Synthesis and characterization of nano-sized BaxSr1?xSO4 (0 ≤ x ≤ 1) solid solution by a simple surfactant-free aqueous solution route

A facile aqueous solution route has been employed to synthesize Ba _x Sr_1−x SO₄ (0 ≤ x ≤ 1) solid solution nanocrystals at room temperature without using any surfactants or templates. The as-synthesized products were characterized by means of X-ray diffraction (XRD), X-ray fluorescence spectrometer (XRF), scanning electron microscopy (SEM), and differential scanning calorimetry-thermogravimetry (DSC-TG). The Ba _x Sr_1−x SO₄ solid solution nanocrystals exhibit an orthorhombic structure and an ellipsoidal-shaped morphology with an average size of 80–100 nm. The lattice parameters of Ba _x Sr_1−x SO₄ solid solution crystals increase with increasing x value. However, they are not strictly coincident with the Vegard’s law, which indicates that the as-obtained products are non-ideal solid solutions. The Ba _x Sr_1−x SO₄ solid solution nanocrystals have an excellent thermal stability from ambient temperature to 1300°C with a structural transition from orthorhombic to cubic phase at about 1111°C.     

Superconductivity and Ferromagnetism of the Ru-1232 Compounds in the (Ru1?xNbx)Sr2(GdCe1.8Sr0.2)Cu2Oz System

The Ru-1232 compounds have been synthesized in the (Ru_1–xNb _x )Sr₂(GdCe_1.8Sr_0.2)Cu₂O _z system, and effects of Nb substitution for Ru on superconductivity and ferromagnetism of the Ru-1232 compounds have been investigated. First, X-ray powder diffraction study shows that nearly the single 1232 phase samples can be obtained in the x composition range from 0.0 to 0.3. Then, from the electrical resistivity study, it is found that each of the samples shows resistivity dropping phenomenon at two temperatures of T _c ^l and T _c ^h, which originates from superconductivity of the Ru-1232 phase and the Ru-1222 one, respectively. Both of the starting temperatures are lowering with increasing Nb content x. Lastly, from the magnetic susceptibility study, it is found that superconducting transition temperature T _c is 20 K for the Ru-1232 sample with x = 0.0 and the ferromagnetic transition temperature T _m is about 90 K. This study also shows that both of the values of T _c and T _m become low with increasing x from 0.0 to 0.3.     

Superconductivity of Ba1 ? xKxBiO3 (0.35 < x < 1) Synthesized by the High Pressure and High Temperature Technique

Ba_{1 – x} K _x BiO₃ (BKBO) samples with 0.35 < x < 1 were synthesized by the high pressure and high temperature technique. XRD analysis showed that the BKBO samples were single phase for the whole range of the potassium doping concentration. The change of superconducting transition temperature, T _c, as well as lattice parameters have been investigated upon doping concentration. As the K doping concentration (x) increases from x = 0.37, T _c decreases from 30.4 K to almost zero at x = 0.74. However, in some BKBO samples without including any barium in the starting composition (x = 1), which is denoted as KBO samples, superconductivity is observed with T _c as high as 9 K with partial substitutions of Bi at the K site. Depending on the synthesis condition of the KBO samples, T _c and lattice parameters were different from sample to sample. Compared with other superconducting bismuthates, the evolution of T _c by potassium doping in the cubic BKBO system is discussed in terms of its electronic band structure.     

Microstructures and thermoelectric properties of p-type pseudo-binary AgxBi0.5Sb1.5−xTe3 (x = 0.05–0.4) alloys prepared by cold pressing

The p-type pseudo-binary Ag_xBi_0.5Sb_1.5−xTe₃ (x = 0.05–0.4) alloys were prepared by cold pressing. The thermal conductivities (κ) were calculated from the values of heat capacities, densities and thermal diffusivities measured, and range approximately from 0.66 to 0.56 (W K^− 1 m^− 1) for the Ag_xBi_0.5Sb_1.5−xTe₃ alloy with molar fraction x being 0.4. Combining with the electrical properties obtained in the previous study, the maximum dimensionless figure of merit ZT of 1.1 was obtained at the temperature of 558 K.     

Nanostripes in GdBa2Cu3Ox high-Tc superconductors

High-T_c superconductors with light rare earth (LRE) elements instead of Y exhibit nanoscale stripe structures on the surface as observed by atomic force microscopy (AFM) and scanning tunneling microscopy (STM) scans. Within the GdBa₂Cu₃O_x (GdBCO) system exhibiting relatively high critical current densities, nanoclusters arranged in a stripe-like fashion are observed in undoped material, while adding of nanoparticles (ZnO₂, ZrO₂) leads to the formation of nanostripes as observed in other LRE superconductors. The nanostripes in doped GdBCO exhibit periodicties between 20 and 50 nm and corresponding step heights of 0.3–0.8 nm. Using polarized light microscopy and electron backscatter diffraction (EBSD) analysis, we determined the direction of the nanostripes with respect to the known twin structure.     

Doping-induced microstructural, textural and optical properties of In2Ti1−xVxO5+δ semiconductors and their role in the photocatalytic splitting of water

The physicochemical properties of V-doped indium titanates (In₂Ti_1−xV_xO_5+δ, 0.0 ≤ x ≤ 0.2) were investigated by using XPS, powder XRD, UV–vis, SEM and luminescence spectroscopy techniques. The Rietveld refinement of XRD data revealed that even though the V-containing samples were isostructural with In₂TiO₅ (orthorhombic space group Pnma), a systematic x-dependent variation was noticeable in the Ti–O bond lengths in [TiO₆] octahedral units, cell parameters and in the value of δ. XPS results confirmed the coexistence of V⁵⁺ and V⁴⁺ states, leading thereby to an enhancement in oxygen non-stoichiometry in the doped samples. A loading-dependent progressive shift from 400 to 750 nm was also observed in the onset of the absorption edge, indicating a significant narrowing of the band gap. Furthermore, the samples with higher V-content were comprised of the grain clusters having larger size and an irregular shape. The UV–vis, photoluminescence and thermoluminescence studies indicate that the doping-induced lattice defects may give rise to certain closely spaced acceptor/donor energy levels in between the band gap of host matrix. The indium titanates are found to serve as stable photocatalysts for water splitting under visible light, where oxygen was the major reaction product. The role of microstructural and morphological properties in the photocatalytic activity is discussed.     

Internal Oxidation in Bi2.1 ? xPbxSr2 ? yCa1 ? zRy + zCu2O8 + d (R = Y, Nd, La) Solid Solutions

Bi_{2.1 − x} Pb_xSr₂CaCu₂O_{8 + d} samples containing Y, Nd, or La on the Sr or Ca site were synthesized at 760–790°C in flowing N₂ and were oxidized in air at different temperatures. The samples were characterized by x-ray diffraction, transmission electron microscopy, thermogravimetry, chemical analysis, inelastic neutron scattering, and EXAFS spectroscopy. The oxidation kinetics of the solid solutions and the microstructure of the oxidation products were shown to correlate with the rare-earth content.__________Translated from Neorganicheskie Materialy, Vol. 41, No. 8, 2005, pp. 966–970.Original Russian Text Copyright © 2005 by Knotko, Garshev, Pulkin, Kirdyankin, Putlyaev.     

Synthesis and characterization of LiCo0.3−xGaxNi0.7O2 (x = 0, 0.05) as a cathode material for lithium ion battery

The single phase of LiCo_0.3−xGa_xNi_0.7O₂ (x = 0, 0.05) was synthesized by a sol–gel method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and electrochemical performance. The powders are homogeneous and have a good-layered structure. The synthesized LiCo_0.25Ga_0.05Ni_0.7O₂ exhibits better electrochemical performance with an initial discharge capacity of 180.0 mAh g⁻¹ and a capacity retention of 95.2% after 50 cycles between 2.8 and 4.4 V at 0.2C rate. The study on the structural evolution of the material during the cycling shows that Ga-doping improves the structure stability of LiCo_0.3Ni_0.7O₂ at ambient temperature and 55 °C. Meanwhile, Ga-doping not only suppresses the alternating current (AC) impedance of LiCo_0.3Ni_0.7O₂ but also promotes the Li⁺ diffusion in LiCo_0.3Ni_0.7O₂. Furthermore, thermal stability of the charged LiCo_0.25Ga_0.05Ni_0.7O₂ is improved, which may be attributed to the retard of O₂ evolution in LiCo_0.3Ni_0.7O₂ and the suppression of electrolyte oxidation during cycling by Ga-doping_.     

Superconducting transition temperatures in the Ru-1232 system, RuSr2(Gd1? x Ln x Ce1.8Sr0.2)Cu2O z (Ln = Sm, Dy, and Ho)

We have investigated effects of the lanthanide element Ln and the composition changes on the superconducting transition temperatureT _c in the Ru-1232 system, RuSr₂(Gd_1−x Ln _x Ce_1.8Sr_0.2)Cu₂O _z (Ln = Sm, Dy, and Ho). At first, in the case of the samples with Ln = Sm among almost the single 1232 phase samples, the values of the superconducting onset temperatureT _co are almost the same forx=0.00−0.15, and each of the lattice parametersa andc is almost constant. While, in each of the cases of the samples with Ln = Dy and Ho, the sample withx=0.05 shows the maximum values for both the superconducting onset temperatureT _co and the zero resistivity temperatureT _cz. Especially for the sample with Ln = Dy, the values ofT _co andT _cz are 18.5 and 6.5 K, respectively. These are higher than those of the mother sample of RuSr₂(GdCe_1.8Sr_0.2)Cu₂O _z . Moreover, from variations ofT _co, lattice parameters ofa andc in the RuSr₂(Gd_1−x Dy _x Ce_1.8Sr_0.2)Cu₂O _z system as a function of Dy contentx, the relationship between the superconducting transition temperature and the lattice parameters in the present system are investigated.     

Chemical solution deposition of YBa2Cu3O7−x coated conductors

At present, the development of superconducting YBa₂Cu₃O_7−x coated conductors attracts much attention due to their enormous application potential in electric power systems. Worldwide research is focused on the investigation and improvement of buffer materials and YBa₂Cu₃O_7−x superconducting properties as well as low-cost manufacturing processes in cooperation with industrial companies. Accordingly, chemical solution deposition has emerged as a highly competitive, versatile, and cost-effective technique for fabricating coated conductors of high performance. New chemical solution approaches are under development for buffer layer deposition. In order to achieve high critical current carrying YBa₂Cu₃O_7−x layers, the established trifluoroacetate route is favored. This paper reviews the most recent work on chemical solution deposition within the IFW Dresden while also considering achievements on this specific research topic worldwide.     

Structural, electrochemical and thermal properties of LiNi0.8−xCo0.2CexO2 as cathode materials for lithium ion batteries

A series of cathode materials for lithium ion batteries with the formula LiNi_0.8−xCo_0.2Ce_xO₂ (0 ≤ x ≤ 0.03) were synthesized by sol–gel method using citric acid as a chelating agent. The effects of cerium substitution on the structural, electrochemical and thermal properties of the cathode materials are investigated through X-ray diffraction (XRD), charge–discharge cycling, cyclic voltammogram (CV), electrochemical impedance spectroscopy (EIS) experiments and differential scanning calorimetry (DSC). Results show that the Ce substitution made the layered structure of materials more regular and less cation-ion mixing. An effective improved cycling performance is observed for cerium-doped cathode materials, which is interpreted to a significant suppression of phase transitions and charge-transfer impedance increasing during cycling. The thermal stability of cerium-doped materials is also improved, which can be attributed to its lower oxidation ability and enhanced structural stability at delithiated state.     

Chemical vapor deposition of the superconductor YBa2Cu3O7?x(s) from the gas phase

The deposition of the condensed phase YBa₂Cu₃O_7–x from a gas mixture composed of YCl₃, BaCl₂, Cu₃Cl₃, and Ar reacting with another consisting of O₂ and Ar in a flow system at elevated temperatures was investigated by means of the virtual equilibrium model, and the deposition rates were computed as a function of input gas stream compositions. The optimum growth conditions were identified.     

Structural, electronic and optical properties of Sn1−xSbxO2

The goal of this paper is to undertake a detailed first principle calculation of the structural, electronic and optical properties of Sn_1−xSb_xO₂. The results show that the stability of Sn_1−xSb_xO₂ in the full range of Sb content points to the probability of a continuous solid solution, where the increasing Sb content leads to volume expansion with different variation trends in the lattice constants. The increase of Sb concentration in the semiconductor–metal–semimetal transition occurs in consonance with the corresponding changes in its structural, electronic and optical properties. Two competing mechanisms play essential roles in this transition, namely; the many body effect and the atom disorder. Our calculations concur with previous X-ray diffraction, sheet resistance, resistivity and optical parameters detections. The studies present a practical way of tailoring the physical behaviors of Sn_1−xSb_xO₂ through the alloying technique.     

Interfacial fracture for TiN/SiNx nano-multilayer coatings on Si(1 1 1) characterized by nanoindentation experiments

Fracture behavior for TiN/SiN_x nano-multilayer coatings on Si(1 1 1) substrates, deposited using magnetron sputtering Ti and Si, is characterized by nanoindentation experiments, and the morphologies of the indentations are revealed by scanning electron microscopy, along with in situ atomic force microscopy (AFM) in nanoindentation experiments. During nanoindentation experiments, under the condition that the displacement limit mode is used and a strain rate is kept at 0.05/s, an interfacial (between the coating and substrate) fracture is observed as the maximum indenter displacement into the coating reaches 2500 nm, and the corresponding unloading segment in the load–displacement curve shows an obvious discontinuity. This discontinuity is attributed to the rebound of the detached film during unloading. The interfacial fracture toughness for TiN/SiN_x nano-multilayer coating on Si(1 1 1), which is strongly dependent on the preferred orientation for the TiN layer as well as the interfaces between TiN and SiN_x layer in the multilayer stack, is calculated.     

Structural study of Si1 − xGex nanocrystals embedded in SiO2 films

We have investigated the structural properties of Si_1 − xGe_x nanocrystals formed in an amorphous SiO₂ matrix by magnetron sputtering deposition. The influence of deposition parameters on nanocrystal size, shape, arrangement and internal structure was examined by X-ray diffraction, Raman spectroscopy, grazing incidence small angle X-ray scattering, and high resolution transmission electron microscopy. We found conditions for the formation of spherical Si_1 − xGe_x nanocrystals with average sizes between 3 and 13 nm, uniformly distributed in the matrix. In addition we have shown the influence of deposition parameters on average nanocrystal size and Ge content x.     

High-pressure Bi(Mg1 ? xZnx)1/2Ti1/2O3 perovskite solid solutions

We report the preparation of Bi(Mg_{1 − x} Zn _x )_1/2Ti_1/2O₃ ceramics at a pressure of 6 GPa and temperatures from 1370 to 1570 K. In the composition ranges 0 < x < 0.5 and 0.8 < x < 1, the ceramics consist of perovskite solid solutions. The solid solutions with x < 0.5 have an orthorhombic structure (sp. gr. Pnnm), and those with x > 0.7 have a tetragonal structure (sp. gr. P4mn). On heating at atmospheric pressure, the solid solutions with 0.1 < x < 0.5 undergo an irreversible orthorhombic-to-rhombohedral (sp. gr. R3c) phase transition, accompanied by heat absorption and an increase in specific volume. The transition temperature decreases with increasing x. The reduced perovskite cell parameter of the solid solutions increases linearly with x. The Curie temperature of the rhombohedral solid solutions exceeds the decomposition temperature of the perovskite phase.     

Growth and characterization of Bi2Sr2Ca1Cu2O8+x single crystals

High-quality single crystals are well suited to the investigation of some intrinsic material properties. A modified Bridgman method using a sharp temperature gradient (300°C/cm) was used to grow Bi₂Sr₂Ca₁Cu₂O_8+x single crystals. Although the samples were contained in alumina ampoules, no aluminium contamination of the samples was detected. Blade-shaped crystals up to 7–8 mm length and 3–4 mm width could be grown by this method, although extraction from the matrix was difficult. Electron diffraction patterns of the [001] zone axis revealed a high degree of crystallinity. The narrowness of the superconducting transition temperature, as determined by ac susceptibility, also suggests the existence of well-formed crystalline domains. In order to determine the relative orientation of the crystalline domains, electron channeling patterns were recorded from several consecutive growth steps from a fracture surface. The poor contrast of these and Kikuchi patterns suggests the presence of a stacking structure. The results showed a [100] growth direction and (001) cleavage plane. Reversible oxygen loss at the peritectic decomposition temperature of 863°C was observed. Knoop indentation measurements showed that the crystals were quite soft, having a microhardness of 0.44 GPa.     

Correlation of magnetic properties to oxygen and potassium stoichiometry in single-crystal Ba1?xKxBiO3?y

Recent theoretical calculations have suggested the coupling of electrons to high-energy oxygen phonons as an explanation of superconductivity in the Ba_1–x K _x BiO_3–y system. We have synthesized high-quality single crystals of the material and have examined the behaviors of critical field and critical current parameters as a function of changes in the oxygen content and in the Ba/K ratio. We have determined, via positron lifetime spectroscopy and singlecrystal X-ray measurements, that the oxygen stoichiometry in this system can be varied without significant impact on the metal atom sublattice. These results facilitate an investigation of the dependence of critical parameters on dopant and defect levels in this system.     

Structural and mechanical characterization of BCxNy thin films deposited by pulsed reactive magnetron sputtering

BC_xN_y thin films deposited at 250 °C by pulsed reactive magnetron sputtering of a B₄C target in an Ar/N₂ plasma were studied by elastic recoil detection analysis, Fourier transform infrared, Raman, and photoelectron spectroscopy, electron microscopy, and nanoindentation. In the concentration range of 6% to 100% N₂ in the sputter plasma the segregation into nanocrystalline hexagonal boron nitride and amorphous sp² carbon is the dominant process during the film growth. The stoichiometric ratio and structural details of the major phases depend on the N₂ concentration in the plasma and have significant influence on the Young′s modulus and the elastic recovery of the BC_xN_y thin films.     

Relationship between photoluminescence and structural properties of the sputtered Zn1−xCdxO films on Si substrates

Zn_1−xCd_xO (x=0.2, 0.4) alloyed crystal thin films have been deposited on Si(1 1 1) substrates at different temperatures by using dc reactive magnetron sputtering technique. The Zn_1−xCd_xO films are of highly (0 0 2)-preferred orientation possessing the hexagonal wurtzite structure of pure ZnO. At 450 °C, the films have better crystal quality and photoluminescent characteristics. For the films with x=0.2 and 0.4, the corresponding near-band-edge (NBE) energies are 3.10 and 3.03 eV, respectively, both have red-shifts compared with that of ZnO (3.30 eV). For the substrate temperatures lower or higher than 450 °C, the other NBE emission peak appears, the X-ray diffraction intensity of (0 0 2) peak decreases and the related FWHM increases. With the Cd addition up to x=0.4 both the XRD and PL intensity of the Zn_1−xCd_xO films decrease sharply in comparison with x=0.2.