• Volume 28, Issue 2

April 2005,   pages  81-185

• Corrosion of steel structures in sea-bed sediment

Seabed sediment (SBS) is a special soil that is covered by seawater. With the developments in marine oil exploitation and engineering, more and more steel structures have been buried in SBS. SBS corrosion has now become a serious problem in marine environment and an important issue in corrosion science. In this paper, approach in the field of SBS corrosion is reviewed. Electrochemical and microbial corrosion factors, corrosion mechanism, measurement of metal corrosion rate, corrosion evaluation and prediction of corrosion are also discussed here.

• Effect of heat treatment on martensitic transformation in Fe–12.5%Mn–5.5%Si–9%Cr–3.5%Ni alloy

In this study, thermally-induced martensitic transformation ($\gamma(fcc) \rightarrow \varepsilon(hcp)$) in Fe–12.5%Mn–5.5%Si–9%Cr–3.5%Ni (weight) alloy was studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of cooling rate was investigated. It was observed that fast cooled sample exhibited regular overlapping of stacking faults and 𝜀 martensite plates were formed parallel to each other. TEM investigations showed that the orientation relationship between 𝛾–𝜀 phases corresponds to Shoji–Nishiyama type orientation relationship.

• Influence of thermomechanical aging on fatigue behaviour of 2014 Al-alloy

The fatigue behaviour of 2014 Al-alloy has been studied in various thermomechanically aged conditions. It is observed that fatigue properties can be improved by a thermomechanical treatment, which would reduce the concentrations of dispersoids, provide a relatively uniform deformation structure and produce fine distribution of 𝜃' precipitates. Fine 𝜃' particles inhibit dynamic recovery and produce uniform deformation structure, which improves fatigue behaviour. Presence of dispersoids and coarse precipitate particles leads to the formation of persistent slip bands (PSBs) and a highly heterogeneous deformation structure, which cause damage to fatigue properties.

• Growth and characterization of Hg1–𝑥Cd𝑥Te epitaxial films by isothermal vapour phase epitaxy (ISOVPE)

Growth of Hg1–𝑥Cd𝑥Te epitaxial films by a new technique called asymmetric vapour phase epitaxy (ASVPE) has been carried out on CdTe and CZT substrates. The critical problems faced in normal vapour phase epitaxy technique like poor surface morphology, composition gradient and dislocation multiplication have been successfully solved. The epitaxial films have been electrically characterized by using the Hall effect and capacitance–voltage (𝐶–𝑉) measurements.

• Dispersion and rheological studies of Y–PSZ tape casting slurry

Different solvent systems in combination with three different dispersants were tried to find out the suitable solvent–dispersant combination, which give optimum dispersion of PSZ. Based on sedimentation, viscosity and rheology characteristics, zeotropic ethanol : xylene with a ratio of 50 : 50 along with 0.5 wt% phosphate ester was found to be the best solvent and dispersant combination. Optimized tape casting slurry was prepared using PEG 600 and BBP as plasticizers and PVB as the binder. Cyclohexanone was used as the homogenizer. The optimized slurry composition with 58% solid loading exhibited shear-thinning pseudoplastic rheological behaviour. Y–PSZ tapes of ∼ 50 𝜇m thickness free from visible defects were cast with a green tape density of 55%.

• Role of dispersion conditions on grindability of yttria stabilized zirconia (YSZ) powders

A precursor for zirconia – 8 mole% yttria (YSZ–ZrO2–8 m% Y2O3) powder was prepared by coprecipitation and the calcination temperature was fixed as 900°C from TG–DTA and XRD studies. The calcined powder could be dry ground only to a mean particle size (𝐷50) of 6 𝜇m containing substantial amount of coarse agglomerates in the size range 10–100 𝜇m. The dispersion conditions for its wet grinding were evaluated through zeta-potential and viscosity studies. The zeta-potential variation with pH of the aqueous suspensions of the powder exhibited maximum numerical values at 3 and 11 pH, exhibiting the ideal pHs for dispersion stability through electrostatic columbic repulsion mechanism. Slurries of dry ground powders with solid concentration in the range 15–30 vol.% exhibited pseudo-plastic flow characteristics, indicating presence of flocculates. With progress of grinding, the increase in viscosity of the slurries became less significant with decreasing solid concentration. Even though the particle size of the ground slurries decreased with decreasing solid content, there was little change in it for slurries with solid content &lt; 20 vol.%. Grinding conditions for formation of sinter-active powders of YSZ with sub-micron size (𝐷50\ ∼ 0.7 𝜇m free of agglomerates of size &gt; 5 𝜇m) were established. Compacts from this powder could be sintered at 1400°C to translucent bodies with 99% theoretical density.

• Development of calcium phosphate based apatite from hen’s eggshell

Stoichiometric hydroxyapatite with Ca/P molar ratio, 1.67, was synthesized using hen’s eggshell as calcium source and phosphoric acid by precipitation method. Conventional EDTA titration and gravimetric methods were adopted to estimate the amount of calcium and phosphorous, respectively. Fourier-transform infrared (FT–IR) and X-ray diffraction (XRD) techniques were employed to investigate the formation of the HAP phase. Thermal analysis (TG–DTA) was carried out to investigate the thermal stability of HAP powder. FT–IR spectra show the characteristic peaks for phosphate and hydroxyl groups. XRD results reveal that the major characteristic peaks of HAP appear in the region of approximately 26°, 28°, 29°, 30–35°, 39°, 46°, 49° and 50° (2𝜃) and also indicate that there are no occurrences of secondary phases during HAP formation. TG–DTA result depicts that the synthesized HAP was stable up to 1300°C.

• Preparation of nanocrystalline ferroelectric BaNb2O6 by citrate gel method

A gel was formed when a aqueous solution of BaCl2, NbF5 and citric acid in stoichiometric ratio is heated on a water bath. This gel on decomposition at 600°C yielded the nano crystallites of BaNb2O6, as confirmed by X-ray diffraction study (XRD). This is a much lower temperature as compared to that prepared by traditional solid state method (1000°C) as reported for the formation of BaNb2O6. Transmission electron microscopic (TEM) investigations revealed that the average particle size is 50 nm for the calcined powders. The room temperature dielectric constant at 1 kHz is found to be 1000. The ferroelectric hysteresis loop parameters of these samples were also studied.

• Microstructure and electrical conductivity of Al–SiCp composites produced by spray forming process

Al–SiCp composites have been synthesized by spray forming process with variation in particle flow rate, size of reinforcement particles and their volume fraction. The microstructure of composites and their electrical conductivity have been investigated. The results showed a uniform dispersion of large size particulate phase in the matrix of the primary 𝛼-phase with its equiaxed grain morphology. However, clustering of small size particles was observed at the grain boundary and grain junctions. The grain size of the composite materials was observed to be lower than that of the base Al-alloy. The composite materials invariably indicated their lower electrical conductivity compared to that of the monolithic Al-alloy. The electrical conductivity of composites decreased with increase in the volume fraction and decrease in size of the reinforcement particles. A high flow rate of particles during spray deposition resulted in a decrease in its conductivity. These results are explained in the light of thermal mismatch between the matrix and the reinforcement phases resulting in generation of high dislocation density. The droplet-particle interaction and resulting microstructure evolution during the spray deposition of the composites are discussed.

• Some studies on the reaction between fly ash and lime

The reaction between fly ash (FA) and lime is extensively exploited for the manufacture of building bricks, blocks and aggregates. To get a better idea of this reaction, FA from different sources were mixed in different ratios with lime and compacted. The compacts were treated both by ordinary water and hydrothermal curing to promote lime bearing hydrate bond formation e.g. CaO–SiO2–H2O (C–S–H), CaO–Al2O3–H2O (C–A–H) etc. The decrease in free lime content in these compacts was measured as a function of curing time and curing process. This drop in this content was correlated to the chemical composition of the fly ashes. The mathematical relationships between free lime remaining in the compacts after its maximum decrease in concentration and lime binding modulus (a ratio between the amount of added lime and the total amount of lime binding constituents present in FA) for both types of curing were developed. Further, the rate of decrease in free CaO content under both types of curing conditions was compared from kinetic study. From this study the orders of the reactions and rate constants were found out.

• A comparative study of proton transport properties of metal (IV) tungstates and their organic derivatives

New hybrid inorgano–organic materials were synthesized by anchoring organic moieties, ortho chlorophenol and para chlorophenol onto metal (IV) tungstates viz. tin tungstate (SnW), titanium tungstate (TiW) and zirconium tungstate (ZW) to give SnWoCP, SnWpCP, TiWoCP, TiWpCP, ZWoCP and ZWpCP, respectively. The materials were characterized for elemental analysis, thermal analysis (TGA, DSC), X-ray analysis and FTIR spectroscopy. Chemical resistivity of these materials were assessed in several acidic, basic and organic media. Further, the study of transport properties of these materials has been explored by measuring proton conductivity at different temperatures in the range 30–175°C using HP4192A impedance analyser over a frequency range 5 Hz–13 MHz at a signal level below 1 V. Based on the specific conductance data and Arrhenius plots, a suitable mechanism was proposed and conductance performance of derivatized and nonderivatized materials compared.

• Adsorption and intercalation of anionic surfactants onto layered double hydroxides—XRD study

Layered double hydroxides (LDH) with brucite like structure was modified with various anionic surfactants containing sulfonate, carboxyl, phosphonate and sulfate end group through ion-exchange method. XRD reports indicated that the sulfonate group containing surfactants led to an adsorption process whereas the sulfate, carboxyl and phosphonate group containing surfactant led to an intercalation process. This can be evidenced from the change in basal spacing of LDH. The presence of anionic surfactants in the LDH was supported by FTIR spectroscopy. The FTIR spectrum indicated that complete removal of carbonate anion from the inter layer space of LDH is very difficult. The phosphonate intercalated HT showed less thermal stability than pristine LDH.

• Effect of annealing temperature on the structural–microstructural and electrical characteristics of thallium bearing HTSC films prepared by chemical spray pyrolysis technique

In order to get good quality reproducible films of Tl : HTSC system, we have studied the different annealing conditions to finally achieve the optimized annealing condition. In the present investigation, Tl–Ca–Ba–Cu–O superconducting films have been prepared on YSZ (100) and MgO (100) single crystal substrates via precursor route followed by thallination. The post deposition heat treatments of the precursor films were carried out for various annealing temperatures (870°C, 890°C) and durations (1 and 2 min). The optimized thallination procedure occurred at 870°C for 2 min into good quality films with 𝑇c (𝑅 = 0) ∼ 103 K for YSZ and 𝑇c (𝑅 = 0) ∼ 98 K for MgO substrates, respectively. Further we have correlated the structural/microstructural characteristics of the films.

• Superconductivity and electrical resistivity in alkali metal doped fullerides: Phonon mechanism

We consider a two-peak model for the phonon density of states to investigate the nature of electron pairing mechanism for superconducting state in fullerides. We first study the intercage interactions between the adjacent C60 cages and expansion of lattice due to the intercalation of alkali atoms based on the spring model to estimate phonon frequencies from the dynamical matrix for the intermolecular alkali-C60 phonons. Electronic parameter as repulsive parameter and the attractive coupling strength are obtained within the random phase approximation. Transition temperature, 𝑇c, is obtained in a situation when the free electrons in lowest molecular orbital are coupled with alkali-C60 phonons as 5 K, which is much lower as compared to reported 𝑇c (≈ 20 K). The superconducting pairing is mainly driven by the high frequency intramolecular phonons and their effects enhance it to 22 K. To illustrate the usefulness of the above approach, the carbon isotope exponent and the pressure effect are also estimated. Temperature dependence of electrical resistivity is then analysed within the same model phonon spectrum. It is inferred from the two-peak model for phonon density of states that high frequency intramolecular phonon modes play a major role in pairing mechanism with possibly some contribution from alkali-C60 phonon to describe most of the superconducting and normal state properties of doped fullerides.

• Estimation of CE–CVM energy parameters from miscibility gap data

The powerful framework of cluster expansion–cluster variation methods (CE–CVM) expresses alloy free energy in terms of energy (model) parameters, macroscopic variables (composition and temperature) and microscopic variables (correlation functions). A simultaneous optimization of thermodynamic and phase equilibria data using CE–CVM is critically dependent on giving good initial values of energy parameters, macroscopic and microscopic variables, respectively. No standard method for obtaining the initial values of the energy parameters is available in literature. As a starting point, a method has been devised to estimate the values of energy parameters from consolute point (miscibility gap maximum) data. Empirical relations among energy parameters, temperature (𝑇c), composition (𝑥c) and 𝑑2}𝑇/𝑑𝑥2 at the consolute point, have been developed using CE–CVM free energy functions for bcc and fcc structures in the tetrahedron and tetrahedron–octahedron approximations, respectively. Thus from the observed data of 𝑇c, 𝑥c and 𝑑2}𝑇/𝑑𝑥2 in the above relations, good initial values of energy parameters can be obtained. Further, a necessary modification to the classical NR method for solving simultaneous nonlinear/transcendental equations with a double root in one variable and a simple root in the other has been presented.

• Thermodynamic modelling of phase equilibria in Al–Ga–P–As system

A generalized thermodynamic expression of the liquid Al–Ga–P–As alloys is used in conjunction with the solid solution model in determining the solid–liquid equilibria at 1173 K and 1273 K. The liquid solution model contains thirtyseven parameters. Twentyfour of them pertain to those of the six constituent binaries, twelve refer to the specific ternary interactions. Additionally the liquid solution model also contains a specific quaternary interaction parameter. The latter has been evaluated here based on the experimental data available in the literature. The present research shows an excellent agreement between the derived and experimental values at 1173 K and 1273 K for the system. The article also presents a comparison between the evaluated values with those based on the regular solution model for the liquid alloys.

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