On the study of phase formation and critical current density in superconducting MgB2

Superconducting bulk MgB₂ samples have been synthesized by employing sintering technique without using any additional process steps, generally undertaken in view of the substantial loss of magnesium, during heat treatment. Starting with Mg rich powders having different atomic ratios of Mg : B, as against the nominally required Mg : B = 1:2 ratio, we have obtained superconducting MgB₂ samples of different characteristics. The effect of excess Mg in the starting mixture and processing temperature on the phase-formation, transition temperature (T _C) and critical current density (J _C) have been investigated by electrical transport and a.c. susceptibility measurements. The X-ray diffraction and X-ray photoelectron spectroscopic analyses of MgB₂ bulk samples have been carried out to understand the role of excess Mg and the effect of processing temperature. It is established that MgB₂ samples with high critical current density can be synthesized from a Mg rich powder having Mg : B in 2:2 ratio, at temperatures around 790°C. Critical current density has been found to vary systematically with processing temperature.     

Studies on broad spectrum corrosion resistant oxide coatings

The corrosion resistant oxide coatings, developed and applied by the conventional vitreous enamelling techniques, showed superior resistance to a range of mineral acids at various strengths and temperatures, alkaline solutions, boiling water and chrome plating solutions. These coatings possess considerable abrasion and impact resistance as well as high thermal shock resistance. The properties of the coating system have been studied in detail and found to be strongly dependent on composition and processing parameters. These coatings have been characterized by X-ray diffraction analysis and SEM studies. Some of the coating materials have been found to be biocompatible.     

Synthesis, characterization and gas sensing property of hydroxyapatite ceramic

Hydroxyapatite (HAp) biomaterial ceramic was synthesized by three different processing routes viz. wet chemical process, microwave irradiation process, and hydrothermal technique. The synthesized ceramic powders were characterized by SEM, XRD, FTIR and XPS techniques. The dielectric measurements were carried out as a function of frequency at room temperature and the preliminary study on CO gas sensing property of hydroxyapatite was investigated. The XRD pattern of the hydroxyapatite biomaterial revealed that hydroxyapatite ceramic has hexagonal structure. The average crystallite size was found to be in the range 31–54 nm. Absorption bands corresponding to phosphate and hydroxyl functional groups, which are characteristic of hydroxyapatite, were confirmed by FTIR. The dielectric constant was found to vary in the range 9–13 at room temperature. Hydroxyapatite can be used as CO gas sensor at an optimum temperature near 125°C. X-ray photoelectron spectroscopic studies showed the Ca/P ratio of 1.63 for the HAp sample prepared by chemical process. The microwave irradiation technique yielded calcium rich HAp whereas calcium deficient HAp was obtained by hydrothermal method.     

Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering

Abstract

The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method.     

Structural morphology of amorphous conducting carbon film

Amorphous conducting carbon films deposited over quartz substrates were analysed using X-ray diffraction and AFM technique. X-ray diffraction data reveal disorder and roughness in the plane of graphene sheet as compared to that of graphite. This roughness increases with decrease in preparation temperature. The AFM data shows surface roughness of carbon films depending on preparation temperatures. The surface roughness increases with decrease in preparation temperature. Also some nucleating islands were seen on the samples prepared at 900°C, which are not present on the films prepared at 700°C. Detailed analysis of these islands reveals distorted graphitic lattice arrangement. So we believe these islands to be nucleating graphitic. Power spectrum density (PSD) analysis of the carbon surface indicates a transition from the nonlinear growth mode to linear surface-diffusion dominated growth mode resulting in a relatively smoother surface as one moves from low preparation temperature to high preparation temperature. The amorphous carbon films deposited over a rough quartz substrate reveal nucleating diamond like structures. The density of these nucleating diamond like structures was found to be independent of substrate temperature (700–900° C).     

Homogenization of zinc distribution in vertical Bridgman grown Cd0.96Zn0.04Te crystals

One of the most pressing issues in the growth of high quality single crystal Cd _0.96 Zn _0.04 Te material, is to achieve homogenization of the high axial variation of Zn concentration, caused by the larger than unity segregation coefficient of Zn in CdTe. This is achieved in our crystals (i) by thermal annealing of the CdZnTe crystal, which redistributes the as grown Zn distribution by solid state diffusion of Zn (this solid state diffusion of Zn occurs at three stages (a) during the growth when the solidified crystal is near to the melting point temperature, (b) during the post growth annealing of the crystal at a high temperature and (c) during the cooldown to room temperature) and (ii) by the reduction of Zn segregation during the growth stage by enhanced convective mixing of the melt, through a proper choice of ampoule and furnace dimensions. By adopting suitable growth parameters and sufficient post growth annealing it has been possible to grow Cd _0.96 Zn _0.04 Te crystals, which have nearly 75% of their fraction within 1% Zn concentration variation.     

Effects of organic binders on the sintering of isostatically compacted zirconia powders

Certain processing-related flaws in cold isostatically pressed ceramic powder compacts may arise from the delayed burn-out of organic binders until the sintering temperature is approached, although the isostatic compaction technique usually gives a higher and much more uniform green density than the conventional die compaction technique. For the 3 mol% Y₂O₃-doped zirconia powder in which 3 wt% PEG 1500 was introduced, the sintered density and sintering shrinkage were found to decrease in a near linear manner with increasing isostatic compaction pressure. The processing-related defects were identified as intergranular pores (1–5 m). It is considered that these processing-related defects are a consequence of incomplete organic burn-out at low and intermediate temperatures in the heating-up period and the swelling of intergranular pores associated with the burn-out of residual organic binders at temperatures close to the sintering temperature. A higher calcination temperature and an extended calcination dwell time may be required to eliminate the organic residuals in the isostatically pressed ceramic powder compacts than in the conventional die-pressed samples.     

External stimuli response on a novel chitosan hydrogel crosslinked with formaldehyde

Keeping in mind the significance of hydrogels as an external stimuli sensitive super absorbing material, some transparent covalent hydrogels of chitosan were prepared by crosslinking with varying amounts of formaldehyde solution used as crosslinking agent. The characteristics of hydrogels were investigated by Fourier transform infrared (FT-IR) spectroscopy and swelling experiments. The effect of crosslinking agent on water absorbency has been investigated. The hydrogels exhibited a relatively higher swelling ratio in the range of 2066–3306% and equilibrium water content (EWC) in the range of 95-38–97 06% at pH 7 and 35°C temperature. The influence of external stimuli such as pH, temperature, and ionic strength of the swelling media on equilibrium swelling properties has been observed. Hydrogels showed a typical pH and temperature responsive behaviour such as low pH and high temperature has maximum swelling while high pH and low temperature show minimum swelling. An increase in the ionic strength of swelling media caused a continuous decrease in the swelling of hydrogels at both acidic and basic pH.     

Growth and characterization of gel grown pure and mixed iron-manganese levo-tartrate crystals

Several applications of iron tartrate and manganese tartrate compounds are reported in the literature. In the present investigation, we have grown pure and mixed iron (II)-manganese levo-tartrate crystals by single diffusion gel growth technique. Crystals with spherulitic morphology were harvested. The colouration of the crystals changed from black to pinkish brown upon increasing the content of manganese in the crystals. The crystals were characterized by FTIR spectroscopy, powder XRD, TGA, VSM and dielectric study. Crystal structures of different mixed crystals were studied. From TGA it was observed that on heating the hydrated crystals became anhydrous and then converted into oxides. Paramagnetic nature of the crystals was revealed from VSM study. The variation of the dielectric constant with frequency was studied. The results are discussed.     

Solution-combustion synthesis of Bi1−x Ln x O1.5 (Ln = Y and La-Yb) oxide ion conductors

Cubic fluorite related Bi_1−x LnxO1.5 (Ln = Y and LaYb) phases are synthesized by solution-combustion method using glycine as the fuel. The cubic fluorite phase is stabilized with 25 mole% of rare earth cations. The lattice parameter of cubic phase increases linearly with size of the lanthanide ion. The synthesized powders are nano-metric in size and exhibit excellent compactability and reach 98% densification even on short period of sintering. The oxides with relatively larger cations Nd, Sm, Eu, Pr and Gd with 25 mole% composition transform to rhombohedral structure while others retain cubic upon sintering. All the phases show high oxide-ion conductivity and the values obtained are in good agreement with the reported values.     

On the electronic structure and equation of state in high pressure studies of solids

We discuss the high pressure behaviour of zinc as an interesting example of controversy, and of extensive interplay between theory and experiment. We present its room temperature electronic structure calculations to study the temperature effect on the occurrence of its controversial axial ratio (c/a) anomaly under pressure, and the related electronic topological transition (ETT). We have employed a dense 63 X 63 X 29 k-point sampling of the Brillouin zone and find that the small (c/a) anomaly near 10 GPa pressure persists at room temperature. A weak signature of the anomaly can be seen in the pressure-volume curve, which gets enhanced in the universal equation of state, along with that of K-point ETTs. We attribute the change of slope in the universal equation of state near 10 GPa pressure, mainly to hybridization effects. The temperature effect in fact enhances the possibility of L-point ETT. We find that the L-point ETT is very sensitive to exchange correlation terms, and hence we suggest that further refinements in the theoretical techniques are needed to resolve the controversies on the ETT in Zn.     

Study of lithium glassy solid electrolyte/electrode interface by impedance analysis

Cells of lithium ion conducting glassy electrolyte Li ₂SO₄-Li₂O-B₂O₃ with different combinations of electrodes (stainless steel blocking electrode, lithium non-blocking electrode and TiS₂ electrode) have been prepared. The a.c. impedance measurements of the cells have been studied at elevated temperature as a function of time. The circuit elements such as bulk resistance, double layer capacitance and charge transfer resistance have been inferred and their time dependence studied. The results show that the electrolyte and the interface are chemically very stable with the different types of electrodes studied here.     

Potentiometric study of polyaniline film synthesized with various dopants and composite-dopant: A comparative study

The potentiometric study of polyaniline (PANI) film synthesized with dopants viz. polyvinyl sulfonic acid (PVS),p-toluene sulfonic acid (p TS), dodecyl benzene sulfonic acid (DBS) and composite-dopants viz. PVS-p TS and PVS-DBS, has been carried out. The synthesized PANI films were characterized by electrochemical technique, UV-visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and conductivity measurement. It was found that the PANI doped with PVS gives good electrochemical properties, conductivity as well as surface morphology as compared to p TS and DBS, whereas in composite dopants the PANI doped with PVS-pTS gives good polymer matrix as compared to PVS-DBS.     

Effect of heat treatment on properties of steam cured fly ash-lime compacts

Four different varieties of class F fly ashes, collected from different sources from the state of West Bengal (India) were mixed with lime in 9 : 1 wt ratio, followed by compaction of the mixes. The compacts were subjected to steam curing to develop an optimum strength by the reaction between fly ash and lime. The steam cured compacts were heated at different elevated temperatures and free lime content, compressive strength, bulk density and water absorption tendency of these compacts were measured and FTIR spectral changes were studied as a function of the heating temperatures. Kinetics of thermal dehydration of the compacts was also studied from thermogravimetric measurements under non-isothermal condition to ascertain the order of dehydration process and the associated activation energy.     

A study of ultrasonic velocity and attenuation on polycrystalline Ni-Zn ferrites

Polycrystalline NiZn ferrites with different grain sizes (1.2 (Am to 10.2 (Am) were prepared by the usual ceramic method. The magnetic properties were measured at room temperature. The ultrasonic velocity and attenuation were measured on Ni-Zn ferrite by using the pulse transmission method at 1 MHz, in the temperature range 300–600 K. The velocity was found to be slightly sample dependent at room temperature and decreased with increasing temperature, except near the Curie temperature, T _c ,where a small anomaly was observed. The longitudinal attenuation (α ₁ )at room temperature was found to be more sample dependent. The temperature variation of ultrasonic longitudinal attenuation exhibited a broad maximum around 400 K and a sharp maximum just below Curie temperature ( T _c ).The above observations were carried out in the demagnetized state. The application of a 380 mT magnetic field allowed us to reach the saturated state of the sample at all the measuring temperatures. The anomaly observed in the thermal variation of velocities (longitudinal and transverse) and attenuation has been qualitatively explained with the help of the temperature variation of the magneto-crystalline anisotropy constant.     

Preparation of Porous Ceramics from Nanocrystalline Zirconia and Their Microstructure

Data are presented on the compaction behavior of nanocrystalline yttria partially stabilized zirconia powder and the effects of compaction pressure, sintering temperature, and sintering time on the microstructure of the resultant ceramics. It is shown that even relatively low (50 MPa) compaction pressures lead to the disintegration of powder particles and aggregates. The compaction behavior of the powder points to changes in the densification mechanism: from quasi-liquid sliding of powder particles at the beginning of the process to the breakdown of large microstructural constituents at the end. In the initial stages of sintering, a robust skeleton forms, which plays a key role in determining the pore structure of the ceramic.     

Studies on conductivity and dielectric properties of polyaniline-zinc sulphide composites

In the present paper, we report electrical conductivity and dielectric studies on the composites of conducting polyaniline (PANI) with crystalline semiconducting ZnS powder, wherein PANI has been taken as inclusion and ZnS crystallites as the host matrix. From the studies, it has been observed that the value of room temperature d.c. conductivity of the composites with volume fraction of PANI > 0.65 shows an unusual behaviour wherein, conductivity values of the composites exceed that of PANI itself with maximum value as high as 6 times that of PANI at the volume fraction of 0.85. A similar trend has also been observed for the real and imaginary parts of complex dielectric constant values of the composites. This unusual behaviour in the d.c. conductivity and dielectric properties has been attributed to the enhancement in the degree of crystallinity of PANI as a consequence of its interfacial interaction with ZnS matrix. The results of optical microscopy show coating of PANI all around the ZnS particles. The temperature dependent conductivity studies suggest the quasi one-dimensional VRH conduction in PANI as well as its composites with ZnS. FTIR and XRD studies have also been reported.     

Synthesis and magnetic study of Co-Al substituted calcium hexaferrite

A series of calcium substituted polycrystalline ferrite ceramics with magnetoplumbite structures were synthesized using perfect stoichiometric mixtures of oxides with chemical composition, CaAl_xCo_xFe_12−2xO₁₉ (x = 2−5), by standard ceramic technique. The variation in the values ofH _candM _s,which depends on the additive content and the temperature, was studied by means of a vibration magnetometer. The strong variation observed in coercivity, saturation magnetization and Curie temperature with chemical composition give rise to the possibility of controlling these properties and hence applying these compounds in the millimeter— microwave range.     

Overview literature on matrix assisted laser desorption ionization mass spectroscopy (MALDI MS): Basics and its applications in characterizing polymeric materials

Matrix assisted laser desorption ionization mass spectroscopy (MALDI MS) is a technique which allows the measurement of molecular mass > 200,000 Daltons by ionization and vapourization without degradation. This technique is useful for the mass analysis of synthetic polymers, which have very low volatility. The basic principles of and its applications for polymer characterization have been discussed in this paper. In addition, the possibilities of combining MALDI MS with chromatographic and other analytical techniques have also been discussed.     

A new high temperature resistant glass-ceramic coating for gas turbine engine components

A new high temperature and abrasion resistant glass-ceramic coating system (based on MgO-Al₂O₃-TiO₂ and ZnO-Al₂O₃-SiO₂ based glass systems) for gas turbine engine components has been developed. Thermal shock resistance, adherence at 90°-bend test and static oxidation resistance at the required working temperature (1000°C) for continuous service and abrasion resistance are evaluated using suitable standard methods. The coating materials and the resultant coatings are characterized using differential thermal analysis, differential thermogravimetric analysis, X-ray diffraction analysis, optical microscopy and scanning electron microscopy. The properties evaluated clearly showed the suitability of these coatings for protection of different hot zone components in different types of engines. XRD analysis of the coating materials and the resultant coatings showed presence of a number of microcrystalline phases. SEM micrographs indicate strong chemical bonding at the metal-ceramic interface. Optical micrographs showed smooth glossy impervious defect free surface finish.