the dose of 50 mg/kg, showed 44 % diuretic activity compared to the reference drug. No lethal effects were observed among albino mice even at the higher dose of 3000 mg/kg. It is concluded that aqueous extract of Boswellia serrata oleo gum, at the dose of 50 mg/kg showed significant effects on urinary volume and concentration of urinary electrolytes with no signs of toxicity.
Gel polymer electrolytes (GPEs) are developed using poly(1-vinylpyrrolidone-co-vinyl acetate) [P(VP-co-VAc)] as the host polymer, lithium bis(trifluoromethane) sulfonimide [LiTFSI] as the lithium salt and ionic liquid, and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide [EMImTFSI] by using solution casting technique. The effect of ionic liquid on ionic conductivity is studied and the optimum ionic conductivity at room temperature is found to be 2.14 × 10(-6) S cm(-1) for sample containing 25 wt% of EMImTFSI. The temperature dependence of ionic conductivity from 303 K to 353 K exhibits Arrhenius plot behaviour. The thermal stability of the polymer electrolyte system is studied by using thermogravimetric analysis (TGA) while the structural and morphological properties of the polymer electrolyte is studied by using Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction analysis (XRD), respectively.
Graphene is an attention-grabbing material in electronics, physics, chemistry, and even biology because of its unique properties such as high surface-area-to-volume ratio. Also, the ability of graphene-based materials to continuously tune charge carriers from holes to electrons makes them promising for biological applications, especially in lipid bilayer-based sensors. Furthermore, changes in charged lipid membrane properties can be electrically detected by a graphene-based electrolyte-gated graphene field effect transistor (GFET). In this paper, a monolayer graphene-based GFET with a focus on the conductance variation caused by membrane electric charges and thickness is studied. Monolayer graphene conductance as an electrical detection platform is suggested for neutral, negative, and positive electric-charged membrane. The electric charge and thickness of the lipid bilayer (Q LP and L LP) as a function of carrier density are proposed, and the control parameters are defined. Finally, the proposed analytical model is compared with experimental data which indicates good overall agreement.
In this research, two systems are studied. In the first system, the ratio of poly (methyl methacrylate) (PMMA) and poly (vinyl chloride) (PVC) is varied, whereas in the second system, the composition of PMMA-PVC polymer blends is varied with dopant salt, lithium bis (trifluoromethanesulfonyl) imide (LiTFSI) with a fixed ratio of 70 wt% of PMMA to 30 wt% of PVC. Oscillation tests such as amplitude sweep and frequency sweep are discussed in order to study the viscoelastic properties of samples. Elastic properties are much higher than viscous properties within the range in the amplitude sweep and oscillatory shear sweep studies. The crossover of G' and G'' is absent. Linear viscoelastic (LVE) range was further determined in order to perform the frequency sweep. However, the absence of viscous behavior in the frequency sweep indicates the solid-like characteristic within the frequency regime. The viscosity of all samples is found to decrease as shear rate increases.
This paper reports on the direct ability of two positively charged organic polyelectrolytes (natural-based and synthetic) to reduce the atrazine concentration in water. The adsorption study was set up using multiple glass vessels with different polymer dosing levels followed by ultrafiltration with a 1 kDa membrane. The addition of polymers exhibited a capability in reducing the atrazine concentration up to a maximum of 60% in surface-to-volume ratio experiments. In the beginning, the theoretical L-type of the isotherm of Giles' classification was expected with an increase in the dosage of the polymer. However, in this study, the conventional type of isotherm was not observed. It was found that the adsorption of the cationic polymer on the negatively charged glass surface was necessary and influential for the removal of atrazine. Surface-to-volume ratio adsorption experiments were performed to elucidate the mechanisms and the polymer configuration. The glass surface area was determined to be a limiting parameter in the adsorption mechanism.
Tungsten trioxide (WO₃) possesses a small band gap energy of 2.4-2.8 eV and is responsive to both ultraviolet and visible light irradiation including strong absorption of the solar spectrum and stable physicochemical properties. Thus, controlled growth of one-dimensional (1D) WO₃ nanotubular structures with desired length, diameter, and wall thickness has gained significant interest. In the present study, 1D WO₃ nanotubes were successfully synthesized via electrochemical anodization of tungsten (W) foil in an electrolyte composed of 1 M of sodium sulphate (Na₂SO₄) and ammonium fluoride (NH₄F). The influence of NH₄F content on the formation mechanism of anodic WO₃ nanotubular structure was investigated in detail. An optimization of fluoride ions played a critical role in controlling the chemical dissolution reaction in the interface of W/WO₃. Based on the results obtained, a minimum of 0.7 wt% of NH₄F content was required for completing transformation from W foil to WO₃ nanotubular structure with an average diameter of 85 nm and length of 250 nm within 15 min of anodization time. In this case, high aspect ratio of WO₃ nanotubular structure is preferred because larger active surface area will be provided for better photocatalytic and photoelectrochemical (PEC) reactions.
In this work, 10 mol% yttrium-doped ceria powders, Ce0.9Y0.1O1.95, were synthesised using a new mechanical technique, mechanochemical reaction, in which both impact action and shearing forces were applied for efficient fine grinding, subsequently leading to higher homogeneity of the resultant powders. Ce0.9Y0.1O1.95 prepared using this new technique was systematically compared with a sample of the same prepared using conventional solid-state methodology. X-ray diffraction analysis showed all prepared samples were single phase with a cubic fluorite structure. Generally, Y2O3-doped CeO2 electrolytes prepared by mechanochemical reactions were stable at a lower temperature (1100 °C) compared with a sample of the same synthesised using the conventional solid-state method. Characterisations using differential thermal analysis (DTA) and thermogravimetric analysis (TGA) showed no thermal changes and phase transitions, indicating all materials were thermally stable. The electrical properties of the samples investigated by AC impedance spectroscopy in the temperature range 200–800 ˚C are presented and discussed. Scanning electron microscopy (SEM) was used to study the morphology of the materials. Fine-grained powders with uniform grain-size distribution were obtained from the mechanochemical reaction.
Phaleria macrocarpa seeds are rapidly killed with desiccation to moisture content (MC) below 20%. Desiccation tolerance of their embryonic axes was studied for storage and germplasm conservation purposes. Embryonic axes were extracted aseptically from fresh seeds obtained from fully ripe fruits in a horizontal laminar air flow cabinet. They were then desiccated under aseptic condition for periods ranging from 0-8 h. For each desiccation treatment, embryonic axes were drawn randomly for the determination of MC according to ISTA, electrolyte leakage and proliferation on Murashige and Skoog (MS) media supplemented with 1 mg/l 6-benzylaminopurine (BAP) and 1 mg/l 2,4-dichlorophenoxyacetic acid (2,4-D). The results obtained from this study indicated that the embryonic axes could tolerate dehydration down to 13.6% with desiccation for 8 h while retaining relatively high viability of 76.7%. This was supported by only gradual increment of electrolyte leakage with the desiccated embryonic axes. All non-desiccated embryonic axes with MC of 52.5% were capable to grow into normal plantlets in vitro but dehydration to MC of 36.0% and further down to 13.6% generally resulted in callus formation with up to 16.7% of the embryonic axes while at least 60.0% of the other embryonic axes were still capable to proliferate as normal plantlets in vitro.
In this study, a symmetric supercapacitor has been fabricated by adopting the nanostructured iron oxide (Fe304)-activated carbon (Ac) composite as the core electrode materials. The composite electrodes were prepared via a facile mechanical mixing process and PTFE polymeric solution has been used as the electrode material binder. Structural analysis of the nanocomposite electrodes were characterized by scanning electron microscopy ( sEm) and Brunauer-Emmett-Teller (BET) analysis. The electrochemical performances of the prepared supercapacitor were studied using cyclic voltammetry (cv) and electrochemical impedance spectroscopy (Eis) in 1.0 M Na2S03 and 1.0 M Na2SO4 aqueous solutions, respectively. The experimental results showed that the highest specific capacitance of 43 FIg is achieved with a fairly low Fe304 nanomaterials loading (4 wt. %) in 1 M Na2S03. It is clear that the low concentration of nanostructured Fe304 has improved the capacitive performance of the composite via pseudocapacitance charge storage mechanism as well as the enhancement on the specific surface areas of the electrode. However, further increasing of the Fe304 content in the electrode is found to distort the capacitive performance and deteriorate the specific surface area of the electrode, mainly due to the aggregation of the Fe304 particles within the composite. Additionally, the cv results showed that the Fe3041Ac nanocomposite electrode in Na2S03 electrolyte exhibits a better charge storage performance if compared with Na2SO4 solution. It is believed that Fe304 nanoparticles can provide favourable surface adsorption sites for sulphite (S032-) anions which act as catalysts for subsequent redox and intercalation reactions.
This paper is focussed on conductivity and dielectric properties of Poly (vinyl) chloride (Pvc)- ammonium triflate (NH4CF3SO3) - butyltrimethyl ammonium bis (trifluoromethyl sulfonyl) imide (Bu3MeNTf2N) ionic liquid, electrolyte system. The electrolyte is prepared by solution cast technique. In this work, the sample containing 30 wt. % NH4CF3SO3 exhibits the highest room temperature conductivity of 2.50 x 10-7 S cm' . Ionic liquid is added in various quantities to the 70 wt. % Pvc-30 wt. % NH4CF3SO3 composition in order to enhance the conductivity of the sample. The highest conductivity at room temperature is obtained for the sample containing 15 wt. % Bu3MeNTf2N with a value of 1.56 x 10 -4 S cm' . The effects of ionic liquid addition on the frequency dependent dielectric properties of PVC based electrolytes is investigated by electrochemical impedance spectroscopy (Eis) at room temperature. The values of dielectric constant were found to increase with increasing conductivity of the samples. Analysis of the ac conductivity data showed the electrolytes to be of the non-Debye type.