Nano and micro structural studies of thin films of ZnO

Zinc oxide thin films grown by sol–gel and RF sputtering methods have been characterized. The characterization techniques used involve ellipsometry, optical absorption, scanning tunneling microscopy, scanning and transmission electron microscopy. The films grown by sol–gel spin method which followed zinc acetate route exhibited a smoother texture than the films, which were deposited by using zinc nitrate route. The later type of films showed a dendritic character. Nano-structured fine grains of size ranging from 20 to 60 nm were observed with zinc nitrate precursor film. Individual grains show a sharp contrast with different facets and boundaries. Crystal planes and lattice parameters calculated by electron diffraction and X-ray diffraction are quite close and in agreement with the reported values in literature. Scanning tunneling microscopy has been used for measuring the average roughness of the surface and estimating the lattice constants. The STM studies of RF sputtered films, although showing a ZnO structure, exhibited a disturbed lattice. This was presumably due to the fact that after deposition the films were not annealed. Nanographs of 2D and 3D view of atomic positions of ZnO have been presented by using scanning tunneling microscopy.     

Novel model reference adaptive control architecture using semi‐initial excitation‐based switched parameter estimator

This paper is a generalization of the recently developed techniques of initial excitation (IE)–based adaptive control with an introduction to the definition of semi‐initial excitation (semi‐IE), a still more relaxed notion than IE. Classical adaptive controllers typically ensure Lyapunov stability of the extended error dynamics (tracking error + parameter estimation error) and asymptotic tracking, while requiring a stringent condition of persistence of excitation (PE) for parameter convergence. Of late, the authors have proposed a new adaptive control architecture, which guarantees parameter convergence under the online‐verifiable IE condition leading to exponential stability of the extended error dynamics. In earlier works, it has been established that the IE condition is significantly milder than the classical PE condition. The current work further slackens the excitation condition by proposing the concept of semi‐IE. The proposed adaptive controller is proved to ensure convergence of the parameter estimation error to a lower‐dimensional manifold under the weaker semi‐IE condition, while the stronger condition of IE guarantees convergence of the parameter estimation error to zero. The designed algorithm is shown to improve transient response of tracking error sufficiently in contrast to conventional adaptive controllers.     

Pulsed Electrical Stimulation and Surface Charge Induced Cell Growth on Multistage Spark Plasma Sintered Hydroxyapatite‐Barium Titanate Piezobiocomposite

The primary purpose of the present work was to illustrate whether cell proliferation can be enhanced on electroactive bioceramic composite, when the cells are cultured in the presence of external electrical stimulation. The two different aspects of the influence of electric field (E‐field) application toward stimulating the growth/proliferation of bone/connective tissue cells in vitro, (a) intermittent delivery of extremely low strength pulsed electrical stimulation (0.5–4 V/cm, 400 μs DC pulse) and (b) surface charge generated by electrical poling (10 kV/cm) of hydroxyapatite (HA)‐BaTiO₃ piezobiocomposite have been demonstrated. The experimental results establish that the cell growth can be enhanced using the new culture protocol of the intermittent delivery of electrical pulses within a narrow range of stimulation parameters. The optimal E‐field strength for enhanced cellular response for mouse fibroblast L929 and osteogenic cells is in the range of 0.5–1 V/cm. The MTT [3‐(4, 5‐dimethylthiazol‐2‐yl)‐2, 5‐diphenyl tetrazolium bromide] assay results suggested the increased viability of E‐field treated cells over 7 d in culture, implicating the positive impact of electrical pulses on proliferation behavior. The alizarin red assay results showed noticeable increase in Ca‐deposition on the E‐field treated samples in comparison to their untreated counterparts. The negatively charged surfaces of developed piezocomposite stimulated the cell growth in a statistically noticeable manner as compared with the uncharged or positively charged surfaces of similar composition.     

Development of topical gel containing aceclofenac-crospovidone solid dispersion by “Quality by Design (QbD)” approach

This article describes the development, optimization, and evaluation of Carbopol 940 topical gel containing aceclofenac-crospovidone (1:4) solid dispersion using “Quality by Design (QbD)” approach based on 2³ factorial design. The effect of crospovidone, tri-ethanolamine, and ethyl alcohol amount on the drug permeation profile of the topical gel containing aceclofenac-crospovidone solid dispersion was optimized by 2³ factorial design. The optimized gel showed improved permeation profile with cumulative drug permeation of 26.262 ± 2.157%, and permeation flux of 0.059 ± 0.011 μg/cm²/h. These gels were characterized by pH, viscosity, gel strength and FTIR study. The in vivo anti-inflammatory activity of the optimized gel was evaluated in rats using carrageenan-induced rat-paw oedema model and found excellent anti-inflammatory comparable with a marketed gel without producing any skin irritation.     

Electrophoretic Deposition of Zirconia Thin Film on Nonconducting Substrate for Solid Oxide Fuel Cell Application

Electrophoretic deposition (EPD) of 8 mol% yttria‐stabilized zirconia (YSZ) electrolyte thin film has been carried out onto nonconducting porous NiO‐YSZ cermet anode substrate using a fugitive and electrically conducting polymer interlayer for solid oxide fuel cell (SOFC) application. Such polymer interlayer burnt out during the high‐temperature sintering process (1400°C for 6 h) leaving behind a well adhered, dense, and uniform ceramic YSZ electrolyte film on the top of the porous anode substrate. The EPD kinetics have been studied in depth. It is found that homogeneous and uniform film could be obtained onto the polymer‐coated substrate at an applied voltage of 15 V for 1 min. After the half‐cell (anode + electrolyte) is co‐fired at 1400°C, a suitable cathode composition (La_0.65Sr_0.3MnO₃) thick film paste is screen printed on the top of the sintered YSZ electrolyte. A second stage of sintering of such cathode thick film at 1100°C for 2 h finally yield a single cell SOFC. Such single cell produced a power output of 0.91 W/cm² at 0.7 V when measured at 800°C using hydrogen and oxygen as fuel and oxidant, respectively.     

One pot synthesis of nano Ag in calcium alginate beads and its catalytic application in p‐Nitrophenol reduction with kinetic parameter estimation and model fitting

In this work, one step process of synthesis of silver nanoparticles (Agnp) embedded in insitu formed calcium alginate (CA) beads is stated. CA, formed from the reaction between sodium alginate and calcium hydroxide, acts as reducing and stabilizing agent as well as support for nanoparticles. The reaction mechanism for the formation and stabilization of Agnp is proposed where the vicinal dihydroxy groups of alginate are assumed to act as the reducing agent for Ag⁺ to Ag°. Transmission electron microscopy (TEM), x‐ray diffraction (XRD), UV‐vis spectroscopy, field emission scanning electron microscopy (FESEM), and atomic absorption spectroscopy (AAS) were used to characterize the Agnp. The formation of spherical nanoparticles with average size range of 4‐5 nm was confirmed by TEM. Catalytic activity of this nano silver‐calcium alginate (Agnp‐CA) composite was evaluated in the reduction of p‐nitrophenol. Concentrations of sodium alginate, calcium hydroxide, and AgNO₃ are found to be the parameters that critically affect the synthesis of Agnp. The efficacy of the catalyst is expressed on the basis of suitable reaction parameters. Both pseudo‐homogeneous and heterogeneous kinetic models are proposed for the reaction to find the best model and the Eley‐Riedel model is found to fit well with the experimental data. The novelty of this work is that the tandem process of CA bead formation, Agnp formation, and Agnp entrapment in CA have been transformed into a single‐step process. Moreover, elaborations of each step of the ionic mechanisms of Agnp formation and p‐NP reduction with Agnp and the establishment of a heterogeneous kinetic model for the reaction are reported for the first time here.     

Structural drivers controlling sulfur solubility in alkali aluminoborosilicate glasses

If the direct feed approach to vitrify the Hanford's tank waste is implemented, the low activity waste (LAW) will comprise higher concentrations of alkali/alkaline-earth sulfates than expected under the previously proposed vitrification scheme. To ensure a minimal impact of higher sulfate concentrations on the downstream operations and overall cost of vitrification, advanced glass formulations with enhanced sulfate loadings (solubility) are needed. While, the current sulfate solubility predictive models have been successful in designing LAW glasses with sulfate loadings <2 wt.%, it will be difficult for them to design glass compositions with enhanced loadings due to our limited understanding of the fundamental science governing these processes. In this pursuit, this article unearths the underlying compositional and structural drivers controlling the sulfate solubility in model LAW glasses. It has been shown that the preferentially removes non-framework cations from the modifier sites in the silicate network, thus, leading to the polymerization in the glass network via the formation of ring-structured borosilicate units. Furthermore, though the sulfate solubility slightly decreases with increasing Li⁺/Na⁺ in the glasses, the prefers to be charge compensated by Na⁺, as it is easier for to break Na–O bonds instead of Li–O bonds.     

Quantification of Dendritic Spines Remodeling under Physiological Stimuli and in Pathological Conditions

Numerous brain diseases are associated with abnormalities in morphology and density of dendritic spines, small membranous protrusions whose structural geometry correlates with the strength of synaptic connections. Thus, the quantitative analysis of dendritic spines remodeling in microscopic images is one of the key elements towards understanding mechanisms of structural neuronal plasticity and bases of brain pathology. In the following article, we review experimental approaches designed to assess quantitative features of dendritic spines under physiological stimuli and in pathological conditions. We compare various methodological pipelines of biological models, sample preparation, data analysis, image acquisition, sample size, and statistical analysis. The methodology and results of relevant experiments are systematically summarized in a tabular form. In particular, we focus on quantitative data regarding the number of animals, cells, dendritic spines, types of studied parameters, size of observed changes, and their statistical significance.     

Supported Gold Nanoparticles‐Catalyzed Microwave‐Assisted Hydration of Nitriles to Amides under Base‐Free Conditions

Polystyrene‐supported gold (Au@PS) nanoparticles were synthesized by the reduction deposition approach and well characterized by UV‐visible, XRD, TEM, SAED, EDX, and XPS studies. The Au@PS was applied as catalyst for the hydration of nitriles to amides in water under microwave irradiation. Several functionalized aromatic, heterocyclic and aliphatic nitriles were found to be active for synthesis of the corresponding amides where no activation of water by base, ligand and support is needed. Easy recovery, negligible leaching and recyclability for up to eight runs are added advantages of the catalyst under water‐mediated reaction conditions.