Saadat Anwar Siddiqi

The influence of iron on the preparation of silicon nitride from silica

The thermodynamics of carbothermal reduction and nitriding of silica in the temperature range 1200 to 1600° C have been evaluated and may be used to determine the conditions required to form silicon nitride, silicon oxynitride or silicon carbide. The products of reaction are, however, frequently dictated by kinetic rather than thermodynamic considerations and the presence of impurities in the silica and carbon reactants is especially important. α-silicon nitride has been prepared from high purity silica and carbon but under identical conditions of temperature and nitrogen pressure the chemistry of the process changes markedly when a small amount of iron is added to the reactants. Below 1320° C iron has no effect and pure α-silicon nitride is formed but with increasing temperature the proportion of silicon carbide in the product increases. Above 1550° C silicon carbide is the stable solid phase in the Si-C-O-N system at 1 atm pressure. The process chemistry has been investigated by high-temperature reaction studies and X-ray diffraction and reaction mechanisms are proposed on the basis of microstructural observations of reactants and products.

Effect of epitaxy and lattice mismatch on saturation magnetization of γ′-Fe4N thin films

We report the effect of epitaxial growth and lattice mismatch on the enhancement of saturation magnetization (Ms) of ferromagnetic γ′-Fe4N thin films deposited on different single crystal substrates having lattice mismatches from 0% to 11%. It was found that Ms in the γ′-Fe4N film increased with increasing degree of epitaxy and minimizing lattice mismatch between the film and the substrate. Maximum saturation magnetization of 1980±20emu∕cm3 (about 24% higher than previous result) was obtained with LaAlO3(100) substrate having zero lattice mismatch after postannealing of 30min, which is believed to originate from magnetovolume effect in well-ordered epitaxially grown films.

Synthesis of piroxicam loaded novel electrospun biodegradable nanocomposite scaffolds for periodontal regeneration

Development of biodegradable composites having the ability to suppress or eliminate the pathogenic micro-biota or modulate the inflammatory response has attracted great interest in order to limit/repair periodontal tissue destruction. The present report includes the development of non-steroidal anti-inflammatory drug encapsulated novel biodegradable chitosan (CS)/poly(vinyl alcohol) (PVA)/hydroxyapatite (HA) electro-spun (e-spun) composite nanofibrous mats and films and study of the effect of heat treatment on fibers and films morphology. It also describes comparative in-vitro drug release profiles from heat treated and control (non-heat treated) nanofibrous mats and films containing varying concentrations of piroxicam (PX). Electrospinning was used to obtain drug loaded ultrafine fibrous mats. The physical/chemical interactions were evaluated by Fourier Transform Infrared (FT-IR) spectroscopy. The morphology, structure and pore size of the materials were investigated by scanning electron microscopy (SEM). The thermal behavior of the materials was investigated by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). Control (not heat treated) and heat treated e-spun fibers mats and films were tested for in vitro drug release studies at physiological pH7.4 and initially, as per requirement burst release patterns were observed from both fibers and films and later sustained release profiles were noted. In vitro cytocompatibility was performed using VERO cell line of epithelial cells and all the synthesized materials were found to be non-cytotoxic. The current observations suggested that these materials are potential candidates for periodontal regeneration.

Triethyl orthoformate mediated a novel crosslinking method for the preparation of hydrogels for tissue engineering applications: characterization and in vitro cytocompatibility analysis

This paper describes the development of a new crosslinking method for the synthesis of novel hydrogel films from chitosan and PVA for potential use in various biomedical applications. These hydrogel membranes were synthesized by blending different ratios of chitosan (CS) and poly(vinyl alcohol) (PVA) solutions and were crosslinked with 2.5% (w/v) triethyl orthoformate (TEOF) in the presence of 17% (w/v) sulfuric acid. The physical/chemical interactions and the presence of specific functional groups in the synthesized materials were evaluated by Fourier transform infrared (FT-IR) spectroscopy. The morphology, structure and pore size of the materials were investigated by scanning electron microscopy (SEM). Thermal gravimetric analysis (TGA) proved that these crosslinked hydrogel films have good thermal stability which was decreased as the CS ratio was increased. Differential scanning calorimetry (DSC) exhibited that CS and PVA were present in the amorphous form. The solution absorption properties were performed in phosphate buffer saline (PBS) solution of pH7.4. The 20% PVA-80% CS crosslinked hydrogel films showed a greater degree of solution absorption (183%) as compared to other compositions. The hydrogels with greater CS concentration (60% and 80%) demonstrated relatively more porous structure, better cell viability and proliferation and also revealed good blood clotting ability even after crosslinking. Based on the observed facts these hydrogels can be tailored for their potential utilization in wound healing and skin tissue engineering applications.

Enhanced magnetization of sol-gel synthesized Pb-doped strontium hexaferrites nanocrystallites at low temperature

Effect of Pb doping on the structural and low temperature magnetic properties of SrPbxFe12-xO19 (x = 0, 0.1, 0.2, 0.3, and 0.4), synthesized by sol-gel autocombustion technique, has been investigated. The powder samples were sintered at 800°C for 2 h in order to develop the stable hexagonal phase, characteristic of the SrFe12O19 structure. The consequences of Pb substitution (at iron sites) on various structural parameters like lattice constants, unit cell volume, crystallite size, and porosity have been discussed. Fourier transform infrared frequency bands were utilized to determine the formation of tetrahedral and octahedral clusters of M-type ferrites. Hexagonal texture of the grains, a characteristic of the hexagonal crystal structure of SrFe12O19, was refined by Pb substitution. The magnetic properties, determined using a vibrating sample magnetometer, revealed that saturation magnetization decreased, while coercivity was increased with the increase of Pb contents. However, the increased squareness ratio and hence the energy product motivate the utilization of these ferrite compositions where hard magnetic characteristics are required.The increased values of saturation magnetization were observed at reduced temperature of 200 K, attributable to the better spin alignments of individual magnetic moments at low temperature.

Room Temperature Magnetic Behavior of Sol-Gel Synthesized Mn Doped ZnO

Mn doped ZnO nano-crystallites were synthesized by state of the art sol-gel derived auto-combustion technique. As-burnt powder was investigated with different characterization techniques to explore the properties of Mn doped ZnO dilute magnetic semiconductor. X-ray diffraction measurements indicate that Mn doped ZnO retain wurtzite type hexagonal crystal structure like ZnO. Compositional and morphological studies were carried out by energy dispersive X-ray analysis and scanning electron microscopy, respectively. Temperature dependent resistivity of the sample exhibited the semiconducting behavior of the DMS material. Room temperature magnetic properties determined by vibrating sample magnetometer, revealed the presence of ferromagnetic and diamagnetic contributions in Mn doped ZnO.

Effect of Co substitution on the structural, electrical, and magnetic properties of Bi0.9La0.1FeO3 by sol-gel synthesis

Cobalt (Co)-doped Bi0.9La0.1FeO3 multiferroics were synthesized by a sol-gel method based on the autocombustion technique. As-synthesized powder was examined using various characterization techniques to explore the effect of Co substitution on the properties of Bi0.9La0.1FeO3. X-ray diffraction reveals that Co-doped Bi0.9La0.1FeO3 preserves the perovskite-type rhombohedral structure of BiFeO3, and the composition without Co preserves the original structure of the phase; however, a second-phase Bi2Fe4O9 has been identified in all other compositions. Surface morphological studies were performed by scanning electron microscopy. Temperature-dependent resistivity of the samples reveals the characteristic insulating behavior of the multiferroic material. The resistivity is found to decrease with the increase both in temperature and Co content. Room temperature frequency-dependent dielectric measurements were also reported. Magnetic measurements show the enhancement in magnetization with the increase in Co content.

A new synthetic methodology for the preparation of biocompatible and organo-soluble barbituric- and thiobarbituric acid based chitosan derivatives for biomedical applications

Chitosans poor solubility especially in organic solvents limits its use with other organo-soluble polymers; however such combinations are highly required to tailor their properties for specific biomedical applications. This paper describes the development of a new synthetic methodology for the synthesis of organo-soluble chitosan derivatives. These derivatives were synthesized from chitosan (CS), triethyl orthoformate and barbituric or thiobarbituric acid in the presence of 2-butannol. The chemical interactions and new functional motifs in the synthesized CS derivatives were evaluated by FTIR, DSC/TGA, UV/VIS, XRD and (1)H NMR spectroscopy. A cytotoxicity investigation for these materials was performed by cell culture method using VERO cell line and all the synthesized derivatives were found to be non-toxic. The solubility analysis showed that these derivatives were readily soluble in organic solvents including DMSO and DMF. Their potential to use with organo-soluble commercially available polymers was exploited by electrospinning; the synthesized derivatives in combination with polycaprolactone delivered nanofibrous membranes.

Production of chitosan PVA PCL hydrogels to bind heparin and induce angiogenesis

ABSTRACT New blood vessel formation is an essential part of wound healing to provide cells with the nutrients and oxygen for their survival. Many nonhealing ulcers fail to heal because of poor blood supply and skin grafts will also fail to take on poorly vascularized wound beds. There is a real need for proangiogenic biomaterials to assist wound healing. In vivo heparin binds proangiogenic growth factors and helps regulate new blood vessel formation, hence heparin containing biomaterials are attractive. To achieve a hydrogel with high heparin binding capacity a composite of chitosan, poly(vinyl alcohol) (PVA) and polycaprolactone (PCL) was produced. Chitosan is a biodegradable natural polymer with great potential for biomedical applications due to its biocompatibility, high charge density and nontoxicity. PVA is biocompatible and nontoxic with good chemical stability, film-forming ability, and high hydrophilicity. PCL has physicochemical and mechanical properties comparable to those of the biological tissues and due its hydrophilic nature helps in the sustained release of drugs. Accordingly in this study we explored a range of PCL concentrations from 4% to 16% added to hydrogels composed of chitosan and PVA. Heparin was blended into the polymer mixture and the nanoporous structure was created by freeze-drying the PCL hydrogel. The physical properties of the hydrogels were evaluated by Fourier transform infrared spectroscopy (FTIR) and XPS confirmed the presence of sulfur on the surface of the hydrogels. Their porous morphology was investigated by scanning electron microscope (SEM). The Chick Chorionic Allantoic Membrane (CAM) assay was used to study the angiogenic potential of these materials and histology (H&E and Goldner trochome) was used to confirm the presence of new blood vessels inside the hydrogels. We report that the addition of 8% PCL to the hydrogels gave porous structures containing heparin, which significantly increased new blood vessel formation into the hydrogels. These hydrogels offer a new approach to biomaterials, which could be added to wounds to improve vascularization. GRAPHICAL ABSTRACT

Structural, Magnetic, and Electrical Properties of Al3+ Substituted CuZn-ferrites

Nanocrystalline Cu0.5Zn0.5AlxFe2−xO2 (x=0.0, 0.1, 0.2, 0.3, 0.4, and 0.5) ferrite materials were synthesized using standard solid state reaction technique. The effects of Al3+ contents on the structural, electrical, and magnetic properties were investigated. Single phase cubic spinel structure was revealed by X-ray diffraction analysis. The crystallite size was evaluated considering the most intense diffraction peak (311) using Scherrer formula. Lattice constant decreased, whereas porosity increased with the increase in Al3+ concentration. The value of saturation magnetization decreased with increasing aluminum contents. Temperature dependent value of direct current electrical resistivity has been determined. It is observed that the substitution of Al3+ has significant impact on the dielectric constant, tangent of dielectric loss angle and dielectric loss factor. The variation in dielectric properties was attributed to space charge polarization.