X-ray photoemission study of MgB<Subscript>2</Subscript> films synthesized from in-situ annealed MgB<Subscript>2</Subscript>/Mg multilayers

Superconducting MgB₂ films were obtained by in-situ annealing of precursor multilayers deposited at low substrate temperature by sputtering from a MgB₂ stoichiometric target and by thermal evaporation of pure Mg. After an in-situ annealing at 500–600 °C, the films showed a zero resistance critical temperature up to 31 K. The as-obtained MgB₂ films were investigated by X-ray photoelectron spectroscopy (XPS) and X-ray auger electron spectroscopy (XAES). The electronic structure was studied by monitoring the B 1s, Mg 2p, O 1s core-levels and the Mg KL₂L₃ Auger line. For comparison, the electronic structure of an MgB₂ commercial superconducting sputtering target, of a not-annealed precursor film and of a sample obtained by direct sputtering from the MgB₂ target have also been investigated. Electron spectroscopy showed that in the superconducting systems the Mg KL₂L₃ Auger line kinetic energy position is always higher by about 0.9 eV with respect to the energy position of the same Auger line measured in the non-superconducting samples. PACS 74.25Jb; 74.78.Bz; 74.70.Ad     

Light intensity and temperature dependence on performance of a photoelectrochemical cells of ITO/TiO<Subscript>2</Subscript>/PVC-LiClO<Subscript>4</Subscript>/graphite

The photovoltaic characteristics of a photoelectrochemical cell of ITO/TiO₂/PVC-LiClO₄/graphite are reported. This paper is concerned with the influence of light intensity and temperature on short-circuit current density, J_sc and open-circuit voltage, V_oc of the device. The photoelectrochemical cell material was a screen-printed layer of titanium dioxide onto an ITO-covered glass substrate, which was used as a working electrode of the cell. The solid electrolyte was polivinylchloride-lithium perchlorate. The graphite film serves as a counter electrode of the cell. The current density–voltage characteristics of the device under an illumination of 20, 40, 60, 80 and 100 mW cm⁻² light from a tungsten halogen lamp were recorded at 40 °C as well as under an illumination of 100 mW cm⁻² at 30, 35, 40, 45 and 50 °C, respectively. It was found that the short-circuit current density, J_sc of the device increases with both light intensity and temperature. The J_sc obtained at 100 mW cm⁻² was 1.0 μAcm⁻² and that at 50 °C was 0.7 μAcm⁻².     

Physical property characterization of bulk MgB<Subscript>2</Subscript> superconductor

We report synthesis, structure/micro-structure, resistivity under magnetic field [ρ(T)H], Raman spectra, thermoelectric power S(T), thermal conductivity κ(T), and magnetization of ambient pressure argon annealed polycrystalline bulk samples of MgB₂, processed under identical conditions. The compound crystallizes in hexagonal structure with space group P6/mmm. Transmission electron microscopy (TEM) reveals electron micrographs showing various types of defect features along with the presence of 3–4 nm thick amorphous layers forming the grain boundaries of otherwise crystalline MgB₂. Raman spectra of the compound at room temperature exhibited characteristic phonon peak at 600 cm^-1. Superconductivity is observed at 37.2 K by magnetic susceptibility χ(T), resistivity ρ(T), thermoelectric power S(T), and thermal conductivity κ(T) measurements. The power law fitting of ρ(T) give rise to Debye temperature (Θ_D) at 1400 K which is found consistent with the theoretical fitting of S(T), exhibiting Θ _D of 1410 K and carrier density of 3.81 × 10²⁸/m³. Thermal conductivity κ(T) shows a jump at 38 K, i.e., at T_c, which was missing in some earlier reports. Critical current density (J_c) of up to 10⁵ A/cm² in 1–2 T (Tesla) fields at temperatures (T) of up to 10 K is seen from magnetization measurements. The irreversibility field, defined as the field related to merging of M(H) loops is found to be 78, 68 and 42 kOe at 4, 10 and 20 K respectively. The superconducting performance parameters viz. irreversibility field (H_irr) and critical current density J_c(H) of the studied MgB₂ are improved profoundly with addition of nano-SiC and nano-diamond. The physical property parameters measured for polycrystalline MgB₂ are compared with earlier reports and a consolidated insight of various physical properties is presented.     

MgB2 coated conductors directly grown on flexible metallic Hastelloy tapes by hybrid physical–chemical vapor deposition

MgB₂ coated conductors (CCs), which can avoid the low packing density problem of powder-in-tube (PIT) processed wires, can be a realistic solution for practical engineering applications. Here we report on the superior superconducting properties of MgB₂ CCs grown directly on the flexible metallic Hastelloy tapes without any buffer layer at various deposition temperatures from 520 to 600 °C by using hybrid physical–chemical vapor deposition (HPCVD) technique. The superconducting transition temperatures (T_c) are in the range of 38.5–39.4 K, comparable to bulk samples and high quality thin films. Clear (101) and (002) reflection peaks of MgB₂ are observed in the X-ray diffraction patterns without any indication of chemical reaction between MgB₂ and Hastelloy tapes. From scanning electron microscopy, it was found that connection between MgB₂ grains and voids strongly depend on the growth temperature. A systematic increase in the flux pinning force density and thereby the critical current density with decreasing growth temperature was observed for the MgB₂ CCs. The critical current density (J_c) of J_c(5 K, 0 T) ～10⁷ A/cm² and J_c(5 K, 2.5 T) ～10⁵ A/cm² has been obtained for the sample fabricated at a low growth temperature of 520 °C. The enhanced J_c (H) behavior can be understood on the basis of the variation in the microstructure of MgB₂ CCs with growth temperature.     

Electrophysical properties and the structure of the YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript> compound thermally restored after low-temperature decomposition

The electrophysical properties and structure of the nonstoichiometric high-temperature superconductor YBa₂Cu₃O _y restored at T = 930–950°C after low-temperature decomposition (T = 200°C) into phases different in the oxygen content have been studied. It has been shown that, unlike heat treatments at T ≤ 900°C, the superconducting properties are almost completely restored for 3–5 h during grain recrystallization, which is impossible at lower temperatures. After short-term annealing at T = 930–950°C (for 1–2 h), the ceramic material still contains a significant number of structural defects, most likely, in cation sublattices. These defects can contribute to the pinning of magnetic vortices, which substantially increases the critical current density in magnetic fields up to 2 T as compared to ceramic materials produced by the conventional technology.     

Evolution of the structure and properties of the MgB<Subscript>2</Subscript> superconductor under isothermal annealing

The effect of comparatively weak actions on the structure of the two-gap BCS superconductor MgB₂ was studied. The MgB₂ samples studied differed in terms of the annealing time at 900°C. It was found that the lattice parameters, residual resistivity, and critical temperature depend only weakly on the annealing time, whereas the electrical resistivity decreases by a few times when the annealing time is increased from 2 to 10 h. It is assumed that the observed effects may be caused by the influence of Mg and B atom ordering in the MgB₂ lattice on charge transfer over the two-dimensional B-B σ bonds.     

Mechanism of the formation of structure during high-temperature annealing of MgB<Subscript>2</Subscript> bulk samples deformed under pressure

MgB₂ superconductors subjected to deformation under pressure on Bridgeman anvils and subsequent annealings at 800 and 950°C were investigated by X-ray diffraction, scanning electron microscopy, and microanalysis. It was shown that at these temperatures crystals of MgB₂ phase along the residual boron dissolute in the residual liquid magnesium with the formation of both dense and loose areas of MgB₂ phase. The latter has a negative influence on critical current. At the same time, after these treatments, the samples become more uniform by the phase and chemical composition.     

Photoluminescence,thermoluminescence and electron spin resonance studies on Eu<Superscript>3+</Superscript> doped Ca<Subscript>3</Subscript>Al<Subscript>2</Subscript>O<Subscript>6</Subscript> red phosphors

Tricalcium aluminate doped with Eu³⁺ was prepared at furnace temperatures as low as 500°C by using the convenient combustion route and examined using powder X-ray diffraction, scanning electron microscope and photoluminescence techniques. A room-temperature photoluminescence study showed that the phosphors can be efficiently excited by UV/Visible region, emitting a red light with a peak wavelength of 616 nm corresponding to the ⁵D₀–⁷F₂ transition of Eu³⁺ ions. The phosphor exhibits three thermoluminescence (TL) peaks at 195°C, 325°C and 390°C. Electron Spin Resonance (ESR) studies were carried out to study the defect centres induced in the phosphor by gamma irradiation and also to identify the defect centres responsible for the TL process. Room-temperature ESR spectrum of irradiated phosphor appears to be a superposition of three distinct centres. One of the centres (centre I) with principal g-value 2.0130 is identified as O⁻ ion while centre II with an axially symmetric principal values g _∥=2.0030 and g _⊥=2.0072 is assigned to an F⁺ centre (singly ionized oxygen vacancy). O⁻ ion (hole centre) correlates with the TL peak at 195°C and the F⁺ centre (electron centre), which acts as a recombination centre, is also correlated to the 195°C TL peak. F⁺ centre further appears to be related to the high temperature peak at 390°C. Centre III is also assigned to an F⁺ centre and seems to be the recombination centre for the TL peak at 325°C.     

纳米C和SiC掺杂对MgB2带材超导性能的影响

采用X射线衍射仪，扫描电镜，超导量子干涉仪等仪器对纳米C和SiC掺杂的MgB₂带材进行了表征，并采用标准四引线法对样品的临界电流进行了测试. 实验表明，C和SiC掺杂在提高MgB₂带材高场下的临界电流密度方面具有显著效果. 在温度为4.2 K、磁场大于9 T条件下，C和SiC掺杂样品的临界电流密度与未掺杂样品相比均提高一个数量级以上. 掺杂样品高磁场下良好的临界电流性能主要归因于C对B的替代所产生的晶格畸变、位错等缺陷和局部成分变化而导致的有效晶内钉扎作用. 实验结果表明，SiC掺杂的MgB2带材之所以具有非常好的高场电流特性，和C掺杂的样品一样， C对B的替代起到十分关键的作用. 关键词： 2带材')" href="#">MgB₂带材 C掺杂 SiC掺杂 临界电流性能     

Synthesis and gas sensing properties of perovskite CdSnO<Subscript>3</Subscript> nanoparticles

The CdSnO₃ semiconducting oxide that can be used as a gas-sensitive material for detecting ethanol gas is reported in this paper. CdSnO₃ nanoparticles were prepared by a chemical co-precipitation synthesis method, in which the preparation conditions were carefully controlled. The n-type gas-sensing semiconductors were obtained from the as-synthesized powders calcined at 600°C for 1 h. The phase and microstructure of the obtained nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) method with a gas adsorption analyzer. CdSnO₃ has a small particle size range of 30–50 nm and a high surface area of 9.12 m²/g, and a uniformity global shape. The gas sensitivity and operating temperature, and selectivity of CdSnO₃-based sensors were measured in detail. The gas sensors fabricated by CdSnO₃ nanoparticles had good sensitivity and selectivity to vapor of C₂H₅OH when working temperature at 267°C, the value of gas sensitivity at 100 ppm of C₂H₅OH gas can reach 11.2 times. Furthermore, gas-sensing mechanism was studied by using chromatographic analysis.     

Nanocrystalline CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> powders prepared by egg white solution route: synthesis,characterization and its giant dielectric properties

Nanocrystalline CaCu₃Ti₄O₁₂ powders with particle sizes of 50–90 nm were synthesized by a simple method using Ca(NO₃)₂·4H₂O, Cu(NO₃)₂·4H₂O, titanium(diisoproproxide) bis(2,4-pentanedionate) and freshly extracted egg white (ovalbumin) in aqueous medium. The synthesized precursor was characterized by TG-DTA to determine the thermal decomposition and crystallization temperature which was found to be at above 400 °C. The precursor was calcined at 700 and 800 °C in air for 8 h to obtain nanocrystalline powders of CaCu₃Ti₄O₁₂. The calcined CaCu₃Ti₄O₁₂ powders were characterized by XRD, FTIR, SEM and TEM. Sintering of the powders was conducted in air at 1100 °C for 16 h. The XRD results indicated that all sintered samples have a typical perovskite CaCu₃Ti₄O₁₂ structure and a small amount of CuO, although the sintered sample of the 700 °C calcined powders contained some amount of CaTiO₃. SEM micrographs showed the average grain sizes of 12.0±7.8 and 15.5±8.9 μm for the sintered CaCu₃Ti₄O₁₂ ceramics prepared using the CaCu₃Ti₄O₁₂ powders calcined at 700 and 800 °C, respectively. The sintered samples exhibit a giant dielectric constant, ε^′ of ∼ 1.5–5×10⁴. The dielectric behavior of both samples exhibits Debye-like relaxation, and can be explained based on a Maxwell–Wagner model. PACS 77.22.Gm; 81.05.Je; 81.07.Wx; 81.20.Ev     

Influence of Ni addition on the process of phase formation in MgB2 bulk

Nickel is an important sheath material for the fabrication of MgB₂ wires. However, the effects of Ni doping on the phase formation and superconducting properties of MgB₂ remain controversial. In this work, Ni powder is selected for doping in MgB₂ bulk in order to examine the corresponding changes. Combining with the DSC analysis and in-situ XRD results, we find indications that the Ni powder reacted with Mg and B, forming MgNi_2.5B₂ at 600°C. The ternary compound began to decompose at a temperature above 800°C. The reactive phase, MgNi_2.5B₂, acted as an obstacle to the supercurrent flow, creating weak links among the MgB₂ grain boundaries. However, it is found that the added Ni formed a eutectic liquid phase with Mg at 506°C. The liquid phase helps the formation of MgB₂ at low temperature, which not only increases the density of the sample, but also improves the grain connectivity. Consequently, the presence of Ni in the MgB₂ sample is not necessarily a disadvantage; it depends on the desired application.     

MgB2 coated superconducting tapes with high critical current densities fabricated by hybrid physical-chemical vapor deposition

The MgB₂ coated superconducting tapes have been fabricated on textured Cu (0 0 1) and polycrystalline Hastelloy tapes using coated conductor technique, which has been developed for the second generation high temperature superconducting wires. The MgB₂/Cu tapes were fabricated over a wide temperature range of 460-520 °C by using hybrid physical-chemical vapor deposition (HPCVD) technique. The tapes exhibited the critical temperatures (T_c) ranging between 36 and 38 K with superconducting transition width (ΔT_c) of about 0.3-0.6 K. The highest critical current density (J_c) of 1.34 × 10⁵ A/cm² at 5 K under 3 T is obtained for the MgB₂/Cu tape grown at 460 °C. To further improve the flux pinning property of MgB₂ tapes, SiC is coated as an impurity layer on the Cu tape. In contrast to pure MgB₂/Cu tapes, the MgB₂ on SiC-coated Cu tapes exhibited opposite trend in the dependence of J_c with growth temperature. The improved flux pinning by the additional defects created by SiC-impurity layer along with the MgB₂ grain boundaries lead to strong improvement in J_c for the MgB₂/SiC/Cu tapes. The MgB₂/Hastelloy superconducting tapes fabricated at a temperature of 520 °C showed the critical temperatures ranging between 38.5 and 39.6 K. We obtained much higher J_c values over the wide field range for MgB₂/Hastelloy tapes than the previously reported data on other metallic substrates, such as Cu, SS, and Nb. The J_c values of J_c(20 K, 0 T) ∼5.8 × 10⁶ A/cm² and J_c(20 K, 1.5 T) ∼2.4 × 10⁵ A/cm² is obtained for the 2-μm-thick MgB₂/Hastelloy tape. This paper will review the merits of coated conductor approach along with the HPCVD technique to fabricate MgB₂ conductors with high T_c and J_c values which are useful for large scale applications.     

Growth and sintering effects of hydrated polycrystalline Li<Subscript>2</Subscript>WO<Subscript>4</Subscript>

Polycrystalline Li₂WO₄ was sintered at temperatures, 400, 450, 500, 550, 600, 650, and 700 °C. After sintering at each particular temperature, the Li₂WO₄ was cooled to room temperature. The X-ray diffraction pattern of Li₂WO₄ exhibits dominant peaks attributable to 7Li₂WO₄.4H₂O (cubic) and Li₂WO₄ (hexagonal) and thus reveals the extent of hydration of the material. The composition varies on heating at several temperatures as shown by the presence of new peaks in the diffractogram. Thermogravimetric analysis is used to correlate respective structural and thermal properties in variation. The impedance spectra show the presence of a semicircle in the higher frequency regions and straight line behaviors at lower frequencies. SEM micrographs depict the image of sintered Li₂WO₄. Grain growth studies reveal the sensitiveness of grain toward temperature. The maximum grain size is observed to be ≈5.7 μm at 700 °C.     

Properties of MgB2 superconductor chemically treated by acetic acid

Commercial Alfa Aesar MgB₂ powder was chemically treated by acetic acid with the aim of MgO removing. Single-core MgB₂/Fe ex situ wires have been made by powder-in-tube (PIT) process using the powders treated with different acid concentration. All samples were annealed in argon at 950 °C/0.5 h. Differences in transition temperatures and critical currents of acetic acid treated MgB₂ are related to the normal state resistivity, effective carbon substitution from the organic solvent and the active area fraction (grain-connectivity).     

Thermally stimulated transformations in brookite-containing TiO<Subscript>2</Subscript> nanopowders produced by the hydrolysis of TiCl<Subscript>4</Subscript>

TiO₂ nanopowder is produced by the low-temperature hydrolysis of TiCl₄. The phase composition of the sample is found to form at a hydrolysis temperature of 30–38°C. Low-temperature annealing (up to 440°C) increases the degree of crystallinity of the phases present in the sample (anatase, brookite) and only weakly affects their ratio. At 500°C, the sample consists of three phases: rutile is detected apart from anatase and brookite. Brookite begins to fail at 600°C; at 700°C, crystalline brookite fails completely.     

Nanosized IrO<Subscript>2</Subscript> electrocatalysts for oxygen evolution reaction in an SPE electrolyzer

Nanosized IrO₂ electrocatalysts (d ~ 7–9 nm) with specific surface area up to 100 m² g⁻¹ were synthesized and characterized for the oxygen evolution reaction in a solid polymer electrolyte (SPE) electrolyzer. The catalysts were prepared by a colloidal method in aqueous solution and a subsequent thermal treatment. An iridium hydroxide hydrate precursor was obtained at ~100 °C, which was, successively, calcined at different temperatures from 200 to 500 °C. The physico-chemical characterization was carried out by X-ray diffraction (XRD), thermogravimetry–differential scanning calorimetry (TG–DSC) and transmission electron microscopy (TEM). IrO₂ catalysts were sprayed onto a Nafion 115 membrane up to a loading of 3 mg cm⁻². A Pt catalyst was used at the cathode compartment with a loading of 0.6 mg cm⁻². The electrochemical activity for water electrolysis of the membrane-electrode assemblies (MEAs) was investigated in a single cell SPE electrolyzer by steady-state polarization curves, impedance spectroscopy and chrono-amperometric measurements. A maximum current density of 1.3 A cm⁻² was obtained at 1.8 V and 80 °C for the IrO₂ catalyst calcined at 400 °C for 1 h. A stable performance was recorded in single cell for this anode catalyst at 80 °C. The suitable catalytic activity and stability of the most performing catalyst were interpreted in terms of proper combination between nanostructure and suitable morphology.     

Thermostable photocatalytically active TiO<Subscript>2</Subscript> anatase nanoparticles

Anatase is the low-temperature (300–550 °C) crystalline polymorph of TiO₂ and it transforms to rutile upon heating. For applications utilizing the photocatalytic properties of nanoscale anatase at elevated temperatures (over 600 °C) the issue of phase stabilisation is of major interest. In this study, binary TiO₂/SiO₂ particles were synthesized by a flame aerosol process with TiCl₄ and SiCl₄ as precursors. The theoretical Si/Ti ratio was varied in the range of 0.7–1.3 mol/mol. The synthesized TiO₂/SiO₂ samples were heat treated at 900 and 1,000 °C for 3 h to determine the thermostability of anatase. Pyrogenic TiO₂ P25 (from Evonik/Degussa, Germany) widely applied as photocatalyst was used as non-thermostabilized reference material for comparison of photocatalytic activity of powders. Both the non-calcinated and calcinated powders were characterized by means of XRD, TEM and BET. Photocatalytic activity was examined with dichloroacetic acid (DCA) chosen as a model compound. It was found that SiO₂ stabilized the material retarding the collapse of catalyst surface area during calcination. The weighted anatase content of 85% remains completely unchanged even after calcination at 1,000 °C. The presence of SiO₂ layer/bridge as spacer between TiO₂ particles freezes the grain growth: the average crystallite size increased negligibly from 17 to 18 nm even during the calcination at 1,000 °C. Due to the stabilizing effect of SiO₂ the titania nanoparticles calcinated at 900 and 1,000 °C show significant photocatalytic activity. Furthermore, the increase in photocatalytic activity with calcination temperature indicates that the titania surface becomes more accessible either due to intensified cracking of the SiO₂ layer or due to enhanced transport of SiO₂ into the necks thus releasing additional titania surface.     

Effects of doping with nanoscale Co3O4 particles on the superconducting properties of powder-in-tube processed MgB2 tapes

Nanoscale Co₃O₄ particles were doped into MgB₂ tapes with the aim of developing superconducting wires with high-current-carrying capacity. Fe-sheathed MgB₂ tapes with a mono-core were prepared using the in situ powder-in-tube (PIT) process with the addition of 0.2–1.0 mol% Co₃O₄. The critical temperature decreased monotonically with an increasing amount of doped Co₃O₄ particles for all heat-treatment temperatures from 600 to 900 °C. However, the transport critical current density (J_c) at 4.2 K varied with the heat-treatment temperatures. The J_c values in magnetic fields ranging from 7 to 12 T decreased monotonically with increasing Co₃O₄ doping level for a heat-treatment temperature of 600 °C. In contrast, some improvements on the J_c values of the Co₃O₄ doped tapes were observed in the magnetic fields below 10 T for 700 and 800 °C. Furthermore, J_c values in all the fields measured increased as the Co₃O₄ doping level increase from 0 to 1 mol% for 900 °C. This heat-treatment temperature dependence of the J_c values could be explained in terms of the heat-treatment temperature dependence of the irreversibility field with Co₃O₄ doping.     

Ultra-sharp α-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoflakes: growth mechanism and field-emission

We report the synthesis of single-crystalline α-Fe₂O₃ nanoflakes from a simple Fe–air reaction within the temperatures range of 260–400 °C. The nanoflakes synthesized at the lowest temperature (260 °C) in this work show an ultra-sharp morphology: 5–10 nm in thickness, 1–2 μm in length, 20 nm in base-width and around 5 nm at the tips; successfully demonstrate the promising electron field emission properties of a large-scaled α-Fe₂O₃ nanostructure film and exhibit the potential applications as future field-emission (FE) electron sources and displays (FEDs). The formation and growth of α-Fe₂O₃ nanostructures were discussed based on the surface diffusion mechanism. PACS 79.60.Jv; 79.70.+q; 77.84.Bw