Superconducting Properties of Iodine-Intercalated Bi<Subscript>2</Subscript>Sr<Subscript>2</Subscript>Ca<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>10+<Emphasis Type="Italic">x</Emphasis></Subscript>

The superconducting properties of iodine-intercalated high-temperature superconducting Bi₂Sr₂Ca₂Cu₃O_10+x phase (Bi-2223) were systematically studied. It was found that for samples containing a significant amount of Bi₂Sr₂CaCu₂O_8+x , iodine intercalation results in the dramatic decrease of the inter-granular critical current density, as well as a significant decrease of the critical temperature (T _c), the critical current density in the grains (J _cg), and of the amount of Bi-2223. For samples with a large amount of Bi-2223, T _c changes insignificantly, whereas J _cg can even increase. We argue that the different behavior of the superconducting parameters is the result of various oxygen concentrations, and we explain the effect of iodine intercalation based on the parabolic dependence between T _c and the number of holes per CuO₂ layer. The H(T) curves (determined from the peak position in the loss signal of ac susceptibility) for intercalated samples deviate significantly from the quasi 2D-like behavior, pointing toward an enhancement of the 3D fluctuations of vortices. For the change in the values and dimensionality of the flux pinning in the process of the intercalation, we attempted a qualitative explanation based on the models proposed in literature.     

Enhanced Superconducting Properties of Air-Processed GdBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7-δ</Subscript> Single Domains with BaCO<Subscript>3</Subscript>/BaCuO<Subscript>2−<Emphasis Type="Italic">x</Emphasis></Subscript> Addition

Single domain GdBa₂Cu_7-δ (Gd123) bulk superconductors were fabricated in air by top-seeding melt-texture growth. Performance of the air-processed Gd123 was successfully enhanced by addition of both BaCO₃ and BaCuO_2−x , which suppress the formation of Gd_1+x Ba_2−x Cu₃O_7-δ solid solutions. The optimum doping amount ranges from 0.05 to 0.15, M BaCO₃ and 0.05 to 0.1, M BaCuO_2−x per molar Gd123. The distribution of the second phase particles was observed by scanning electron microscopy. A narrow band formed by Gd₂BaCuO₅ particle concentration appeared around the seeding zone in both a–b plane and c-growth sector in Gd123 single grain. Trapped magnetic field density reached 0.67, T for sample with 24 mm in diameter and 8, mm in thickness and a high critical current density J _c up to 91,200, A/cm² was achieved at 77, K under self-field.     

Spectral parameters of Nd<Superscript>3+</Superscript> ion in Sr<Subscript>6</Subscript>NdSc(BO<Subscript>3</Subscript>)<Subscript>6</Subscript> crystal

The spectroscopic study of Nd³⁺ in Sr₆NdSc(BO₃)₆ crystal had been performed. Based on the Judd-Ofelt theory to analyze the optical strengths measured in absorption spectra, the following spectral parameters were obtained: intensity parameters are ₂ = 1.108 × 10^–20 cm², ₄ = 2.884 × 10^–20 cm², ₆ = 3.085 × 10^–20 cm², the radiative lifetime is 385 s, the quantum efficiency is 12.5%. The fluorescence branch ratios were calculated: ₁ = 0.423, ₂ = 0.482, ₃ = 0.092, ₄ = 0.005.     

Spectral parameters of Er<Superscript>3+</Superscript> ion in Yb<Superscript>3+</Superscript>/Er<Superscript>3+</Superscript>:KY(WO<Subscript>4</Subscript>)<Subscript>2</Subscript> crystal

The spectral parameters of Er³⁺ in Yb³⁺/Er³⁺:KY(WO₄)₂ crystal with space group C2/c have been investigated based on Judd-Ofelt theory. The spectral parameters were obtained: the intensity parameters are: ₂ = 6.33 × 10^–20 cm², ₄ = 1.35 × 10^–20 cm², ₆ = 1.90 × 10^–20 cm². The radiative lifetime and the fluorescence branch ratios were calculated. The emission cross section _e (at 1536 nm) is 2.0 × 10^–21 cm².     

Morphology and conductivity studies of a new solid polymer electrolyte: (PEG)<Subscript>x</Subscript>LiClO<Subscript>4</Subscript>

A new solid polymer electrolyte, (PEG)_xLiClO₄, consisting of poly(ethylene)glycol of molecular weight 2000 and LiClO₄ was prepared and characterized using XRD, IR, SEM, DSC, NMR and impedance spectroscopy techniques. XRD and IR results show the formation of the polymer-salt complex. The samples with higher salt concentration are softer, less opaque and less smooth compared to the low salt concentration samples. DSC studies show an increase in the glass transition temperature and a decrease in the degree of crystallinity with increase in the salt concentration. Melting temperature of SPEs is lower than the pure PEG 2000. Room temperature¹H and⁷Li NMR studies were also carried out for the (PEG)_xLiClO₄ system. The¹H linewidth decreases as salt concentration increases in a similar way to the decrease in the crystalline fraction and reaches a minimum at aroundx = 46 and then increases.⁷Li linewidth was found to decrease first and then to slightly increase after reaching a minimum atx = 46 signifying the highest mobility of Li ions for this composition. Room temperature conductivity first increases with salt concentration and reaches a maximum value (σ = 7.3 × 10⁻⁷ S/cm) atx = 46 and subsequently decreases. The temperature dependence of the conductivity can be fitted to the Arrhenius and the VTF equations in different temperature ranges. The ionic conductivity reaches a high value of ∼10 ⁻⁴S/cm close to the melting temperature.     

Preparation of Y<Subscript>2</Subscript>O<Subscript>3</Subscript> Buffer Layer on LaAlO<Subscript>3</Subscript> Substrate by TFA-MOD Method

Chemical solution deposition is a promising technique for fabrication of high-temperature superconducting films and oxide buffer layers due to its reproducibility and low cost. In this work, Y₂O₃ buffer layers were prepared on (100) LaAlO₃ substrates by mental organic deposition method using trifluoroacetate. The resulting Y₂O₃ films crystallized as a single phase at 900°C and showed a low degree ofc-axis orientation. The scanning electron micrography showed that the surface of the films was smooth with a uniform grain size of approximately 10 nm.     

Epitaxial Growth of CeO<Subscript>2</Subscript>/YSZ/CeO<Subscript>2</Subscript> Buffer Layers on Textured Ni Substrates for YBCO Conductors

CeO₂/YSZ/CeO₂ buffer layers were deposited on textured Ni substrates byin situ pulsed laser deposition. The out-of-plane texture and in-plane texture of the buffer layers were characterized by X-ray diffraction ω-scans and ϕ-scans. Using this CeO₂/YSZ/CeO₂ architecture as the buffer layers, high quality YBCO films with a zero-resistanceT _c about 90 K and a self-field critical current densitiesJ _c above 10⁶ A/cm² at 77 K can be obtained on Ni substrates.     

Impedance analysis of Pb<Subscript>2</Subscript>Sb<Subscript>3</Subscript>LaTi<Subscript>5</Subscript>O<Subscript>18</Subscript> ceramic

Polycrystalline sample of Pb₂Sb₃LaTi₅O₁₈, a member of tungsten- bronze (TB family, was prepared using a high temperature solid- state reaction technique. XRD analysis indicated the formation of a single-phase orthorhombic structure. The dielectric studies revealed the diffuse phase transition and the transition temperature was found to be at 52° C. Impedance plots were used as tools to analyse the sample behaviour as a function of frequency. Cole-Cole plots showed Debye relaxation. The activation energy was estimated to be 0·634 eV from the temperature variation of d.c. conductivity. The nature of variation of d.c. conductivity with temperature suggested NTCR behaviour.     

Compatibility of RuO<Subscript>2</Subscript> electrodes with PZT ceramics

Because of its high electrical conductivity and good diffusion barrier properties ruthenium dioxide (RuO₂) is a good electrode material for use with ferroelectric lead zirconate-titanate (PZT) solid solutions. Under certain conditions, RuO₂ can react with PZT to form lead ruthenate (Pb₂Ru₂O_6·5) during processing at elevated temperatures resulting in lead depletion from PZT. The standard Gibbs energies of formation of RuO₂ and Pb₂Ru₂O_6·5 and activities of components of the PZT solid solution have been determined recently. Using this data along with older thermodynamic information on PbZrO₃ and PbTiO₃, the stability domain of Pb₂Ru₂O_6·5 is computed as a function of PZT composition, temperature and oxygen partial pressure in the gas phase. The results show PbZrO₃-rich compositions are more prone to react with RuO₂ at all temperatures. Increasing temperature and decreasing oxygen partial pressure suppress the reaction. Graphically displayed are the reaction zones as a function of oxygen partial pressure and PZT composition at temperatures 973,1173 and 1373 K.     

Nano Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Induced Fluxoid Jumps and Low Field Enhanced Critical Current Density in MgB<Subscript>2</Subscript> Superconductor

Nano particle of Fe₃O₄ (nFe₃O₄) up to 6 at% were doped in the superconducting MgB₂ samples. Despite the strong ferromagnetic nature of Fe₃O₄, both the ac susceptibility and the resistivity measurements show that up to 4 at% of Fe₃O₄, T _c =38 K is not changed, whereas for 6% T _c decreases by 6 K. This indicates that a low concentration of Fe does not substitute either the Mg or B sites and probably occupies the intergrain spaces. For 0.5% doped Fe₃O₄, an increase in J _c with respect to the pure MgB₂ samples is observed in the lower field and temperature regions (H<2 T and 20 K) indicating an enhanced flux pinning and the magnetic activation, i.e., the interaction between the magnetic dipole of Fe ion and the vortices is weak in comparison to the effective pinning potential. Whereas, at H>2 T, J _c of the doped samples is always less than that of MgB₂, and the activation is dominant in comparison with the effective pinning potential provided by the doping. Flux jumps are observed in lower T and H regions for the samples doped up to 1% nFe₃O₄ only. Magnetization plots of higher Fe content samples exhibited clear paramagnetic background. Mossbauer measurements for the higher (4, 6 at%) nFe₃O₄ doped MgB₂ samples show that at RT, the hyperfine field for both samples is ∼100 kOe and ∼120 kOe at 90 K. This means that the nFe₃O₄ particles decompose and form possibly an intermetallic Fe-B phase in the matrix.     

Microwave Response of Perfect YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−<Emphasis Type="Italic">x</Emphasis></Subscript> Thin Films Deposited on CeO<Subscript>2</Subscript>-Buffered Saphire: A Probe for Pairing Symmetry

Microwave surface impedance, Z _s(T), of epitaxial YBCO thin films deposited on CeO₂-buffered sapphire substrates, was measured at several discrete frequencies within the range 5–134 GHz by use of coplanar resonator and end-plate cavity resonator techniques. The main features of obtained experimental results are as follows: (i) surface resistance R _s(T) at low temperatures obeys the exponential law: R _s(T) = R _res+R ₀⋅exp [−δ/T] with a small gap δ value (δ≈ 0.7 T _c); (ii) the most perfect quasi-single-crystalline films reveal a distinct two-peak structure of R _s(T) dependence, which is not observable in films with a less ordered crystal structure. These features are believed to reveal some intrinsic electron properties of such films, namely: (i) mixed (d+is) type symmetry of electron pairing, and (ii) dominant role of extended c-oriented defects (e.g., edge dislocation arrays or twin planes) in quasiparticles scattering for the most perfect films, which demonstrate the two-peak anomalous R _s(T) behavior.     

Li-storage and cycling properties of spinel,CdFe<Subscript>2</Subscript>O<Subscript>4</Subscript>, as an anode for lithium ion batteries

Cadmium ferrite, CdFe₂O₄, is synthesized by urea combustion method followed by calcination at 900°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and selected area electron diffraction (SAED) techniques. The Li-storage and cycling behaviour are examined by galvanostatic cycling, cyclic voltammetry (CV) and impedance spectroscopy in the voltage range, 0·005–3·0 V vs Li at room temperature. CdFe₂O₄ shows a first cycle reversible capacity of 870 (± 10) mAhg⁻¹ at 0·07C-rate, but the capacity degrades at 4 mAhg⁻¹ per cycle and retains only 680 (± 10) mAhg⁻¹ after 50 cycles. Heat-treated electrode of CdFe₂O₄ (300°C; 12 h, Ar) shows a significantly improved cycling performance under the above cycling conditions and a stable capacity of 810 (± 10) mAhg⁻¹ corresponding to 8·7 moles of Li per mole of CdFe₂O₄ (vs theoretical, 9·0 moles of Li) is maintained up to 60 cycles, with a coulombic efficiency, 96–98%. Rate capability of heat-treated CdFe₂O₄ is also good: reversible capacities of 650 (± 10) and 450 (± 10) mAhg⁻¹ at 0·5 C and 1·4 C (1 C = 840 mAg⁻¹) are observed, respectively. The reasons for the improved cycling performance are discussed. From the CV data in 2–15 cycles, the average discharge potential is measured to be ∼0·9 V, whereas the charge potential is ∼2·1 V. Based on the galvanostatic and CV data, ex situ-XRD, -TEM and -SAED studies, a reaction mechanism is proposed. The impedance parameters as a function of voltage during the 1st cycle have been evaluated and interpreted. Dedicated to Prof. C N R Rao on his 75th birthday, and his contributions to science for the past 56 years     

Crystallization kinetics of amorphous Te<Subscript>x</Subscript>(Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript>)<Subscript>1-<Emphasis Type="Italic">x</Emphasis></Subscript> glasses

The activation energy plays a dominant role in deciding the utility of the material for the specific purpose—here storage. The dependence of the peak temperature of crystallization (T _p)on the composition and heating rate (β) has been studied here. From the heating rate dependence,T _p the activation energy for crystallization (E _c)has been evaluated. The activation energy,E _ccalculated using three different approaches is found to decrease with the increase in Bi content. This analysis helps in finding the suitability of an alloy to be used in phase transition optical memories/switches. The results have been analysed using Kissinger’s equation for non-isothermal crystallization of materials.     

Promoting effect of CeO<Subscript>2</Subscript> on cyclohexanol conversion over CeO<Subscript>2</Subscript>-ZnO mixed oxide materials prepared by amorphous citrate process

CeO₂-ZnO materials were prepared by amorphous citrate process and characterized by TGA, XRD, UV-DRS and surface area measurements. TGA showed that the citrate precursors decompose in the range 350–550°C producing CeO₂-containing catalytic materials. XRD and DRS results indicated the formation of well-dispersed interstitialZn _xCe⁴⁺ _1−2x Ce³⁺ _2x O₂ solid solution on ZnO matrix. Addition of CeO₂ to ZnO produced high surface area mixed oxide materials in citrate method. Cyclohexanol conversion reaction was carried out on these catalytic materials to investigate the effect of rare earth oxide on the activity and selectivity. It was found that CeO₂ promotes the activity of ZnO without affecting the selectivity to cyclohexanone significantly. The factors such as reaction temperature and WHSV have turned out to be important for cyclohexanol conversion over CeO₂-containing ZnO catalyst materials.     

Interfacial microstructure and strength of diffusion brazed joint between Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiC and 9Cr1MoV steel

Joining of composite, Al₂O₃-TiC, with heat-resistant 9Cr1MoV steel, was carried out by diffusion brazing technology, using a combination of Ti, Cu and Ti as multi-interlayer. The interfacial strength was measured by shear testing and the result was explained by the fracture morphology. Microstructural characterization of the Al₂O₃-TiC/9Cr1MoV joint was investigated by X-ray diffraction (XRD) and scanning electron microscope (SEM) with energy-dispersion spectroscopy (EDS). The results indicate that a Al₂O₃-TiC/9Cr1MoV joint with a shear strength of 122 MPa can be obtained by controlling heating temperature at 1130°C for 60 min with a pressure of 12 MPa. Multi-interlayer Ti/Cu/Ti was fused fully and diffusion occurred to produce interfacial layer between Al₂O₃-TiC and 9Cr1MoV steel. The total thickness of the interfacial layer is about 100 μm and Ti₃AlC₂, TiC, Cu and Fe₂Ti are found to occur in the interface layer.     

Ethanol gas sensing properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-doped ZnO thick film resistors

The characterization and ethanol gas sensing properties of pure and doped ZnO thick films were investigated. Thick films of pure zinc oxide were prepared by the screen printing technique. Pure zinc oxide was almost insensitive to ethanol. Thick films of Al₂O₃ (1 wt%) doped ZnO were observed to be highly sensitive to ethanol vapours at 300°C. Aluminium oxide grains dispersed around ZnO grains would result into the barrier height among the grains. Upon exposure of ethanol vapours, the barrier height would decrease greatly leading to drastic increase in conductance. It is reported that the surface misfits, calcination temperature and operating temperature can affect the microstructure and gas sensing performance of the sensor. The efforts are, therefore, made to create surface misfits by doping Al₂O₃ into zinc oxide and to study the sensing performance. The quick response and fast recovery are the main features of this sensor. The effects of microstructure and additive concentration on the gas response, selectivity, response time and recovery time of the sensor in the presence of ethanol vapours were studied and discussed.     

Superconducting YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7−δ</Subscript> thick film (T<Subscript>c</Subscript>(0) = 92 K) on a newly developed perovskite ceramic substrate

A complex perovskite oxide, YbBa₂NbO₆, as a non-reacting substrate for YBa₂Cu₃O_7-° super-conducting film has been developed. The dielectric constant and loss factor values of the material are in the range suitable for its use as substrate for microwave applications. A YBa₂Cu₃O_7−δ superconducting thick film dip coated on YbBa₂NbO₆ substrate gave a T_c (0) of 92 K and current density of ∼ 1.3 × 10⁴ A cm⁻².     

Crystal Electric Field Excitations in the Non-Fermy Liquid Compound YbRh<Subscript>2</Subscript>Si<Subscript>2</Subscript>

We have calculated the crystalline electric field (CEF) splitting of the energy levels of Yb³⁺ (4f¹³) in the clean Yb-based heavy fermion compound YbRh₂Si₂. The data of inelastic neutron scattering and electron spin resonance measurements in YbRh₂Si₂, together with relevant structural, thermodynamic, and magnetic properties, were used as input in the calculations of the possible CEF level scheme in this non-Fermi-liquid compound. Two possible sets of the CEF parameters with the Γ₆ or Γ₇ ground-state symmetry are discussed. PACS: 71.27.+a; 75.20.Hr; 76.30.−v.     

Effects of talc and clay addition on pressureless sintering of porous Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics

Porous Si₃N₄ ceramics were successfully synthesized using cheaper talc and clay as sintering additives by pressureless sintering technology and the microstructure and mechanical properties of the ceramics were also investigated. The results indicated that the ceramics consisted of elongated β-Si₃N₄ and small Si₂N₂O grains. Fibrous β-Si₃N₄ grains developed in the porous microstructure, and the grain morphology and size were affected by different sintering conditions. Adding 20% talc and clay sintered at 1700°C for 2 h, the porous Si₃N₄ ceramics were obtained with excellent properties. The final mechanical properties of the Si₃N₄ ceramics were as follows: porosity, P ₀ = 45·39%; density, ρ = 1·663·g·cm⁻³; flexural strength, σ _b (average) = 131·59 MPa; Weibull modulus, m = 16·20.     

Effect of sintering temperature on structural and electrical properties of gadolinium doped ceria (Ce<Subscript>0·9</Subscript>Gd<Subscript>0·1</Subscript>O<Subscript>1·95</Subscript>)

Gadolinium doped ceria oxide is one of the promising materials as an electrolyte for IT-SOFCs. Ce_0·9Gd_0·1O_1·95 (GDC10) powder was prepared by solid state reaction and sintered at 1473 K, 1573 K, 1673 K and 1773 K. All samples were studied using X-ray diffraction, scanning electron micrograph and d.c. conductivity measurement. The crystallinity and surface morphology of the samples improved with sintering temperature. Further, the electrical conductivity measurement indicated that the conduction mechanism is mainly ionic. The conductivity of samples sintered at 1673 K and 1773 K at 800°C are of the order of 0·1 S-cm⁻¹. The activation energies decreased from 1·25–0·82 eV with increase in sintering temperature.