Preparation of ultrafine CsCl crystallites by combined cryogenic and room temperature ball milling

The present investigation reports the preparation and microstructural characterization of ultrafine CsCl crystallites using combined cryogenic and room temperature (RT) mechanical milling. The milling has been performed in evacuated WC vials under high purity argon atmosphere. The low temperature milling has been utilized as an effective means of rapid fracturing of the CsCl crystallites. This was followed by RT milling for different time durations. The final crystallite size obtained is 10 +/- 6 nm for sample cryo-milled for 11 h and subsequently RT milled for 35 h. The experimental findings indicate the strong effect of duration of cryo-milling on the final size of the crystallites. The prolonged room temperature milling leads to increase of the crystallite size due to deformation-induced sintering. The results have been discussed in the light of currently available literature. (C) 2011 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Nanocrystalline TiO(2) preparation by microwave route and nature of anatase-rutile phase transition in nano TiO(2)

Nanopowders of TiO(2) has been prepared using a microwave irradiation-assisted route, starting from a metalorganic precursor, bis(ethyl-3-oxo-butanoato)oxotitanium (IV), [TiO(etob)(2)](2). Polyvinylpyrrolidone (PVP) was used as a capping agent. The as-prepared amorphous powders crystallize into anatase phase, when calcined. At higher calcination temperature, the rutile phase is observed to form in increasing quantities as the calcination temperature is raised. The structural and physicochemical properties were measured using XRD, FT-IR, SEM, TEM and thermal analyses. The mechanisms of formation of nano-TiO(2) from the metal-organic precursor and the irreversible phase transformation of nano TiO(2) from anatase to rutile structure at higher temperatures have been discussed. It is suggested that a unique step of initiation of transformation takes place in Ti(1/2)O layers in anatase which propagates. This mechanism rationalizes several key observations associated with the anatase rutile transformation.

Preparation of a thermally sensitive ammonium perchlorate

The effect of ultrasound on the thermal decomposition behaviour of ammonium perchlorate (AP) has been investigated. It was observed that significant changes in the thermal behaviour of A-P, followed using differential thermal analysis and thermogravimetry, was observed when AP was subjected to power ultrasound in water saturated with oxygen-nitrogen mixture. The decomposition temperature of AP was found to have been lowered by nearly 25degreesC. A similar thermal sensitization was observed in AP when subjected to sonication in the presence of transition metal oxides. Kinetic parameters were calculated for AP, modified AP and catalyzed AP decomposition using non-isothermal kinetics. The activation energy for the decomposition of the sonicated AP samples were found to be lower than normal AP.

Mutual inhibition and capacity sharing during parallel preparation of serial eye movements

Many common activities, like reading, scanning scenes, or searching for an inconspicuous item in a cluttered environment, entail serial movements of the eyes that shift the gaze from one object to another. Previous studies have shown that the primate brain is capable of programming sequential saccadic eye movements in parallel. Given that the onset of saccades directed to a target are unpredictable in individual trials, what prevents a saccade during parallel programming from being executed in the direction of the second target before execution of another saccade in the direction of the first target remains unclear. Using a computational model, here we demonstrate that sequential saccades inhibit each other and share the brain's limited processing resources (capacity) so that the planning of a saccade in the direction of the first target always finishes first. In this framework, the latency of a saccade increases linearly with the fraction of capacity allocated to the other saccade in the sequence, and exponentially with the duration of capacity sharing. Our study establishes a link between the dual-task paradigm and the ramp-to-threshold model of response time to identify a physiologically viable mechanism that preserves the serial order of saccades without compromising the speed of performance.

Electroless Ni-W-P Coating and Its Nano-WS2 Composite: Preparation and Properties

The ternary alloy Ni-W-P and its WS2 nanocomposite coatings were successfully obtained on low-carbon steel using the electroless plating technique. The sodium tungstate (Na2WO4) concentration in the bath was varied to obtain Ni-W-P deposits containing various Ni and P contents. WS2 composite was obtained with a suitable concentration of Na2WO4 in Ni-P coating. These deposits were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray analysis (EDX) studies. The corrosion behavior was investigated by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) studies in 3.5 wt % NaCl solutions, and the corrosion rates of the coatings for Ni-P, Ni-W-P, and Ni-W-P-WS2 were found to be 2.571 x 10(-5), 8.219 x 10(-7), and 7.986 x 10(-7) g/h, respectively. An increase in the codeposition of alloying metal tungsten (W) enhanced the corrosion resistance and microhardness and changed the structure and morphology of the deposits. Incorporation of WS2 nanoparticles to Ni-W-P alloy coating reduced the coefficient of friction from 0.16 to 0.11 and also helped in improving the corrosion resistance of the coating further.

Preparation and characterization chemistry of nano-crystalline Ni-Cu-Zn ferrite

In submitted research; nanocrystalline powders having elements Ni0.5Cu0.25Zn0.25Fe2 xInxO4 with varied amounts of indium ( x = 0.0, 0.1, 0.2, 0.3 and 0.4) were grown-up by modified citrate to nitrate alchemy. The realism of single phase cubic spinel creation of the synthesized ferrite samples was studied by the DTA-TGA, XRD, SEM, EDX, FT-IR, VSM and dielectric measurements. SEM was applied to inspect the morphological variations and EDX was used to determine the compositional mass ratios. The studies on the dielectric constant (epsilon'), dielectric loss (epsilon `'), loss tangent (tan delta), ac conductivity (sigma(ac)), resistive and reactive parts of the impedance analysis (Z' and Z `') at room temperature were also carried out. The saturation magnetizations (Ms) were determined using the vibrating sample magnetometer (VSM). Ms. decreased with the increase In3+ doping content, as Fe3+ of 5(mu B) ions are replaced by In3+ of 5 mu(B) ions. (C) 2012 Elsevier B. V. All rights reserved.

Preparation of Freestanding Zn Nanocrystallites by Combined Milling at Cryogenic and Room Temperatures

The present investigation reports the preparation of freestanding nanocrystalline Zn by combined mechanical milling at cryogenic and room temperatures. The cryomilling is used as an effective means of rapid fracturing. The detailed scanning electron microscopy and transmission electron microscopy observations indicate that the minimum crystallite size is 6 +/- A 2 nm after 3 hours of cryomilling. The crystallite size increases to 30 +/- A 2 nm after 3 hours of room temperature milling of the cryomilled powder due to deformation-induced sintering. Detailed theoretical analysis allows us to obtain a diagram of size of the nanoparticles formed vs temperature to explain the experimental findings.

Interconnected, ultrafine osmium nanoclusters: preparation and surface enhanced Raman scattering activity

Interconnected Os nanochains consisting of ultrafine particles prepared using a simple procedure yield a coupled surface plasmon peak in the visible region and can be used as substrates for surface enhanced Raman scattering of various analytes.

Preparation of Self Assembled Sodium Oleate Monolayer on Mild Steel and Its Corrosion Inhibition Behavior in Saline water

A self assembled monolayer (SAM) of sodium oleate was generated on mild steel by the dip coating method. Formation of the SAM on mild steel was examined using Infrared Reflection Absorption Spectroscopy (IRRAS) and contact angle measurements. The chemical and anticorrosive properties of the SAM were analyzed using different techniques. IRRAS and water contact angle data revealed the crystallinity and chemical stability of the SAM modified mild steel. The electrochemical measurements showed that the mild steel with the sodium oleate derived SAM exhibited better corrosion resistance in saline water. The effect of temperature and pH on the SAM formation and its anti corrosion ability was explored.

Preparation of zinc oxide coatings by using newly designed metal-organic complexes of Zn: Effect of molecular structure of the precursor and surfactant over the crystallization, growth and luminescence

We report large scale deposition of tapered zinc oxide (ZnO) nanorods on Si(100) substrate by using newly designed metal-organic complex of zinc (Zn) as the precursor, and microwave irradiation assisted chemical synthesis as a process. The coatings are uniform and high density ZnO nanorods (similar to 1.5 mu m length) grow over the entire area (625 mm(2)) of the substrate within 1-5 min of microwave irradiation. ZnO coatings obtained by solution phase deposition yield strong UV emission. Variation of the molecular structure/molecular weight of the precursors and surfactants influence the crystallinity, morphology, and optical properties of ZnO coatings. The precursors in addition with the surfactant and the solvent are widely used to obtain desired coating on any substrate. The growth mechanism and the schematics of the growth process of ZnO coatings on Si(100) are discussed. (c) 2013 Elsevier B.V. All rights reserved.

Preparation and electrochemical performance of porous hematite (alpha-Fe2O3) nanostructures as supercapacitor electrode material

Porous alpha-Fe2O3 nanostructures have been synthesized by sol-gel route. The effect of preparation temperature on the morphology, structure, and electrochemical stability upon cycling has been studied for supercapacitor application. The discharge capacitance of alpha-Fe2O3 prepared at 300 A degrees C is 193 F g(-1), when the electrodes are cycled in 0.5 M Na2SO3 at a specific current of 1 A g(-1). The capacitance retention after 1,000 cycles is about 92 % of the initial capacitance at a current density of 2 A g(-1). The high discharge capacitance as well as stability of alpha-Fe2O3 electrodes is attributed to large surface area and porosity of the material. There is a decrease in specific capacitance (SC) on increasing the preparation temperature. As iron oxides are inexpensive, the synthetic route adopted for alpha-Fe2O3 in the present study is convenient and the SC is high with good cycling stability, the porous alpha-Fe2O3 is a potential material for supercapacitors.

A critical review on in situ reduction of graphene oxide during preparation of conducting polymeric nanocomposites

Graphene oxide (GO), prepared by chemical oxidation of graphite, serves as a building block for developing polymeric nanocomposites. However, their application in electrical conductivity is limited by the fact that the oxygen sites on GO trap electrons and impede charge transport. Conducting nanocomposites can be developed by reducing GO. Various strategies have been adopted to either reduce GO ex situ, before the composite preparation, or in situ during the development of the nanocomposites. The current state of research on in situ reduction of GO during the preparation of conducting polymeric nanocomposites is discussed in this review. The mechanism and the efficiency of reduction is discussed with respect to various strategies employed during the preparation of the nanocomposite, the type of polymer used, and the processing conditions employed, etc. Its overall effect on the electrical conductivity of the nanocomposites is also discussed and the future outlook in this area is presented.

One-step synthesis of a cyclic 2,17-dioxo3,3](4,4 `)biphenylophane and first preparation of a microporous polymer network from a macrocyclic precursor by cyclotrimerization

One-step synthesis of a cyclic 2,17-dioxo3,3](4,4') biphenylophane (MC) was achieved in high yield; its structure was verified by single crystal X-ray analysis. As a first example, a microporous polymer network was formed from macrocycle MC via acid-catalysed cyclotrimerization yielding a BET surface area of ca. 570 m(2) g(-1).