• Volume 32, Issue 5

October 2009,   pages  465-561

• Preparation and characterization of nano-hydroxyapatite powder using sol–gel technique

Hydroxyapatite (HA) nano powders (20–60 nm) were synthesized using a sol–gel route with calcium nitrate and phosphoric acid as calcium and phosphorus precursors, respectively. Double distilled water was used as a diluting media for HA sol preparation and ammonia was used to adjust the pH. After aging, the HA gel was dried at 65°C and calcined to different temperatures ranging from 200–800°C. The dried and calcined powders were characterized for phase composition using X-ray diffractometry, elemental dispersive X-ray and Fourier transform infra-red spectroscopy. The particle size and morphology were studied using transmission electron microscopy. Calcination revealed HA nano powders of increased particle size and crystallinity with increase in temperature. For all calcinations temperatures, the particle size distribution analysis of HA powders showed skewed distribution plot. At temperature of 700°C and above, formation of CaO was noticed which was attributed to phosphorous volatilization. This study showed that high purity HA with varying degrees of crystallinity could be obtained using this simple technique.

• Effect of external energy on atomic, crystalline and powder characteristics of antimony and bismuth powders

Next to atoms and molecules the powders are the smallest state of matter available in high purities and large quantities. The effect of any external energy on the shape, morphology and structure can thus be studied with relative ease. The present investigation deals with the effect of a non-contact external energy on the powders of antimony and bismuth. The characteristics of powders treated by external energy are compared with the as received powders (control). The average particle sizes, 𝑑50 and 𝑑99, the sizes below which 99% of the particles are present showed significant increase and decrease indicating that the energy had caused deformation and fracture as if the powders have been subjected to high energy milling.

To be able to understand the reasons for these changes the powders are characterized by techniques such as X-ray diffraction (XRD), surface area determination (BET), thermal analytical techniques such as DTA–DTG, DSC–TGA and SDTA and scanning electron microscopy (SEM).

The treated powder samples exhibited remarkable changes in the powder characteristics at all structural levels starting from polycrystalline particles, through single crystal to atoms. The external energy had changed the lattice parameters of the unit cell which in turn changed the crystallite size and density. The lattice parameters are then used to compute the weight and effective nuclear charge of the atom which showed significant variation. It is speculated that the external energy is acting on the nucleus through some reversible weak interaction of larger cross section causing changes in the proton to neutron ratios. Thus the effect is felt by all the atoms, and hence the unit cell, single crystal grain and grain boundaries. The stresses generated in turn may have caused deformation or fracture of the weak interfaces such as the crystallite and grain boundaries.

• Nano-tribological characteristics of TiO2 films on 3-mercaptopropyl trimethoxysilane sulfonated self-assembled monolayer

Silane coupling reagent (3-mercaptopropyl trimethoxysilane (MPTS)) was used to prepare twodimensional self-assembled monolayer (SAM) on silicon substrate. The terminal –SH group was in situ oxidized to –SO3H group to endow the film with good chemisorption ability. Then TiO2 thin films were deposited on the oxidized MPTS–SAM to form composite thin films, making use of the chemisorption ability of the –SO3H group. Atomic force microscope (AFM) and contact angle measurements were used to characterize TiO2 films. Adhesive force and friction force of TiO2 thin films and silicon substrate were measured under various applied normal loads and scanning speed of AFM tip. Results showed that the friction force increased with applied normal loads and scanning speed of AFM tip. In order to study the effect of capillary force, tests were performed in various relative humidities. Results showed that the adhesive force of silicon substrate increases with relative humidities and the adhesive force of TiO2 thin films only increases slightly with relative humidity. Research showed that surfaces with more hydrophobic property revealed the lower adhesive and friction forces.

• Characterization and photoluminescence studies of CdTe nanoparticles before and after transfer from liquid phase to polystyrene

The major objective of this work was to detect the change of photoluminescence (PL) intensity of CdTe nanoparticles (NPs) before and after transfer from liquid phase to polystyrene (PS) matrix by electrospinning technique. Thio-stabilized CdTe NPs were first synthesized in aqueous, then enwrapped by cetyltrimethylammonium bromide (CTAB), and finally, transferred into PS matrix to form CdTe/PS nanofibres by electrospinning. Then, CdTe/PS nanofibres were characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM) to observe their morphology and distribution, respectively. The selective area electronic diffraction (SAED) pattern proved that the CdTe NPs were cubic lattice. The PL spectrum indicated that CdTe NPs have been transferred into PS nanofibres, and the PL intensity of CdTe NPs in the nanofibres was even higher than that before CdTe NPs were introduced into PS nanofibres. Moreover, X-ray photoelectron spectra (XPS) revealed that thiol-stabilized CdTe NPs were enwrapped by CTAB, and PS acted as a dispersant in the process of electrospinning.

• Catalytic synthesis of ZnO nanorods on patterned silicon wafer—An optimum material for gas sensor

ZnO nanorods have been synthesized over etch-patterned Si (110) wafer using annealed silver thin film as growth catalyst. The growth of ZnO nanorods were performed by a two-step process. Initially, the deposition of Zn thin film was done on the annealed silver catalyst film over etch-patterned Si (110) substrate by thermal evaporation, and then annealed at 800°C in air. The etching of the patterned Si (110) wafers was carried out by 50% aqueous KOH solution. The samples were investigated by optical microscopy, scanning electron microscopy, X-ray diffraction, Raman spectroscopy and room temperature photoluminescence spectroscopy. V’ shaped grooves with no undercut were formed after etching due to the anisotropic nature of the KOH etchant. The etch-patterned wafer was used to provide larger surface area for ZnO growth by forming V’-grooves. This ZnO film may be predicted as a very good material for gas sensor.

• Role of particle size in visible light photocatalysis of Congo Red using TiO2.[ZnFe2O4]𝑥 nanocomposites

TiO2.[ZnFe2O4]𝑥 (𝑥 = 0.0–0.5) nanocomposites (NCs) with an average particle size of 72.4 nm were synthesized by the method of co-precipitation/hydrolysis (CPH). For the comparison of particle-size dependent effects, a set of polycrystalline samples with similar compositions was also prepared by solid state reaction (SSR) route. Average particle size for SSR prepared samples was about 3.0 𝜇m. All the samples were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), particle size analyzer, Raman spectroscopy and Fourier transform infra-red (FTIR) spectroscopy. Their visible light photocatalytic activity was tested for the degradation of Congo Red dye. Maximum photodegradation was observed for the NC with 𝑥 = 0.1 synthesized by CPH (particle size, 71 nm). Similar composition prepared by SSR method (particle size, 6.19 𝜇m) showed lower photoactivity in comparison even with that observed for pure TiO2 (particle size, 4.03 𝜇m). It was, therefore, concluded that enhanced photodegradation is directly related to the reduced particle size of the composites, which implies that photosensitization is the process primarily involved. Although, doping of TiO2 with ZnFe2O4 does extend the cut-off wavelength towards visible parts of the spectrum, its contribution in the enhancement is not as significant as that due to the photosensitization.

• Functionalization of hydroxyl terminated polybutadiene with biologically active fluorescent molecule

A biologically active molecule, 2-chloro-4,6-bis(dimethylamino)-1,3,5-triazine (CBDT), has been covalently attached at the terminal carbon atoms of the hydroxyl terminated polybutadiene (HTPB) backbone. The modification of HTPB backbone by CBDT molecule does not affect the unique physico-chemical properties such as fluidity, hydroxyl value and microstructure of the parent HTPB. The formation of hydrogen bonding between the terminal hydroxyl groups and the nitrogen atoms of triazine moiety is the driving force for the terminal attachment chemistry. The functionalized HTPB (HTPB–CBDT) shows a strong fluorescence emission at 385 nm.

• Photoluminescence and Raman studies in swift heavy ion irradiated polycrystalline aluminum oxide

Polycrystalline aluminum oxide is synthesized by combustion technique and XRD studies of the sample revealed the 𝛼-phase. The synthesized sample is irradiated with 120 MeV swift Au9+ ions for the fluence in the range from 1 × 1011 to 1 × 1013 ions cm-2. A broad photoluminescence (PL) emission with peak at ∼447 nm and two sharp emissions with peak at ∼ 679 and ∼ 695 nm are observed in pristine when sample was excited with 326 nm. However, in the irradiated samples the PL intensity at ∼ 447, 679 and 695 nm decreases with increase in ion fluence. The 𝛼-Al2O3 gives rise to seven Raman modes with Raman intensity with peaks at ∼ 253, 396, 417, 546, 630, 842, 867 cm-1 observed in pristine. The intensity of these modes decreases with increase in ion fluence. However, the Raman modes observed at lower fluences are found to disappear at higher fluence.

• Preparation of dual-sensitive graft copolymer hydrogel based on N-maleoyl-chitosan and poly(N-isopropylacrylamide) by electron beam radiation

Organic solvent-soluble N-maleoyl-chitosan (NMCS) was synthesized by reaction of chitosan with maleic anhydride (MAH) in N,N-dimethylformamide (DMF). N-maleoyl-chitosan-graft-poly(N-isopropylacrylamide) (NMCS-g-PNIPAAm) copolymer hydrogel was prepared via free radical polymerization by electron beam (EB) irradiation. The copolymer obtained was analysed by FT–IR, XRD and thermal gravimetric analysis (TGA). It was found that the grafting yield and grafting efficiency increased with increasing radiation absorbed dose and monomer amount, and then decreased. The swelling ratio of the copolymer hydrogel was low at pH 4–5, and LCST of the hydrogel was around 32°C.

• Kinetics of crystallization of a Fe-based multicomponent amorphous alloy

The Fe-based multicomponent amorphous alloys (also referred to as metallic glasses) are known to exhibit soft magnetic properties and, it makes them important for many technological applications. However, metallic glasses are in a thermodynamically metastable state and in case of high temperature operating conditions, the thermally activated crystallization would be detrimental to their magnetic properties. The study of crystallization kinetics of metallic glasses gives useful insight about its thermal stability. In the present work, crystallization study of Fe67Co18B14Si1 (2605CO) metallic glass has been carried out using differential scanning calorimetry (DSC) technique. Mössbauer study has also been undertaken to know the phases formed during the crystallization process. The alloy shows two-stage crystallization. The activation energy has been derived using the Kissinger method. It is found to be equal to 220 kJ/mol and 349 kJ/mol for the first and second crystallization peaks, respectively. The Mössbauer study indicates the formation of 𝛼-(Fe, Co) and (Fe, Co)3B phases in the alloy.

• Effect of cerium and thermomechanical processing on microstructure and mechanical properties of Fe–10.5Al–0.8C alloy

The effect of cerium content and thermomechanical processing on structure and properties of Fe–10.5 wt.%Al–0.8 wt%C alloy has been investigated. Alloys were prepared by a combination of air induction melting with flux cover (AIMFC) and electroslag remelting (ESR). The ESR ingots were hot-forged and hotrolled at 1373 K as well as warm-rolled at 923 K and heat-treated. Hot-rolled, warm-rolled and heat treated alloys were examined using optical microscopy, scanning electron microscopy (SEM) and X-ray diffraction to understand the microstructure of these alloys. The ternary, Fe–10.5 wt.%Al–0.8 wt.%C alloy showed the presence of two phases; Fe–Al with bcc structure, and large volume fraction of Fe3AlC0.5 precipitates. Addition of cerium to Fe–10.5 wt.%Al–0.8 wt.%C alloy resulted in three phases, the additional phase being small volume fraction of fine cerium oxy-carbide precipitates. Improvement in tensile elongation from 3–6.4% was achieved by increasing the cerium content from 0.01–0.2 wt.% and further improvement in tensile elongation from 6.4–10% was achieved by warm-rolling and heat treatment.

• Silicalite-1 zeolite membranes on unmodified and modified surfaces of ceramic supports: A comparative study

Silicalite-1 zeolite membranes were prepared hydrothermally on the porous ceramic supports, both unmodified and modified with 3-aminopropyl triethoxysilane (APTES) as a coupling agent following ex situ (secondary) crystal growth process. The microstructure of the membranes was examined by scanning electron microscopy (SEM). The permeation study with a single gas, nitrogen (N2) was performed through the membranes. For the surface modified support, a more surface coverage of the seed crystals on the porous support was observed resulting in a relatively higher dense packing of the crystals during secondary crystal growth process compared to that obtained from the unmodified support. The membrane developed on surface modified support rendered lower permeance value i.e. 9 × 10-7 mol m-2 s-1 Pa-1 of N2 compared to that formed on the unmodified support which gave permeance value of 20 × 10-7 mol m-2 s-1 Pa-1 of N2.

• Preparation of copper and silicon/copper powders by a gas evaporation-condensation method

Pure and silicon-coated metal copper nano to submicron-sized powders were prepared by gas evaporation and condensation. This powder was synthesized by using an industrial electron accelerator, ELV-6, with Ar as the carrier gas. Vapour from the liquefied metal surface was transferred to the cold zone by the carrier gas and precipitated as spherical Cu metal and Si/Cu composite powders. The mean diameter of the resulting powder was 100–200 nm.

• High-temperature oxidation behaviour of Ti3Si(1–𝑥)Al𝑥C2 in air

The oxidation behaviours of bulk Ti3Si(1–𝑥)Al𝑥C2 prepared by hot pressing were investigated. The results showed that the isothermal oxidation behaviour of Ti3SiC2 obeyed a parabolic law between 900 and 1100°C, and followed a two-step parabolic rate law between 1200°C and 1300°C. The cyclic oxidation behaviour of material is assumed to obey a three-step parabolic rate law at 1100°C and 1200°C. The calculated activation energy of isothermal oxidation is 101.43 kJ.mol-1. The oxide layers consisted of a mass of 𝛼-Al2O3 and little TiO2 and SiO2 are observed on Ti3SiC2 as a dense and adhesive protect scale. The oxidation mechanism varies with the additive aluminum that greatly improves the oxidation resistance of Ti3SiC2.

• Electrochemical and SEM properties of Co2+ ion in hexagonal mesophase of pluronic lyotropic liquid crystal template

The electrochemical and SEM properties of Co2+ ion in hexagonal mesophase of the pluronic lyotropic liquid crystal template are reported. The cyclic voltammetric studies evidenced the occurrence of two slow electron transfer reduction processes. Such a reaction presumably related to the reduction of Co2+ ion to Co metal. The hexagonal (H1) lyotropic liquid crystalline phases of P84 surfactant have been used to template the electrochemical deposition of nanostructured cobalt films as well as its uses as background electrolyte. Electrochemical studies show that these films have very high surface areas, which reveals that the deposited film exhibits promising properties. The electrode parameters of Co(II) ion in hexagonal meso phase of the lyotropic liquid crystal ternary system (pluronic P84/cobalt/𝑝-xylene) is determined using cyclic voltammetry, deduced convolutive voltammetry and chronoamperometry techniques. The morphology of nanostructured deposited films of Co2+ ion in pluronic lyotropic liquid crystal template was investigated via scanning electron microscopy (SEM) technique.

• Influence of seeding on crystallization behaviour of BaNaB9O15 glasses

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