The synthesis of high coercivity cobalt-in-carbon nanotube hybrid structures and their optical limiting properties

Magnetic heterostructures with carbon nanotubes having multiple functionalities are fascinating materials which can be manipulated by means of an external magnetic field. In this paper we report our investigations on the synthesis and optical limiting properties of pristine cobalt nanotubes and high coercivity cobalt-in-carbon nanotubes (a new nanosystem where carbon nanotubes are filled with cobalt nanotubes). A general mobility assisted growth mechanism for the formation of one-dimensional nanostructures inside nanopores is verified in the case of carbon nanotubes. The open-aperture z-scan technique is employed for the optical limiting measurements in which nanosecond laser pulses at 532 nm have been used for optical excitation. Compared to the benchmark pristine carbon nanotubes these materials show an enhanced nonlinear optical absorption, and the nonlinear optical parameters calculated from the data show that these materials are efficient optical limiters. To the best of our knowledge this is the first report where the optical limiting properties of metal nanotubes are compared to those of carbon nanotubes

On the synthesis and magnetic properties of multiwall carbon nanotube– superparamagnetic iron oxide nanoparticle nanocomposites

Multiwall carbon nanotubes (MWCNTs) possessing an average inner diameter of 150 nm were synthesized by template assisted chemical vapor deposition over an alumina template. Aqueous ferrofluid based on superparamagnetic iron oxide nanoparticles (SPIONs) was prepared by a controlled co-precipitation technique, and this ferrofluid was used to fill the MWCNTs by nanocapillarity. The filling of nanotubes with iron oxide nanoparticles was confirmed by electron microscopy. Selected area electron diffraction indicated the presence of iron oxide and graphitic carbon from MWCNTs. The magnetic phase transition during cooling of the MWCNT–SPION composite was investigated by low temperature magnetization studies and zero field cooled (ZFC) and field cooled experiments. The ZFC curve exhibited a blocking at ∼110 K. A peculiar ferromagnetic ordering exhibited by the MWCNT–SPION composite above room temperature is because of the ferromagnetic interaction emanating from the clustering of superparamagnetic particles in the constrained volume of an MWCNT. This kind of MWCNT–SPION composite can be envisaged as a good agent for various biomedical applications

Synthesis of High Coercivity Cobalt Nanotubes with Acetate Precursors and Elucidation of the Mechanism of Growth

Cobalt nanotubes (CoNTs) with very high longitudinal coercivity were prepared by electrodeposition of cobalt acetate for the first time by using anodized alumina (AAO) template. They were then characterized with X-ray diffraction (XRD), a field emission scanning electron microscope (FESEM), and a transmission electron microscope (TEM). Formation of a highly ordered hexagonal cobalt phase is observed. Room temperature SQUID (superconducting quantum interference device) magnetometer measurements indicate that the easy axis of magnetization is parallel to the nanotube axis. These CoNTs exhibit very high longitudinal coercivity of ∼820 Oe. A very high intertubular interaction resulting from magnetostatic dipolar interaction between nanotubes is observed. Thick-walled nanotubes were also fabricated by using cobalt acetate tetrahydrate precursors. A plausible mechanism for the formation of CoNTs based on mobility assisted growth is proposed. The role of the hydration layer and the mobility of metal ions are elucidated in the case of the growth mechanism of one-dimensional geometry

Development of functionalised multiwalled carbon nanotube/polyaniline composites for electrical applications

Combining intrinsically conducting polymers with carbon nanotubes (CNT) helps in creating composites with superior electrical and thermal characteristics. These composites are capable of replacing metals and semiconductors as they possess unique combination of electrical conductivity, flexibility, stretchability, softness and bio-compatibility. Their potential for use in various organic devices such as super capacitors, printable conductors, optoelectronic devices, sensors, actuators, electrochemical devices, electromagnetic interference shielding, field effect transistors, LEDs, thermoelectrics etc. makes them excellent substitutes for present day semiconductors.However, many of these potential applications have not been fully exploited because of various open–ended challenges. Composites meant for use in organic devices require highly stable conductivity for the longevity of the devices. CNT when incorporated at specific proportions, and with special methods contributes quite positively to this end.The increasing demand for energy and depleting fossil fuel reserves has broadened the scope for research into alternative energy sources. A unique and efficient method for harnessing energy is thermoelectric energy conversion method. Here, heat is converted directly into electricity using a class of materials known as thermoelectric materials. Though polymers have low electrical conductivity and thermo power, their low thermal conductivity favours use as a thermoelectric material. The thermally disconnected, but electrically connected carrier pathways in CNT/Polymer composites can satisfy the so-called “phonon-glass/electron-crystal” property required for thermoelectric materials. Strain sensing is commonly used for monitoring in engineering, medicine, space or ocean research. Polymeric composites are ideal candidates for the manufacture of strain sensors. Conducting elastomeric composites containing CNT are widely used for this application. These CNT/Polymer composites offer resistance change over a large strain range due to the low Young‟s modulus and higher elasticity. They are also capable of covering surfaces with arbitrary curvatures.Due to the high operating frequency and bandwidth of electronic equipments electromagnetic interference (EMI) has attained the tag of an „environmental pollutant‟, affecting other electronic devices as well as living organisms. Among the EMI shielding materials, polymer composites based on carbon nanotubes show great promise. High strength and stiffness, extremely high aspect ratio, and good electrical conductivity of CNT make it a filler of choice for shielding applications. A method for better dispersion, orientation and connectivity of the CNT in polymer matrix is required to enhance conductivity and EMI shielding. This thesis presents a detailed study on the synthesis of functionalised multiwalled carbon nanotube/polyaniline composites and their application in electronic devices. The major areas focused include DC conductivity retention at high temperature, thermoelectric, strain sensing and electromagnetic interference shielding properties, thermogravimetric, dynamic mechanical and tensile analysis in addition to structural and morphological studies.

Zeolite Encapsulated Complexes Of Fe,Co,Ni,Cu And Pd:Synthesis , Characterization And Catalysis-2003

This thesis deals with the synthesis, characterization and catalysis activity studies of some zeolite encapsulated complexes. Encapsulation inside the zeolite cages makes the catalysts more stable. Further, the framework prevents the complexes from dimerising. Catalysis by metal complexes encapsulated in the cavities of zeolites and other molecular sieves has many features of homogeneous, heterogenous and enzymatic catalysis. Serious attempts has been made to gain product selectivity in catalysis .The catalytic activity shown by the encapsulated complexes can be correlated to the structure of the active site inside the zeolite pore. It deals with the studies on the partial oxidation of benzyl alcohol to benzaldehyde. The oxidatio was carried out using hydrogen peroxide as oxidant in presence of PdYDMG and CuYSPP as catalysts. The product (benzaldehyde) was detected using TLC and confirmed using GC.The catalytic activity of the complexes was tested for oxidation under various conditions. The operating conditions like the amount of the catalyst, reaction time, oxidant to substrate ratio, reaction temprature, and solvents have been optimized. No further oxidation products were obtained on continuing the reaction for four hours beyond the optimum time. Maximum conversion was obtained at room temperature and the percentage conversion decreased with increase in temperature. Activity was found to be dependent on the solvent used. With increasing awareness about the dangers of environmental degradation, research in chemistry is getting increasing geared to the development of “green chemistry,” by designing environmentally friendly products and processes that bring down the generation and use of hazardous substances.

Studies on the Synthesis and Transformations of A Few Dibenzoylalkene – Type Systems

The aim of the study is to synthesise several dibenzoylakene-type systems such as acenaphthenone-2-ylidene ketones 47 and phenanthrenone-9-ylidene ketones 48 by the condensation reaction of acenaphthenequinone and phenanthrenequinone with methyl ketones. Here studies the thermal and photochemical transformations of acenaphthaenone-2-ylidene ketones 3a-c.These acenaphthenone –2-ylidene ketones underwent extensive decomposition on heating. The objectives of present study is to synthesise acenaphthenone-2-ylidene ketones by the Claisen-Schmidt condensation of acenaphthenequinone and methyl ketones, it is to synthesise phenanthrenone –9-ylidene ketones by the Claisen-Schmidt condensation of phenanthrequinone and methyl ketones, thermal studies on acenaphthenone-2-ylidene ketones and phenanthrenone-9-ylidene ketones, photochemical studies on acenaphthenone-2-ylidene ketones and phenanthrenone –9-ylidene ketones to establish the generality of dibenzoyalkene rearrangement. Cyclic voltammetric studies on these dibezoyalkenes to compare their redox behaviour with that of the cis and trans isomers of dibenzoyl-ethylene, dibenzoylstilbene. These results should provide some information about their reactivity, and to assess and exploit the potential of these systems as quinonemethides. This study conclude that a number of new dibenzolalkene-type systems have been synthesized by the Claisen-Schmidt condensation of 1,2-diketones such as phenanthequinone and acenaphthenequinone with methyl ketones. Some of these compounds have been shown to undergo interesting photochemical transformations. Based on the results it is conclude that phenanthjrenone-9-ylidene ketones are excellent Michael acceptors. Methanol adds to these to yield the corresponding furanols. These furanols are unstable and are slowly converted to phenanthro-2 (3H)-furanones.

Synthesis and Characterization Of Some Transition Metal Complexes Of Multidentate Ligands

Coordination chemistry of schiff bases is of considerable interest due to their various magnetic, catalytic and biological applications. Here it describes the spectral characterization of schiff bases and its Mn (II), Cu (II) and Ni (II) complexes. Then synthesis and spectral characterization of Zn (II), Cd (II) and Co (II) complexes of schiff base derived from 3-Formylsalicilic Acid and 1,3-diaminopropane. Then it discusses the synthesis and spectral studies of Copper (II) complexes of 2-Hydroxyacetophenone N-phenyl semicarbazone. Finally it discusses the synthesis and spectral characterization of Co (III) complexes of salicylaldehyde N-phenyl semicarbazone. The preparation and characterization of Cobalt (III) complexes of salicylaldehyde, N-phenylthiosemicarbazone containing hetrocyclic bases phenalthroline and bipyridine. Thiocyanate, azide and perchlorate ions act as coligands. Elemental analysis suggests +3 state for Cobalt. HNMR, IR and UV-visible spectra characterize the complexes.

Synthesis, Spectral Characterization, Structural Studies and Biological Investigations of Transition Metal Complexes of Some Acid Hydrazones

This study concentrates the chemical properties of hydrazones due to its chelating capability and their pharmacological applications. Studies cover the preparation of different acid hydrazones and their structural studies and studies on their antimicrobial activity, synthesis and spectral characterization of different complexes of copper oxovanadium, manganese, nickel etc. Effect of incorporation of heterocyclic bases to the coordination sphere, change in the biological activity of acid hydrazones upon coordination, development of X-ray quality single crystals and its X-ray diffraction studies, studies on the redox behavior of the coordinated metal ions and correlation between the stereochemistry and biological activities.

Studies on the Synthesis and Transformations of a Few 2(3H)- and 3(2H)-Furanones

The thesis entitled studies on the synthesis and transformations of a few 2(3H)- and 3(2H)- furanones. Furanones represent an interesting class of heterocyclic compounds, which constitute the central ring system of many natural products. The derivatives of furan is divided, depending on their structure 2(3H)-furanones(I), 2(5H)-furanones(II), and 3(2H)-furanones(III). Systems I&II are unsatured gama lactones known as ‘butenolides’. Compounds of this type also known as ‘crotonolactones’ based on the parent crotonic acid. In conclusion a number of 2(3H)-and 3(2H)- furanones were synthesized from dibenzoylalkene precursors and were characterized on the basis of spectral analytical and X-ray data. On direct irradiation 3,3-bis(4-chloropheneyl)-5-aryl-3H-furan -2-ones underwent decarbonylation to yield the corresponding alpha, beta- unsaturated carbonyl compounds and upon sensitized irradiation they underwent dimersation arising through a 2+2 cycloaddition reaction. Our studies on 3(2H)-furanones revealed that these compounds are thermally stable, while they undergo extensive decomposition to intractable mixtures under the influence of light. Similarly, the novel dibenzoylalkenes- type systems containing hetroatomatic rings synthesized by us also underwent extensive decomposition under the influence of heat. Some of the 3(2H)-furanones synthesized by us exhibit remarkable anti-proliferative activity.

Kinetic Parameters of Thymidine Kinase and DNA Synthesis During Liver Regeneration: Role Ofthyroid Hormones

The role of thyroid hormones in DNA synthesis and in the activity of Thymidille kinase (TK), a key regulatory enzyme of DNA synthesis was studied in proliferating hepatocytes in vivo. Liver regeneration after partial hepatectomy was used as a model for controlled cell division in rats having different thyroid status - euthyroid, hypothyroid and 3,3',5'-triiodo-L-thyronine (T))-heated hypothyroid. Partial hepatectomy caused a significant elevation of DNA synthesis (p<0.01) in all the three groups compared to their sham-operated counterparts. Hypothyroid liepatectomised animals showed significantly lower (p<0.01) level of DNA synthesis than euthyroid hepatectomised animals. A single subcutaneous close of 1'3 to hypothyroid shamoperated animals resulted in a significant increase (p<0.01) of DNA synthesis in the intact liver. 17tis was comparable to the level of DNA synthesis occurring in regenerating liver of euthyroid animals. In hypothyroid hepatectomised animals, "1'3 showed an additive effect on l)NA synthesis and this group exhibited maximum level of DNA synthesis (p<0.0I ). Studies of the kinetic parameters of TK show that the Michelis-Menten constant, (K111) of TK for thymidine was altered by the thyroid status. K11 increased significantly (p<0.01) in untreated hypothyroid animals when compared to the euthyroid rats. '13 treatment of hypothyroid animals reversed this effect and this group showed the lowest value for K111 (p<0.01). Thus our results indicate that thyroid hormones can influence DNA synthesis during liver regeneration and they may regulate the activity of enzymes such as 17rymidine kinase which are important for DNA synthesis and hence cell division.

Effect Insulin on DNA Synthesis and Kinetic Parameters of Thymidine Kinase During Liver Regenaration

The effect of insulin on cell proliferation in vivo has been studied in hepatectomised streptozotocin- diabetic rats. The extent of cell proliferation in sham and hepatectomized- control, diabetic and insulin treated rats were monitored by determining DNA content and [3H]thymidine incorporation into DNA. The kinetic parameters of thymidine kinase a regulatory enzyme for DNA synthesis was also studied in these groups. The rate of DNA synthesis in liver of streptozotocin -diabetic rats was significantly higher 24 hrs post-hepatectomy compared to control and insulin treated diabetic groups. Kinetic studies of thymidine kinase revealed that there was no change in the Michaelis -Menten constant (Km) whereas maximum velocity (Vmax) was elevated in the diabetic hepatectomized groups compared to control and insulin treated hepatectomized groups. Thus our study elucidates the role of insulin in thymidine kinase activity and DNA synthesis.

Ship-in-a-bottle synthesis of 2,4,6-triphenylthiapyrylium cations encapsulated in zeolites Y and beta: a novel robust photocatalyst

The 2,4,6-triphenylthiapyrylium ion has been obtained imprisoned inside the supercages of the tridirectional, large pore zeolites Y and beta via ship-in-a-bottle synthesis from chalcone and acetophenone in the presence of hydrogen sulfide. The resulting solids are efficient and robust photocatalysts that are able to degrade phenol and aniline in water with a higher efficiency than the P-25 TiO2 standard. Preliminary tests have shown that these encapsulated dye materials are also efficient photocatalysts for the oxidative degradation of malodorous sulfurcontaining molecules.

Synthesis of ZnO nanoparticles by hydrothermal method

Stable, OH free zinc oxide (ZnO) nanoparticles were synthesized by hydrothermal method by varying the growth temperature and concentration of the precursors. The formation of ZnO nanoparticles were confirmed by x-ray diffraction (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) studies. The average particle size have been found to be about 7-24 nm and the compositional analysis is done with inductively coupled plasma atomic emission spectroscopy (ICP-AES). Diffuse reflectance spectroscopy (DRS) results shows that the band gap of ZnO nanoparticles is blue shifted with decrease in particle size. Photoluminescence properties of ZnO nanoparticles at room temperature were studied and the green photoluminescent emission from ZnO nanoparticles can originate from the oxygen vacancy or ZnO interstitial related defects.