A simple miniature furnace for routine collection of single crystal x-ray data up to 1000°C on the Hilger and Watts linear diffractometer

A miniature furnace suitable for routine collection of x-ray data up to 1000°C from single crystals on the Hilger and Watts linear diffractometer, without restricting the normally allowed region of reciprocal space on the diffractometer, is described. The crystal is heated primarily by radiation from a surrounding current-heated, stationary platinum coil wound on a silica bracket. The coil is split at its middle to provide a 4 mm gap for crystal mounting and x-irradiation. The crystal, mounted on a standard goniometer head, can be rotated and centred freely, as in the room temperature case. There is no need for any radiation shields or water-cooling arrangement. Investigations up to 1500°C are possible with slight modifications of the furnace.

Assembly of sol-gel-grown $Li _{(x)} CoO_{2}$ nanocrystals through electromagnetic irradiation

We report the fabrication of assembled nanostructures from the pre-synthesized nanocrystals building blocks through optical means of exciton formation and dissociation. We demonstrate that Li (x) CoO2 nanocrystals assemble to an acicular architecture, upon prolonged exposure to ultraviolet-visible radiation emitted from a 125 W mercury vapor lamp, through intermediate excitation of excitons. The results obtained in the present study clearly show how nanocrystals of various materials with band gaps appropriate for excitations of excitons at given optical wavelengths can be assembled to unusual nanoarchitectures through illumination with incoherent light sources. The disappearance of exciton bands due to Li (x) CoO2 phase in the optical spectrum of the irradiated film comprising acicular structure is consistent with the proposed mechanism of exciton dissociation in the observed light-induced assembly process. The assembly process occurs through attractive Coulomb interactions between charged dots created upon exciton dissociation. Our work presents a new type of nanocrystal assembly process that is driven by light and exciton directed.

The effect of composition, electron irradiation and quenching on ionic conductivity in a new solid polymer electrolyte: (PEG) (x) NH4I

We have prepared, characterized and investigated a new PEG-2000 based solid polymer electrolyte (PEG) x NH4I. Ionic conductivity measurements have been made as a function of salt concentration as well as temperature in the range 265–330 K. Selected compositions of the electrolyte were exposed to a beam of 8 MeV electrons to an accumulated dose of 10 kGy to study the effect on ionic conductivity. The electrolyte samples were also quenched at liquid nitrogen temperature and conductivity measurements were made. The ionic conductivity at room temperature exhibits a characteristic double peak for the composition x = 20 and 70. Both electron beam irradiation and quenching at low temperature have resulted in an increase in conductivity by 1–2 orders of magnitude. The enhancement of conductivity upon irradiation and quenching is interpreted as due to an increase in amorphous region and decrease in crystallinity of the electrolyte. DSC and proton NMR measurements also support this conclusion.

Spinodal Decomposition in Tellurite-Based Glasses Induced by Excimer Laser Irradiation

Tellurite-based glasses in the TeO2-K3Li2Nb5O15, TeO2-Ba5Li2Ti2Nb8O30, and V2Te2O9 were fabricated by the conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via the X-ray powder diffraction technique and differential thermal analysis, respectively. The as-quenched samples were irradiated by an excimer laser (248 nm). The effect of laser power, duration of irradiation, and the frequency of the laser pulses on the surface features of the above glasses were studied. The optical microscopic studies carried out on the above systems revealed the presence of quasi-periodic and periodic structures on their surfaces. The local compositional variations of these structures were confirmed by back-scattered electron imaging using scanning electron microscope accompanied by energy-dispersive X-ray analysis. These results were convincing enough to state that the glasses in the present investigations had undergone spinodal decomposition on laser irradiation. The incidence of the interconnected texture of two different phases was observed owing to the quenching effect produced by the heating and cooling cycle of the successive laser pulses. Ring- and line-shaped patterns were also observed, respectively, when the pulse frequency of the laser and the duration of irradiation were increased.

Rapid growth of nanotubes and nanorods of wurtzite ZnO through microwave-irradiation of a metalorganic complex of zinc and a surfactant in solution

Large quantities of single-crystalline ZnO nanorods and nanotubes have been prepared by the microwave, irradiation of a metalorganic complex of zinc, in the presence of a surfactant. The method is simple, fast, and inexpensive (as it uses a domestic microwave oven), and yields pure nanostructures of the hexagonal wurtzite phase of ZnO in min, and requires no conventional templating. The ZnO nanotubes formed have a hollow core with inner diameter varying from 140-160 nm and a wall of thickness, 40-50 nm. The length of nanorods and nanotubes varies in the narrow range of 500-600 nm. These nanostructures have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods and nanotubes are found by SAED to be single-crystalline. The growth process of ZnO nanorods and nanotubes has been investigated by varying the surfactant concentration and microwave irradiation time. Based on the various results obtained, a tentative and plausible mechanism for the formation of ZnO nanostructures is proposed.

Formation of crystalline diamond from amorphous diamond-like carbon films by pulsed laser irradiation

The formation of crystalline diamond films from amorphous diamond-like carbon films by pulsed laser irradiation with a 300 μs non-Q-switched Nd:YAG laser has been established by a combined study of transmission electron microscopy, x-ray photoelectron spectroscopy, and electrical resistivity. The films have been prepared by glow discharge decomposition of a mixture of propane, n-butane, and hydrogen in a rf plasma operating at a frequency of 13.56 MHz. Prior to laser irradiation, the films have been found to be amorphous by transmission electron microscope studies. After irradiation, the electron diffraction patterns clearly point out the formation of cubic diamond structure with a lattice spacing of 3.555 Å. However, the close similarity between diamond and graphite electron diffraction patterns could sometimes be misleading regarding the formation of a diamond structure, and hence, x-ray photoelectron spectroscopic studies have been carried out to confirm the results. A chemical shift in the C 1s core level binding energies towards higher values, viz., from 286.5 to 287.8 eV after laser irradiation, and a high electrical resistivity >1013 Ω cm are consistent with the growth of diamond structure. This novel "low-temperature, low-pressure" synthesis of diamond films offers enormous potential in terms of device compatibility with other solid-state devices.

Microwave irradiation-assisted method for the deposition of adherent oxide films on semiconducting and dielectric substrates

We report a method for the deposition of thin films and thick coatings of metal oxides through the liquid medium, involving the micro waveirradiation of a solution of a metal-organic complex in a suitable dielectric solvent. The process is a combination of sol-gel and dip-coating methods, wherein coatings can be obtained on nonconducting and semiconducting substrates, within a few minutes. Thin films of nanostructured ZnO (wurtzite) have been obtained on Si(100), glass and polymer substrates, the nanostructure determined by process parameters The coatings are strongly adherent and uniform over 15 mm x 15 mm, the growth rate similar to 0.25 mu m/min Coatings of nanocrystalline Fe2O3 and Ga2O3 have also been obtained The method is scalable to larger substrates, and is promising as a low temperature technique for coating dielectric substrates, including flexible polymers. (C) 2010 Elsevier B.V. All rights reserved.

Physico-chemical properties of pure and x-ray irradiated single crystals of KAP

Single crystals of potassium hydrogen phthalate (KAP) have been grown by slow evaporation method from aqueous solutions. Thermal analyses indicate that KAP crystals decompose into phthalic anhydride and KOH around 520 K. Electrical properties of single crystals of KAP have been studied along with the effect of X-ray irradiation of the crystals. The electrical transport appears to be associated with tunneling of protons. The irradiated crystal exhibits lower dielectric constant and higher ac conductivity.

Switching studies and the effect of irradiation on ferroelectric properties of TAAP and DTAAP

Polarization switching processes in TAAP and DTAAP have been studied by the Merz method. The switching process in DTAAP is slower than in TAAP. The temperature dependence of switching time indicates that the crystal might contain groups of domain nuclei with different activation energies. X-ray irradiation causes an increase in the threshold field below which switching could not occur and decrease in the mobility of domain walls. Irradiation decreases the peak value of dielectric constant, Tc and increases the value of coercive field. Domain structure studies on TAAP crystals have shown that the crystals grow as both predominantly single domain and multi domains, depending on which the internal bias increases or remains unaffected upon irradiation.

Critical exponent of the electrical conductivity in the paracoherence region of a thin film of YBa2Cu3O7?x

Critical exponent of the electrical conductivity in the paracoherence region (gamma) of the high temperature superconductor YBa2Cu3O7-x (YBCO) has been estimated for high quality thin film on ZrO2 substrate prepared by high pressure oxygen sputtering. High energy ion irradiation was carried out using 100 MeV O-16(7+) ions at liquid nitrogen to see the effects of disorder on the value of the exponent. The critical exponent from a value of about 2 to 1.62 upon irradiation. Studies were also carried film to see the effect of ageing and annealing.

Effect of lithium ion irradiation on the transport and optical properties of Bridgman grown n-type InSb single crystals

Single crystal (100) wafers of n-InSb were implanted with 50 MeV Li3+ ions at various fluences ranging from 10(10) to 10(14) ions/cm(2) at room temperature. Investigations of the optical, electrical, and structural properties of the as-grown, irradiated, annealed wafers were carried out by infrared and Raman spectroscopies, Hall measurements, and high resolution x-ray diffraction (HRXRD). In the case of samples irradiated with an ion fluence of 1.6x10(14) ions/cm(2), electrical measurements at 80 K reveal that there is a decrease in carrier concentration from 8.5x10(15) (for unirradiated) to 1.1x10(15)/cm(3) and an increase in mobility from 5.4x10(4) to 1.67x10(5) cm(2)/V s. The change in carrier concentration is attributed to the creation of electron trap centers induced by ion beam irradiation and the increase in mobility to the formation of electrical inactive complexes. Nevertheless, even with the irradiation at 1.6x10(14) ions/cm(2) fluence the crystalline quality remains largely unaffected, as is seen from HRXRD and Raman studies. (C) 2001 American Institute of Physics.

Surfactant-mediated Synthesis of Functional Metal Oxide Nanostructures via Microwave Irradiation-assisted Chemical Synthesis

Nanostructured materials have attracted considerable interest in recent years due to their properties which differ strongly from their bulk phase and potential applications in nanoscale electronic and optoelectronic devices. Metal oxide nanostructures can be synthesized by variety of different synthesis techniques developed in recent years such as thermal decomposition, sol-gel technique, chemical coprecipitation, hydrothermal process, solvothermal process, spray pyrolysis, polyol process etc. All the above processes go through a tedious synthesis procedure followed by prolonged heat treatment at elevated temperature and are time consuming. In the present work we describe a rapid microwave irradiation-assisted chemical synthesis technique for the growth of nanoparticles, nanorods, and nanotubes of a variety of metal oxides in the presence of an appropriate surfactant, without the use of any templates The method is simple, inexpensive, and helps one to prepare nanostructures in a very simple way, and in a very short time, measured in minutes. The synthesis procedure employs high quality metalorganic complexes (typically -diketonates) featuring a direct metal-to-oxygen bond in its molecular structure. The complex is dissolved in a suitable solvent, often with a surfactant added, and the solution then subjected to microwave irradiation in a domestic microwave oven operating at 2.45 GHz frequency with power varying from 160-800 W, from a few seconds to a few minutes, leading to the formation of corresponding metal oxides. This method has been used successfully to synthesize nanostructures of a variety of binary and ternary metal oxides such as ZnO, CdO, Fe2O3, CuO, Ga2O3, Gd2O3, ZnFe2O4, etc. There is an observed variation in the morphology of the nanostructures with the change of different parameters such as microwave power, irradiation time, appropriate solvent, surfactant type and concentration. Cationic, anionic, nonionic and polymeric surfactants have been used to generate a variety of nanostructures. Even so, to remove the surfactant, there is either no need of heat treatment or a very brief exposure to heat suffices, to yield highly pure and crystalline oxide materials as prepared. By adducting the metal complexes, the shape of the nanostructures can be controlled further. In this manner, very well formed, single-crystalline, hexagonal nanorods and nanotubes of ZnO have been formed. Adducting the zinc complex leads to the formation of tapered ZnO nanorods with a very fine tip, suitable for electron emission applications. Particle size and their monodispersity can be controlled by a suitable choice of a precursor complex, the surfactant, and its concentration. The resulting metal oxide nanostructures have been characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, FTIR spectroscopy, photoluminescence, and electron emission measurements.

Gray track formation in KTiOPO4 by swift ion irradiation

Potassium titanyl phosphate single crystals were irradiated with 48 MeV lithium ions at fluences varying from 5×1012 to 1016 ions/cm2. The defects created in the crystal have been characterized using x-ray rocking curve measurements, optical transmittance, and photoluminescence spectroscopy. From x-ray rocking curve studies, the full width at half maximum for the irradiated samples was observed to increase, indicating lattice strain caused by the energetic ions. Optical transparency of these samples was found to decrease upon irradiation. The irradiated samples exhibited a broadband luminescence in the 700–900 nm region, for fluences above 5×1013 ions/cm2. The results indicate that ion-beam-induced optical effects in KTiOPO4 single crystals are very similar to the ones obtained for crystals with “gray tracks,” which are attributed to the electronic transitions in the Ti3+ levels.

Comparison of rhodamine B degradation under UV irradiation by two phases of titania nano-photocatalyst

Titania (TiO2) nano-photocatalysts, with different phases, prepared using a modified sol-gel process were employed in the degradation of rhodamine at 10 mg L-1 concentration. The degradation efficiency of these nano-photocatalysts was compared to that of commercial Degussa P25 titania. It was found that the nanocatalysts calcined at 450 degrees C and the Degussa P25 titania had similar photoreactivity profiles. The commercial Degussa P25 nanocatalysts had an overall high apparent rate constant of (K-app) of 0.023 min(-1). The other nanocatalyst had the following rate constants: 0.017, 0.0089, 0.003 and 0.0024 min(-1) for 450, 500, 550 and 600 degrees C calcined catalysts, respectively. This could be attributed to the phase of the titania as the anatase phase is highly photoactive than the other phases. Furthermore, characterisation by differential scanning calorimetry showed the transformation of titania from amorphous to anatase and finally to rutile phase. SEM and TEM characterisations were used to study the surface morphology and internal structure of the nanoparticles. BET results show that as the temperature of calcinations was raised, the surface area reduced marginally. X-ray diffraction was used to confirm the different phases of titania. This study has led to a conclusion that the anatase phase of the titania is the most photoactive nanocatalyst. It also had the highest apparent rate constant of 0.017 min(-1), which is similar to that of the commercial titania.