Microwave Assisted Synthesis and Antimicrobial Study of Schiff Base Vanadium(IV) Complexes of Phenyl Esters of Amino Acids

Schiff base vanadium(IV) complexes of phenyl esters of the two acidic amino acids, i.e., aspartic and glutamic acid, were synthesized. The phenyl esters of these amino acids were synthesized by conventional method whereas the Schiff base vanadium(IV) complexes were synthesized using microwave irradiation. The complexes were characterized by spectroscopic tools such as IR, 1H NMR, mass (ES), ESR, and UV visible spectroscopy. All the complexes were studied for antibacterial and antifungal activity and found to be moderately active.

Microwave-assisted, surfactant-free synthesis of air-stable copper nanostructures and their SERS study

A simple, rapid, and surfactant-free synthesis of crystalline copper nanostructures has been carried out through microwave irradiation of a solution of copper acetylacetonate in benzyl alcohol. The structures are found to be stable against oxidation in ambient air for several months. High-resolution electron microscopy (SEM and TEM) reveals that the copper samples comprise nanospheres measuring about 150 nm in diameter, each made of copper nanocrystals similar to 7 nm in extension. The nanocrystals are densely packed into spherical aggregates, the driving force being minimization of surface area and surface energy, and are thus immune to oxidation in ambient air. Such aggregates can also be adherently supported on SiO2 and Al2O3 when these substrates are immersed in the irradiated solution. The air-stable copper nanostructures exhibit surface enhanced Raman scattering, as evidenced by the detection of 4-mercaptobenzoic acid at 10(-6) M concentrations.

Microwave absorbers designed from PVDF/SAN blends containing multiwall carbon nanotubes anchored cobalt ferrite via a pyrene derivative

Lightweight and flexible electromagnetic shielding materials were designed by selectively localizing multiwall carbon nanotubes (MWNTs) anchored magnetic nanoparticles in melt mixed co-continuous blends of polyvinylidene fluoride (PVDF) and poly(styrene-co-acrylonitrile) (SAN). In order to facilitate better dispersion, the MWNTs were modified using pyrenebutyric acid (PBA) via pi-pi stacking. While one of the two-targeted properties, i.e., high electrical conductivity, was achieved by PBA modified MWNTs, high magnetic loss was accomplished by introducing nickel (NF) or cobalt ferrites (CF). Moreover, the attenuation by absorption can be tuned either by using NF (58% absorption) or CF (64% absorption) in combination with PBA-MWNTs. More interestingly, when CF was anchored on to MWNTs via the pyrene derivative, the minimum reflection loss attained was -55 dB in the Ku band (12-18 GHz) frequency and with a large bandwidth. In addition, the EM waves were blocked mostly by absorption (70%). This study opens new avenues in designing flexible and lightweight microwave absorbers.

Degradation mechanism of polystyrene sulfonic acid membrane and application of its composite membranes in fuel cells

The lifetime behavior of a H-2/O-2 proton exchange membrane (PEM) fuel cell with polystyrene sulfonic acid (PSSA) membrane have been investigated in order to give an insight into the degradation mechanism of the PSSA membrane. The distribution of sulfur concentration in the cross section of the PSSA membrane was measured by energy dispersive analysis of X-ray, and the chemical composition of the PSSA membrane was characterized by infrared spectroscopy before and after the lifetime experiment. The degradation mechanism of the PSSA membrane is postulated as: the oxygen reduction at the cathode proceeds through some peroxide intermediates during the fuel cell operation, and these intermediates have strong oxidative ability and may chemically attack the tertiary hydrogen at the a carbon of the PSSA; the degradation of the PSSA membrane mainly takes place at the cathode side of the cell, and the loss of the aromatic rings and the SO3- groups simultaneously occurs from the PSSA membrane. A new kind of the PSSA-Nafion composite membrane, where the Nafion membrane is bonded with the PSSA membrane and located at the cathode of the cell, was designed to prevent oxidation degradation of the PSSA membrane in fuel cells. The performances of fuel cells with PSSA-Nafion101 and PSSA-recast Nafion composite membranes are demonstrated to be stable after 835 h and 240 h, respectively.

CHEMICAL-IONIZATION MASS-SPECTROMETRY OF BENZOYL PEROXIDE - A RADICAL AROMATIC-SUBSTITUTION RESULTING IN BIPHENYLCARBOXYLIC ACID IN THE GAS-PHASE

A radical aromatic substitution resulting in biphenylcarboxylic acid is inferred for the decomposition of benzoyl peroxide from the chemical ionization and collision-induced dissociation mass spectra. The thermolysis of benzoyl peroxide gives rise to a benzoyloxy radical, which undergoes rapid decarboxylation and hydrogen abstraction leading to phenyl radical and benzoic acid, respectively. Attack of the resulting phenyl radical on the benzoic acid results in bipbenylcarboxylic acid. On the other hand, the phenyl radical abstracts a hydrogen atom to yield benzene, which is then subjected to the attack of a benzoyloxy radical, affording phenyl benzoate. This substitution reaction rather than the recombination of benzoyloxy and phenyl radicals is found to be responsible for the formation of phenyl benzoate under the present conditions.

Determination of trace arsenic and selenium in jellyfish by microwave digestion-hydride generation-atomic fluorescence spectrometry

A method of hydride generation-atomic fluorescence spectrometry was proposed in the present paper for the determination of trace arsenic and selenium in jellyfish. The samples were treated by the combination of microwave digestion and lyophilization. The optimal conditions for treating and analyzing samples were established. The problem of the effect of the superfluous acid in the digesting solution on the results was solved, and the influence of coexisting foreign ions on the determination of arsenic and selenium was investigated. The accuracy of the method was confirmed by the method of standard additions. This method proved to be simple, rapid and repeatable, and is suitable for the analysis of biologic samples containing water.

Effect of microwave treatment on chemical composition and in sacco digestibility of wheat straw in yak cow

Wheat straw was treated with microwave for 4 min and 8 min at a power of 750 W and frequency of 2,450 MHz. Chemical compositions of untreated, 4 min treated and 8 min treated Straws were analyzed and in sacco degradabilities of all these straws in yak rumens were measured. Microwave treatment didn't significantly (p > 0.05) affect the chemical composition of the straw. In sacco dry matter (DM) degradability of the straw after 18 h incubation in rumen was significantly (p < 0.01) improved by microwave treatment. In sacco crude protein (CP) degradability of the straw was not (p > 0.05) affected by microwave treatment. In sacco organic matter (OM) degradability of the straw was increased (p < 0.01) by around 20% for both the 4 min and 8 min microwave treatment, that of acid detergent fibre (ADF) was increased (p < 0.01) by 61.6% and 62.8%, and that of ash free ADF was enhanced by 72.1% and 69.6% for the 4 min and 8 min microwave treatment respectively. No significant difference was observed between the 4 min and 8 min microwave treatment on the degradability of DM, OM, CP, ADF and ash-free ADF of the straw.

Microwave curing for high density package

Summary form only given. Currently the vast majority of adhesive materials in electronic products are bonded using convection heating or infra-red as well as UV-curing. These thermal processing steps can take several hours to perform, slowing throughput and contributing a significant portion of the cost of manufacturing. With the demand for lighter, faster, and smaller electronic devices, there is a need for innovative material processing techniques and control methodologies. The increasing demand for smaller and cheaper devices pose engineering challenges in designing a curing systems that minimize the time required between the curing of devices in a production line, allowing access to the components during curing for alignment and testing. Microwave radiation exhibits several favorable characteristics and over the past few years has attracted increased academic and industrial attention as an alternative solution to curing of flip-chip underfills, bumps, glob top and potting cure, structural bonding, die attach, wafer processing, opto-electronics assembly as well as RF-ID tag bonding. Microwave energy fundamentally accelerates the cure kinetics of polymer adhesives. It provides a route to focus heat into the polymer materials penetrating the substrates that typically remain transparent. Therefore microwave energy can be used to minimise the temperature increase in the surrounding materials. The short path between the energy source and the cured material ensures a rapid heating rate and an overall low thermal budget. In this keynote talk, we will review the principles of microwave curing of materials for high density packing. Emphasis will be placed on recent advances within ongoing research in the UK on the realization of "open-oven" cavities, tailored to address existing challenges. Open-ovens do not require positioning of the device into the cavity through a movable door, hence being more suitable for fully automated processing. Further potential advantages of op- - en-oven curing include the possibility for simultaneous fine placement and curing of the device into a larger assembly. These capabilities promise productivity gains by combining assembly, placement and bonding into a single processing step. Moreover, the proposed design allows for selective heating within a large substrate, which can be useful particularly when the latter includes parts sensitive to increased temperatures.

Comparison of encapsulant curing with convention and microwave systems

Comparison of the performance of a conventional convection oven system with a dual-section microwave system for curing thermosetting polymer encapsulant materials has been performed numerically. A numerical model capable of analysing both the convection and microwave cure processes has been developed and is breifly outliines. The model is used to analyse the curing of a commercially available encapsulant material using both systems. Results obtained from numerical solutions are presented, confirming that the VFM system enables the cure process to be carried out far more rapidly than with the convection oven system. This capability stems from the fundamental heating processes involved, namely that microwave processing enables the heating rate to be varied independently of the material temperature. Variations in cure times, curing rates, maximum temperatures and residual stresses between the processes are fully discussed.

Numerical simulation of encapsulant curing within a variable frequency microwave processing system

Curing of encapsulant material in a simplified microelectronics package using an open oven Variable Frequency Microwave (VFM) system is numerically simulated using a coupled solver approach. A numerical framework capable of simulating electromagnetic field distribution within the oven system, plus heat transfer, cure rate, degree of cure and thermally induced stresses within the encapsulant material is presented. The discrete physical processes have been integrated into a fully coupled solution, enabling usefully accurate results to be generated. Numerical results showing the heating and curing of the encapsulant material have been obtained and are presented in this contribution. The requirement to capture inter-process coupling and the variation in dielectric and thermophysical material properties is discussed and illustrated with simulation results.

Microwave curing of thermosetting polymer materials in microelectronics applications

Thermosetting polymer materials are widely utilised in modern microelectronics packaging technology. These materials are used for a number of functions, such as for device bonding, for structural support applications and for physical protection of semiconductor dies. Typically, convection heating systems are used to raise the temperature of the materials to expedite the polymerisation process. The convection cure process has a number of drawbacks including process durations generally in excess of 1 hour and the requirement to heat the entire printed circuit board assembly, inducing thermomechanical stresses which effect device reliability. Microwave energy is able to raise the temperature of materials in a rapid, controlled manner. As the microwave energy penetrates into the polymer materials, the heating can be considered volumetric – i.e. the rate of heating is approximately constant throughout the material. This enables a maximal heating rate far greater than is available with convection oven systems which only raise the surface temperature of the polymer material and rely on thermal conductivity to transfer heat energy into the bulk. The high heating rate, combined with the ability to vary the operating power of the microwave system, enables the extremely rapid cure processes. Microwave curing of a commercially available encapsulation material has been studied experimentally and through use of numerical modelling techniques. The material assessed is Henkel EO-1080, a single component thermosetting epoxy. The producer has suggested three typical convection oven cure options for EO1080: 20 min at 150C or 90 min at 140C or 120 min at 110C. Rapid curing of materials of this type using advanced microwave systems, such as the FAMOBS system [1], is of great interest to microelectronics system manufacturers as it has the potential to reduce manufacturing costs, increase device reliability and enables new device designs. Experimental analysis has demonstrated that, in a realistic chip-on-board encapsulation scenario, the polymer material can be fully cured in approximately one minute. This corresponds to a reduction in cure time of approximately 95 percent relative to the convection oven process. Numerical assessment of the process [2] also suggests that cure times of approximately 70 seconds are feasible whilst indicating that the decrease in process duration comes at the expense of variation in degree of cure within the polymer.

Stability of 5-aminolevulinic acid in novel non-aqueous gel and patch-type systems intended for topical application.

Aminolevulinic acid (ALA) stability within topical formulations intended for photodynamic therapy (PDT) is poor due to dimerisation to pyrazine-2,5-dipropionic acid (PY). Most strategies to improve stability use low pH vehicles, which can cause cutaneous irritancy. To overcome this problem, a novel approach is investigated that uses a non-aqueous vehicle to retard proton-induced charge separation across the 4-carbonyl group on ALA and lessen nucleophilic attack that leads to condensation dimerisation. Bioadhesive anhydrous vehicles based on methylvinylether-maleic anhydride copolymer patches and poly(ethyleneglycol) or glycerol thickened poly(acrylic acid) gels were formulated. ALA stability fell below pharmaceutically acceptable levels after 6 months, with bioadhesive patches stored at 5°C demonstrating the best stability by maintaining 86.2% of their original loading. Glycerol-based gels maintained 40.2% in similar conditions. However, ALA loss did not correspond to expected increases in PY, indicating the presence of another degradative process that prevented dimerisation. Nuclear magnetic resonance (NMR) analysis was inconclusive in respect of the mechanism observed in the patch system, but showed clearly that an esterification reaction involving ALA and both glycerol and poly(ethyleneglycol) was occurring. This was especially marked in the glycerol gels, where only 2.21% of the total expected PY was detected after 204 days at 5°C. Non-specific esterase hydrolysis demonstrated that ALA was recoverable from the gel systems, further supporting esterified binding within the gel matrices. It is conceivable that skin esterases could duplicate this finding upon topical application of the gel and convert these derivatives back to ALA in situ, provided skin penetration is not affected adversely.

Hexavalent Chromium Adsorption by a Novel Activated Carbon Prepared by Microwave Activation

Microwave heating reduces the preparation time and improves the adsorption quality of activated carbon. In this study, activated carbon was prepared by impregnation of palm kernel fiber with phosphoric acid followed by microwave activation. Three different types of activated carbon were prepared, having high surface areas of 872 m2 g-1, 1256 m2 g-1, and 952 m2 g-1 and pore volumes of 0.598 cc g-1, 1.010 cc g-1, and 0.778 cc g-1, respectively. The combined effects of the different process parameters, such as the initial adsorbate concentration, pH, and temperature, on adsorption efficiency were explored with the help of Box-Behnken design for response surface methodology (RSM). The adsorption rate could be expressed by a polynomial equation as the function of the independent variables. The hexavalent chromium adsorption rate was found to be 19.1 mg g-1 at the optimized conditions of the process parameters, i.e., initial concentration of 60 mg L-1, pH of 3, and operating temperature of 50 oC. Adsorption of Cr(VI) by the prepared activated carbon was spontaneous and followed second-order kinetics. The adsorption mechanism can be described by the Freundlich Isotherm model. The prepared activated carbon has demonstrated comparable performance to other available activated carbons for the adsorption of Cr(VI).

Microwave-Assisted Preparation of Hydrogel-Forming Microneedle Arrays for Transdermal Drug Delivery Applications

A microwave (MW)-assisted crosslinking process to prepare hydrogel-forming microneedle (MN) arrays was evaluated. Conventionally, such MN arrays are prepared using processes that includes a thermal crosslinking step. Polymeric MN arrays were prepared using poly(methyl vinyl ether-alt-maleic acid) crosslinked by reaction with poly(ethylene glycol) over 24 h at 80 °C. Polymeric MN arrays were prepared to compare conventional process with the novel MW-assisted crosslinking method. Infrared spectroscopy was used to evaluate the crosslinking degree, evaluating the area of the carbonyl peaks (2000–1500 cm−1). It was shown that, by using the MW-assisted process, MN with a similar crosslinking degree to those prepared conventionally can be obtained in only 45 min. The effects of the crosslinking process on the properties of these materials were also evaluated. For this purpose swelling kinetics, mechanical characterisation, and insertion studies were performed. The results suggest that MN arrays prepared using the MW assisted process had equivalent properties to those prepared conventionally but can be produced 30 times faster. Finally, an in vitro caffeine permeation across excised porcine skin was performed using conventional and MW-prepared MN arrays. The release profiles obtained can be considered equivalent, delivering in both cases 3000–3500 μg of caffeine after 24 h.

Effect of Drying Conditions on Microwave Conductivity of Polyaniline

ABSTRACT: Polyaniline was synthesized by using ammonium persulfate initiator in the presence of 1M HC1. It was dried under different drying conditions like room temperature drying (for 48 h), oven drying (at 50-60°C for 8 h under a vacuum), and vacuum drying (at room temperature for 16 h). The conductivities of these samples were measured at microwave frequencies. These samples were also pelletized and the measurements were repeated. The cavity perturbation technique was used for the study.