α-Alumina and spinel react into single-phase high-alumina spinel in <3 seconds during flash sintering

In situ X-ray diffraction measurements at the Advanced Photon Source show that α-Al₂O₃ and MgAl₂O₄ react nearly instantaneously and completely, and nearly completely to form single-phase high-alumina spinel during voltage-to-current type of flash sintering experiments. The initial sample was constituted from powders of α-Al₂O₃, MgAl₂O₄ spinel, and cubic 8 mol% Y₂O₃-stabilized ZrO₂ (8YSZ) mixed in equal volume fractions, the spinel to alumina molar ratio being 1:1.5. Specimen temperature was measured by thermal expansion of the platinum standard. These measurements correlated well with a black-body radiation model, using appropriate values for the emissivity of the constituents. Temperatures of 1600-1736°C were reached during the flash, which promoted the formation of alumina-rich spinel. In a second set of experiments, the flash was induced in a current-rate method where the current flowing through the specimen is controlled and increased at a constant rate. In these experiments, we observed the formation of two different compositions of spinel, MgO•3Al₂O₃ and MgO•1.5Al₂O₃, which evolved into a single composition of MgO•2.5Al₂O₃ as the current continued to increase. In summary, flash sintering is an expedient way to create single-phase, alumina-rich spinel.     

Reactive flash sintering: MgO and α-Al2O3 transform and sinter into single-phase polycrystals of MgAl2O4

We show that flash experiments with three phase mixed-powders of yttria-stabilized zirconia (8YSZ), MgO, and α-Al₂O₃ not only produce polycrystals of high density, but also the transformation of magnesia and alumina into single-phase spinel. The presence of zirconia facilitates the onset of the flash. The sintering experiments in the laboratory were extended to live experiments at the National Synchrotron Light Source II at Brookhaven National Laboratory in order to measure the time-dependent evolution of single-phase spinel. The phase transformation occurred in <3 seconds during Stage II. Later, during Stage III the cubic zirconia transformed partly into the monoclinic phase, which reverted back to the cubic phase when the flash was extinguished by turning off the current to the specimen. The results underpin a recent report on the synthesis of single-phase bismuth ferrite from constituent oxides in reactive flash experiments, raising the specter of flash as a method for synthesis as well as sintering of complex oxide ceramics. The role of zirconia in catalyzing the flash in the present study is discussed.     

On the onset of fracture as a silicon-based polymer converts into the ceramic phase

Silicon-based polymers evolve into refractory ceramics when heated gradually up to ~1000°C. The conversion is accompanied by the loss of gaseous species, and by a two-fold increase in density. The shrinkage can produce microcracks if the heating rate is too high, or if the specimen is too thick. This communication builds on earlier work whereby the measurement of gas evolution, and its relationship with viscous flow, are related to the onset of fracture in disk-shaped green (polymer) samples. The onset is determined as a function of the thickness of the disks, and of the heating rate. The results are presented in the form of a processing map. The overlay with gas evolution, and strain-rate measurements, suggest that fracture initiates with the release of hydrogen and methane, starting at temperatures near 750°C.     

Reactive flash sintering of powders of four constituents into a single phase of a complex oxide in a few seconds below 700°C

Recent work on reactive flash sintering of powders of two oxides, bismuth and of iron oxide, into pure single phase bismuth ferrite, which was accomplished in a few seconds at low furnace temperatures, is expanded to four constituents, alumina, lithia, zirconia, and lanthana, to produce reasonably dense polycrystals of a predominantly single phase, cubic LLZO(Al). Transformation and sintering occur concurrently at a furnace temperature near 700°C, in ambient atmosphere, in just a few seconds. The process may simplify the preparation of complex ceramics with new chemistries and dopants, which are predicted from ab intio calculations to have special attributes, not only because the powders sinter quickly at low temperatures, but also because the need for stoichiometric powders as starting materials is obviated.     

Field assisted and flash sintering of alumina and its relationship to conductivity and MgO-doping

We show that flash-sintering in MgO-doped alumina is accompanied by a sharp increase in electrical conductivity. Experiments that measure conductivity in fully dense specimens, prepared by conventional sintering, prove that this is not a cause-and-effect relationship, but instead that the concomitant increase in the sintering rate and the conductivity share a common mechanism. The underlying mechanism, however, is mystifying since electrical conductivity is controlled by the transport of the fastest moving charged species, while sintering, which requires molecular transport or chemical diffusion, is limited by the slow moving charged species. Joule heating of the specimen during flash sintering cannot account for the anomalously high sintering rates. The sintering behavior of MgO-doped alumina is compared to that of nominally pure-alumina: the differences provide insight into the underlying mechanism for flash-sintering. We show that the pre-exponential in the Arrhenius equation for conductivity is enhanced in the non-linear regime, while the activation energy remains unchanged. The nucleation of Frenkel pairs is proposed as a mechanism to explain the coupling between flash-sintering and the non-linear increase in the conductivity.     

Dynamic mechanical analysis and broadband electromagnetic interference shielding characteristics of poly (vinyl alcohol)-poly (4-styrenesulfonic acid)-titanium dioxide nanoparticles based tertiary nanocomposites

ABSTRACT

Novel tertiary nanocomposite films comprising of poly (vinyl alcohol) (PVA), poly (4-styrenesulfonic acid) (PSSA) and titanium dioxide (TiO₂) nanoparticles (NP_S) were prepared using simple solvent casting method. The structural, thermal, morphological, thermo-mechanical and electromagnetic interference (EMI) shielding properties of PVA/PSSA/TiO₂ nanocomposite films were investigated. The EMI shielding effectiveness (SE) of PVA/PSSA/TiO₂ nanocomposite films in the X and Ku band was found to be 12 dB and 13 dB respectively at 25 wt% TiO₂ NPs loading. These results demonstrate the possible applications of PVA/PSSA/TiO₂ nanocomposite films as low cost, lightweight and flexible material for EMI shielding.     

In Vitro Antiamoebic Activity Evaluation and Docking Studies of Metronidazole–Triazole Hybrids

An in‐house database of 520 compounds was docked against Entamoeba histolytica thioredoxin reductase (EhTrR), a promising target for the treatment of amoebiasis. Amongst these, some metronidazole (MTZ)–triazole hybrids were ranked high, with docking scores from ?10.23 to ?7.56. Studies of the binding orientations and conformations show that the head groups of MTZ–triazole hybrids interact with the arginine residues within the binding pocket of EhTrR, making it clear that such is the optimal and most reliable orientation for this class of compounds. The top‐ten MTZ–triazole hybrids were then selected for evaluation of their activity against the HM1:IMSS strain of amoeba. The most active compound, 2‐pyridyl‐(1,2,3‐triazolyl)metronidazole 10 , with an IC₅₀ value of 8.4 nM , was significantly more active than the standard drug MTZ alone. Docking studies revealed that compound 10 may act as an EhTrR inhibitor with activity in the nanomolar range and satisfactory ADME properties; it is a suitable candidate to be carried forward as a potential lead in the discovery of drugs to combat amoebiasis.     

Mechanical property enhancement of non‐bonding electrospun mats via adhesive

In the present study, the effect of adhesive on the morphology of different electrospun polymeric mats was investigated. The modification of two polymers, poly(methyl methacrylate) and poly(vinyl chloride), was carried out by blending the polymers with different amounts of poly(butyl acrylate) (PBA) adhesive to investigate the effect of different amounts of adhesive with heat hardener in hybrid mats. The introduction of various concentrations of PBA into different polymer solutions led to the formation of point‐bonded electrospun fibrous mats. Scanning electron microscopy images indicated that point‐bonded polymer/adhesive fibers were uniformly distributed throughout the mats. Fourier transform infrared spectrometry, contact angle measurements and thermogravimetric analysis were used to study the different properties of the hybrid mats. The tensile strength of the blended fibrous electrospun mats was increased effectively. This enhancement of the mechanical properties of the mats due to the presence of adhesive increases the number of potential applications of the electrospun mats, especially for mechanically weak polymers. Copyright © 2012 Society of Chemical Industry     

Electrochemical and peroxidase-catalyzed oxidation of epinephrine

Electrochemical and peroxidase-catalyzed oxidation of epinephrine (EPI) has been studied. In the electrochemical studies a single well-defined, 4e, 4H⁺, pH-dependent oxidation peak was observed in square wave and cyclic sweep voltammetry at edge plane pyrolytic graphite electrode. In the reverse sweep a redox couple was observed. The decay of the UV-absorbing intermediate generated and the first-order rate constants were calculated at different pH and were found to be ～6.3 × 10^?3 s^?1. The detection limit and sensitivity are found to be 17 × 10^?8 M and 2.325 μA μM^?1 respectively. At pH 7.2, the electro-oxidation product was characterized using NMR and DEPT studies as leucoadrenochrome. The peroxidase-catalyzed oxidation was carried out using horseradish peroxidase and initiated by adding H₂O₂. The identical spectral changes, rate constants and product formed during electrochemical and enzymatic oxidation suggest that the same intermediate species is generated during both the oxidations. A tentative pathway for the oxidation of EPI has been suggested. It is concluded that the electrochemical and peroxidase-catalyzed oxidation of EPI proceed by an identical pathway.     

PDMS microfluidics: A mini review

Polydimethylsiloxane (PDMS) is hailed as one of the foundational materials for microfluidics. Though a silicone-based elastomer of many desirable properties, the emergence of microfluidic fabrication techniques, especially soft lithography, has elevated its status to an exceptional one. In this mini review, we look at the salient aspects that make PDMS so special in achieving such a coveted status in the microfluidics community. A methodical approach is followed to touch upon the application of PDMS in various aspects of microfluidics with the advantages, limitations, and some future directions. © 2020 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48958.