Kausik Dana

Evolution of microstructure in flyash-containing porcelain body on heating at different temperatures

Abstract15 wt% flyash (a calcined byproduct of thermal power plant) was incorporated in a normal triaxial kaolin-quartz-feldspar system by replacing equivalent amount of quartz. The differences in microstructural evolution on heating the compact mass of both normal and flyash-containing porcelain at different temperatures (1150–1300°C) were examined using scanning electron microscopy (SEM) operating in secondary electron image (SEI) mode. Microstructure of normal porcelain did not show the presence of mullite and quartz grains at 1200°C and the viscosity of silica-rich glass restricted the growth of mullite crystals at 1250°C. Flyash porcelain, on the other hand, shows the presence of primary mullite aggregates in the clay relict and a significant growth of mullite crystals in a low viscosity glassy matrix at 1200°C itself. At 1300°C, both the bodies show a larger region of more elongated (> 1 μm) secondary mullite along with clusters of smaller sized primary mullite (< 1 μm). Small primary mullite crystals in the clay relict can be distinguished from elongated secondary mullite crystals in the feldspar relict in their size. Primary mullite aggregates remain stable also at higher temperatures. XRD studies were carried out for quantitative estimation of quartz, mullite and glass, which supported the SEM observations. An attempt was also made to correlate their mechanical strength with the constituent phases.

Immobilization of poly(fluorene) within clay nanocomposite: an easy way to control keto defect.

Blue light emitting cationic polyfluorene polymer(PF)/montmorillonite (MMT) nanocomposites were prepared by solution intercalation and exfoliation method to evaluate the effect of MMT on the nanocomposite structures, properties and morphologies. The properties of PF-MMT composites, containing 1-50 mass% MMT, were characterized unambiguously with the help of multiple analytical techniques, with focus on the keto defect and photostability of PF in the nanocomposites. XRD and HRTEM studies reveal both exfoliation of MMT galleries at lower content of MMT in composites and intercalation of PF chains into the MMT galleries at higher MMT content. The nanocomposites show higher thermal stability than pristine PF as anchorage of nanoclay in PF matrix occur through the electrostatic interaction between nanoclay and polymer. The decrease in Si-O-Si stretching frequency during exfoliation is much higher than in intercalation, as Si-O-Si experience lesser hindrance to vibrate in exfoliated MMT galleries. The gradual redshift of π-π(*) transition peak of PF with increasing MMT content in composites confirms the uncoiling of PF in clay galleries. The photoluminescence characteristics reveal interruption of interchain interaction in this intercalated and exfoliated organic/inorganic hybrid system, which reduces the low-energy emission that results from keto defect. Due to very high aspect ratio of MMT, it can act as an efficient exciton blocking layer and a barrier to oxygen diffusion, which may lead to a device with high color purity and enhanced photostability. Again current-voltage characteristics of nanocomposite films confirm the retention of LED properties after nanocomposite formation.

Organophilic Nano Clay: A Comprehensive Review

Organophilic nano clay is an important organic-inorganic hybrid derived from intelligent combination of two dissimilar components, viz. clays and organic molecules, at the nanometric and molecular level. The clay component of this hybrid provides a 2-D lamellar structure with interesting surface chemistry, which can be engineered by organic molecules. 2:1 layered clay minerals with high cation exchange capacity, e.g. montmorillonite, possess cation exchange sites on the siloxane surface which can be exchanged with suitable organic molecules. Key aspect of this organic treatment is to swell the interlayer space of the clay mineral up to a certain extent reducing interlayer interaction, to produce nanoplatelet of aluminosilicate materials. Those engineered nanoplatelets are used in various fields of applications, viz. polymer nano clay composite, rheological modifier, thickening and gelling agent in paints and lubricants, in waste water treatment, and also as drug delivery vehicle. Intensive research activity in this complex system is attested by evergrowing number of symposia, books and specialized journals devoted to this subject. This present article is an updated review of organophilic nano clay preparation, characterization and application of the material. Important information available in the protected domain of patent is also included.

Bone cement based nanohybrid as a super biomaterial for bone healing

A novel nanohybrid based on bone cement has been developed which is capable of healing fractured bone in 30 days, one-third of the time required for the natural healing process. Nanohybrids of bone cement based on poly(methyl methacrylate) (PMMA), currently used as a grouting material in joint replacement surgery, were prepared by simple mixing with organically modified layered silicates of varying chemical compositions. The temperature arising from exothermic polymerization in one of the nanohybrids is 12 °C lower than that in pure bone cement, thus circumventing the reported cell necrosis that occurs during implantation with pure bone cement. The thermal stability and mechanical superiority of this nanohybrid were verified in terms of its higher degradation temperature, better stiffness, superior toughness, and significantly higher fatigue resistance compared with pure bone cement; these properties make it appropriate for use as an implant material. The biocompatibility and bioactivity of the nanohybrid were confirmed using cell adhesion, cell viability, and fluorescence imaging studies. Osteoconductivity and bone bonding properties were monitored in vivo in rabbits through radiographic imaging and histopathological studies of growing bone and muscle near the surgery site. The observed dissimilarity of the properties of two different nanoclays used as fillers were visualized through interactions measured using spectroscopic techniques. Studies of the influence of different elements on bioactivity showed a higher efficiency for the nanoclay containing greater amounts of iron.

Refractories of alumina-silica system

The inorganic phases belonging to the binary alumina-silica system exhibit a plethora of excellent high temperature properties that make them useful for refractory applications. Synthesized from abundant aluminosilicate minerals, these refractories are ubiquitous in high temperature industrial applications. The refractories of alumina-silica system can be engineered to generate a range of high temperature properties by varying the Al2O3/SiO2 ratio, presence of other oxides and texture. This versatility is unique to this system and is reflected in widely varied fields of applications of these refractories. Composed predominantly of mullite and corundum phases, the non crystalline phases also play important role in determining the property and end use of these refractories. This review covers different theoretical and practical aspects of refractories of aluminosilicate system spanning 30-100% alumina. Important role of microstructure in aluminosilicate refractory has been discussed in light of phase diagram, raw materials and thermo-chemical reactions. The applications of these refractories in different areas have been discussed in detail with structure-property correlation.

Some studies on ceramic body compositions for wall and floor tiles

Three ceramic tile body compositions have been studied using indigenously available natural minerals and industrial solid wastes as raw materials. The physicochemical properties of all the specimens produced under laboratory conditions were compared. It has been observed that elimination of crystalline silica, introduction of alkaline earth oxides in the form of waste materials and precalcined phases promoted sintering and enhanced the fired strength considerably. The results of water absorption, fired shrinkage, coefficient of thermal expansion, hardness, flexural strength and SEM studies indicate the suitability of such compositions for wall and floor tile applications. The surface gain due to lower shrinkage in one of the experimental composition has been calculated and compared with that of a commercial composition.

Studies on the Suitability of Iron-rich Indian Bentonites for Synthesis of Organoclays by Intercalation

In the present study intercalation behaviour of two bentonites from Indian origin were compared with a high-puritycommercial montmorillonite. Experimental bentonites of Indian origin showed low cation exchange capacity (CEC) due to limited Mg2+ substitution. Infra-red spectral study revealed the presence of Fe3+ in octahedral positions. Organic loading of intercalated clays increased with CEC.

SIMULTANEOUS INTERCALATION OF TWO QUATERNARY PHOSPHONIUM SALTS INTO MONTMORILLONITE

Intercalation of montmorillonites with a mixture of intercalates has not been studied extensively. The objective of the present investigation was to study the effects of phosphonium-based intercalate mixtures on the properties (organic loading and basal spacing) of montmorillonite. These phosphonium-intercalated montmorillonites are promising candidates as high-temperature stable nanofillers for application in clay polymer nanocomposites.Two salts with different cationic heads and chain lengths were mixed in varying molar ratios and the mixtures were intercalated into the interlayer space of montmorillonite. Two sets were chosen based on the chain length and the cationic head-group structure of the two intercalated salts (referred to hereafter as set 1 and set 2). The resultant intercalated montmorillonite was characterized by thermogravimetric analysis, X-ray diffraction, and transmission electron microscopy. The organic loading of the intercalated montmorillonite increased with the proportion of longer carbon-chain intercalate in the mixture. The intensity of the characteristic XRD peak of each intercalate varied with the mole fraction percent of that intercalate in the solution mixture. No marked synergistic effect of the intercalate mixture on the basal spacing and organic loading properties of the intercalated montmorillonite was observed — the proportional influence of individual components was found to be more prominent.

Non-Isothermal Kinetic Evaluation of Pyrophyllite Dehydroxylation

Dehydroxylation of clay minerals is an important process with several applications. Despite the industrial use of several well defined clay minerals, only the dehydroxylation kinetics of kaolinite has been reported. Still, the kinetics of these solid state reactions is yet to be understood using unambiguous model. In the present work, we have performed detailed kinetic analysis of dehydroxylation of pyrophyllite clay using non-isothermal kinetics by thermogravimetry (TG) at different heating rates. The TG data has been analysed initially with model-free methods (ASTM E 698, ASTM 1641, Friedman analysis and Ozawa-Flynn-Wall method). Interestingly, both the model-free methods of analysis have unequivocally indicated that activation energy (Eact) changes very marginally with progress of reaction and a single activation energy barrier is present. This surmises that the dehydroxylation process is a single stage process. A multivariate non-linear regression on the dynamic thermal data at different heating rates has been performed to determine the most probable kinetic model based on statistical fit. It has been found that, TG data provides best fit with regression coefficient (r2) value of 0.994, when a single stage Avrami type diffusion reaction model is assumed, and an activation energy of 159 kJ.mol−1.

Development of LTA zeolite membrane from clay by sonication assisted method at room temperature for H 2 -CO 2 and CO 2 -CH 4 separation

In this work, sodium aluminosilicate zeolite powder and membranes were synthesized by ultrasonic irradiation at room temperature using montmorillonite clay as precursor material. For comparison, same zeolite powder and membranes were synthesized at 100 °C also. The synthesized zeolites were characterized by X-ray diffraction (XRD), infrared (IR) spectral analysis, and field-emission scanning electron microscopy (FESEM). XRD and IR results showed that phase pure mainly LTA phase was formed after 15 days of aging at room temperature. By using the zeolite powders as seeds, membranes were synthesized on clay alumina support tubes at room temperature and also at 100 °C. In both the cases membranes were formed on support surface. The membrane thickness was found to be 15 μm. The performances of the membranes were evaluated by single gas as well as mixture gas permeation measurement for H2-CO2 and CO2-CH4 respectively. The H2-CO2 and CO2-CH4 separation selectivity for the mixture gas of the membrane was found to 16.2 and 20.9 at room temperature respectively. To the best of our knowledge, there is no report of synthesis of zeolite membrane at room temperature using clay as raw materials. For the first time we have reported the synthesis of alumino-silicate zeolite membrane on clay alumina support surface using clay as starting material by sonochemical method at room temperature.