Production of bscco bulk high <Emphasis Type="Italic">T</Emphasis><Subscript>c</Subscript> superconductors by sol-gel method and their characterization by ftir and XRD techniques

The production of bulk high T _c superconducting phase (2223) by EDTA-gel (ethylenediaminetetraacetic acid) techniques has been investigated. It is shown that close control of pH is necessary for the production of a well-complexed precursor which allows subsequent decomposition in two stages at 300 and 800°C. The problem of carbonate formation was investigated experimentally and solved. Precursors are characterised by Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) and the sintering behaviour was monitored by dilatometry. At least three different phases Bi₂Sr₂Ca_x−1Cu_xO_8+y (BSCCO); where x=1, 2, 3 were identified within superconducting pellets using XRD, named as Bi₂Sr₂CuO₇ (2201), Bi₂Sr₂CaCu₂O₉ (2212) and Bi₂Sr₂Ca₃O₁₀ (2223). The superconducting properties of the sintered samples were studied by vibrating sample magnetometer (VSM). Transition to a superconducting state around 80 K appeared in samples (sintered at 845°C) containing the Bi₂Sr₂Ca₁Cu₂O_y (2212) phase. Liquid phase sintering of the samples aided the formation of Bi₂Sr₂Ca₂Cu₃O_x (2223) phase at high temperature (860°C), which showed a superconducting transition temperature of 108 K.     

Impact of Pb substitution on the formation of high <Emphasis Type="Italic">T</Emphasis><Subscript>c</Subscript> superconducting phase in BSCCO system derived through sol-gel process

Sol-gel process was employed to synthesize the Pb-BSCCO system having general composition Bi_2−xPb_xSr₂Ca₂Cu₃O_10−δ, where x=0.2, 0.4 and 0.8. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), dilatometry and vibrating sample magnetometer (VSM) were employed to study the materials produced at different stages. Two-stage heating firstly at 300 and then 800°C was adopted in order to avoid the burning of the materials and formation of carbonates. The carbonate formation was avoided by heating the materials firstly at 300°C for 2 h and without intermediate cooling moved to the furnace having temperature 800°C and hold for 2 h. The sintering behaviour of samples was studied by dilatometry and the results revealed that the sample having x=0.4 was stabled up to a temperature of 700°C while samples having x=0.2 and 0.8 to a temperature of 625°C. The maximum shrinkage was observed at 850°C in all the samples. On the basis of dilatometry results, the samples were sintered at 845°C for 60 h to observe the superconducting phases. The highest volume fraction of high superconducting phase (2223) was noticed in the sample containing x=0.4 having onset T _c=110 K.     

Effect of atmospheric pressure on the phase transitions of α,α-trehalose dihydrate DTA study of the dehydration behavior in open systems

The phase transitions of α,α-trehalose dihydrate (T _h) were investigated by either differential thermal analysis (DTA) with an in-house apparatus of variable-pressure type equipped with an open sample holder or commercially available TG (thermal gravimetry)-DTA apparatus for comparison under the same experimental conditions as to the heating rate (2°C min⁻¹), the type of pan (open), and the particle size of T _h (63 μm). The former DTA measurements were carried out under five different total pressures, 101, 75, 61, 48 and 35 kPa, which provided quite helpful information necessary for confirmative assignments of the endothermic peaks due to either melting or dehydration of T _h. The usage of largely different amount of T _h, 126 and 14 mg for the DTA and TG-DTA measurements respectively, led to their different DTA traces, showing that there were largely different extents of the influence by the measured sample surface exposed to the surrounding atmosphere on its dehydration behavior. In addition the high thermal sensitivity achieved with such mass of T _h gave rise to an interesting discovery of an unidentified thermal event at 92°C prior to either melting or dehydration of T _h.     

The formation of superconducting oxide phases in the (Bi,Pb)−Sr−Ca−Cu−O System

The crystallization mechanism of superconducting phases in the (Bi,Pb)?Sr?Ca?Cu?O system was determined on the basis of the results of DTA, DTG and TG studies, supplemented by X-ray examination of ceramic powders obtained by the sol-gel method. It has been demonstrated that the factor determining the formation of superconducting phases: Bi₂Sr₂CaCu₂O_x (low-T _c ) and Bi₂Sr₂Ca₂Cu₃O_x (high-T _c ) is the kinetics of reaction of calcium and strontium carbonates with molten CuBi₂O₄. As a result of the reaction of the bimetallic compound CuBi₂O₄ with SrCO₃ in the liquid phase the compound Bi₂Sr₂CuO₆ is formed. This compound, reacting with calcium and copper oxides, yields superconducting phases: the low-T _c and the high-T _c phase. It has been also observed that an increase in the volume fraction of high-T _c phase in powder subjected to thermal treatment takes place probably due to the repeated disproportionation of low-T _c phase and its repeated synthesis from Bi₂Sr₂CuO₆, CuO and CaO.     

The effect of composition of parenteral solution on the thermal resistance of Bacillus stearothermophilus and Bacillus subtilis spores

Large-volume parenteral solutions were submitted to heat treatments after being inoculated with Bacillus stearothermophilus ATCC 7953 (T _r =121°C) and Bacillus subtilis ATCC 9372 (T _r =104.5°C) spores. The average decimal reduction time for B. stearothermophilus ranged from a D _121°C value of 1.31 to 3.14 min, in glucophysiologic and Ringer’s solutions respectively. For B. subtilis, D _104.5°C value increased from 0.69 to 1.37 min, in Ringer’s (pH=5.91) and 50% glucose (pH 3.05) solutions respectively. The z value ranged from 7.95°C (20% mannitol solution) to 13.14°C (50% glucose solution), corresponding to an activation energy (Ea) of 81.48 and 49.30 kcal/mol, respectively.     

Fabrication and properties of xBiFeO3-(1 − x)Bi4Ti3O12 system by sol–gel process

The thin films of mixture of xBiFeO₃-(1 − x)Bi₄Ti₃O₁₂ (x = 0.4, 0.5, and 0.6) system were prepared by a sol–gel process. The thicknesses of the thin films were 540, 500, and 570 nm, respectively. The crystal structure of all thin films annealed at 650 °C was analyzed by X-ray diffraction. It was found that the thin films at x = 0.4 and 0.5 mainly consisted of a Bi₄Ti₃O₁₂ phase while Bi₅Ti₃FeO₁₅ was the major phase of the thin film at x = 0.6. The thin film (x = 0.6) showed better ferroelectric properties in remnant polarization and polarization fatigue than those observed in the thin films (x = 0.4 and 0.5). The values of remnant polarization 2P _r and coercive field 2E c of the thin film at x = 0.6 were 36 μC/cm² and 192 kV/cm at an applied electric field of 260 kV/cm, respectively. There was almost no polarization fatigue up to 10¹⁰ switching cycles. Also weak ferromagnetism was observed in the thin film at x = 0.6.     

Analysis of structural and magnetic phase transition behaviors of La1−xSrxCrO3 by measurement of heat capacity with thermal relaxation technique

The heat capacity, C_p, of the La_1−xSr_xCrO₃ system and its temperature dependence have been measured by a thermal relaxation technique. Both structural and magnetic phase transitions were detected at temperatures that can be surmised from the phase diagram proposed in previous studies. The observed variation in enthalpy after the first-order structural phase transition, ΔH, showed agreement with those measured by differential scanning calorimetry (DSC). A decrease in the variation in C_p in the second-order magnetic phase transition, ΔC_p, with an increase in Sr content was detected, which can be attributed to a decrease in electronic spin configuration entropy with an increase in Sr content. In the dependence of ΔC_p on Sr content, a bending point was also observed at x  0.12, at which the crystal system varies from an orthorhombic-distorted perovskite structure to a rhombohedral-distorted perovskite structure.     

Effect of strontium substitution on the activity of La2?xSrxNiO4 (x = 0.0–1.2) in NO decomposition

The aim of this work is to study the effect of Sr substitution on the redox properties and catalytic activity of La_2−x Sr _x NiO₄ (x = 0.0–1.2) for NO decomposition. Results suggest that the x = 0.6 sample shows the highest activity. The characterization (TPD, TPR, etc.) of samples indicates that the x = 0.6 sample possesses suitable abilities in both oxidation and reduction, which facilitates the proceeding of oxygen desorption and NO adsorption. At temperature below 700°C, the oxygen desorption is difficult, and is the rate-determining step of NO decomposition. With the increase of reaction temperature (T > 700°C), the oxygen desorption is favorable and, the active adsorption of NO on the active site (NO + V _o + Ni²⁺ → NO⁻-Ni³⁺) turns out to be the rate-determining step. The existence of oxygen vacancy is the prerequisite condition for NO decomposition, but its quantity does not relate much to the activity. Supported by the National Hi-Tech Research and Development Program of China (863 Program)(Grant No. 2004CB 719502) and the National Natural Science Foundation of China (Grant No. 20177022)     

The influence of film thickness and process temperature on <Emphasis Type="Italic">c</Emphasis>-axis orientation of Bi<Subscript>3</Subscript>TiTaO<Subscript>9</Subscript> thin films

Bi-layered ferroelectric Bi₃TiTaO₉ (BTT) thin films with different thickness (ranging from 100 to 400 nm) were successfully fabricated on Pt(111)/TiO₂/SiO₂/(100)Si substrates using chemical solution deposition (CSD) technique at different annealing temperatures. The c-axis orientation of the films was affected by film thickness and process temperature. The thinner the film and the higher the process temperature, the higher the c-axis orientation. With the increase of film thickness, the stress decreased but the film roughness increased, which led to the decrease of c-axis orientation of films. BTT films annealed at 800°C were found to have much improved remament polarization (P _r ) than that of films annealed at 650 and 750°C. The P _r and coercive field (E _c ) values were measured to be 2 μC/cm² and 100 kV/cm, respectively. BTT films showed well-defined ferroelectric properties with grain size larger than 100 nm.     

Following the crystallisation of Bi2Mo2O9 catalyst by combined XRD/QuEXAFS

The formation ofβ-phase Bi₂Mo₂O₉ catalyst from a precursor precipitate has been studied using thein situ combined XRD/QuEXAFS technique and DSC during calcination. Accordingly the precursor was observed to undergo a number of changes in both the molybdenum (VI) coordination and long-range ordering during this heating. Initially the two other forms of bismuth molybdate (α-andγ-phases) were observed to form from the poorly crystalline precursor at about 230°C, however, theβ-phase eventually crystallised after prolonged heating at 560°C. Dedicated to Professor C N R Rao on his 70th birthday     

Thermal behavior of trehalose dihydrate (T h) and β-anhydrous trehalose (T β) by in-situ laboratory parallel-beam X-ray powder diffraction

Thermal behaviors of trehalose dihydrate (T _h) and β-anhydrous trehalose (T _β) have been investigated by in-situ laboratory parallel-beam X-ray powder diffraction. Data indicate that both phases show essentially the same volume expansion but expansion of the anhydrous form is markedly anisotropic due to the features of the hydrogen-bond network. Under the present experimental conditions, dehydration starts at 66 °C and within the 75 < T < 114 °C the presence of the T _α anhydrous polymorphic form has been detected.     

Intracellular release of recombinant green fluorescent protein (gfp uv ) from Escherichia coli

The recombinant green fluorescent protein (gfp _uv ) was expressed by Escherichia coli DH5-α cells transformed with the plasmid pGFPuv. The gfp _uv was selectively permeabilized from the cells in buffer solution (25 mM Tris-HCl, pH 8.0), after freezing (−70°C for 15 h), by four freeze (−20°C)/thaw cycles interlaid by sonication. The average content of released gfp _uv (experiment 2) was 7.76, 34.58, 39.38, 12.90, and 5.38%, for the initial freezing (−70°C) and the first, second, third and fourth freeze/thaw cycles, respectively. Superfusion on freezing was observed between −11°C and −14°C, after which it reached −20°C at 0.83°C/min.     

Thermal and X-ray diffraction studies of the solid–solid interactions in CuO–MoO3/MgO system

The solid–solid interactions in pure and MoO₃-doped CuO/MgO system were investigated using TG, DTA and XRD. The composition of pure mixed solids were 0.1CuO/MgO, 0.2CuO/MgO and 0.3CuO/MgO and the concentrations of MoO₃ were 2.5 and 5 mol%. These solids were prepared by wet impregnation of finely powdered basic magnesium carbonate with solutions containing calculated amounts of copper nitrate and ammonium molybdate followed by heating at 400–1000°C. The results revealed that ammonium molybdate doping of the system investigated enhanced the thermal decomposition of copper nitrate and magnesium hydroxide which decomposed at temperatures lower than those observed in case of the undoped mixed solids by 70 and 100°C, respectively. A portion of CuO present dissolved in the lattice of MgO forming CuO–MgO solid solution with subsequent limited increase in its lattice parameter. The other portion interacted readily with a portion of MoO₃ at temperatures starting from 400°C yielding CuMoO₄ which remained stable up to 1000°C. The other portion of MoO₃ interacted with MgO producing MgMoO₄ at temperatures starting from 400°C and remained also stable at 1000°C. The diffraction peaks of Cu₂MgO₃ phase were detected in the diffractograms of pure and MoO₃-doped 0.3CuO/MgO precalcined at 1000°C. The formation of this phase was accompanied by an endothermic peak at 930°C.     

Studies on the System AIVMoO7-V2O5

The phase equilibria in the system AlVMoO₇-V₂O₅ were investigated over the whole component concentration range up to 1000°C. A phase diagram was constructed from the results of DTA and XRD methods. This revised version was published online in July 2006 with corrections to the Cover Date.     

Synthesis, Crystal Structure, and Magnetic Properties of a Novel Layered Manganese Oxide Sr2MnGaO5+δ

New Sr₂MnGaO_4.97 complex oxide was synthesized by solid state reaction in sealed silica tubes at 950–1000°C. The Sr₂MnGaO_4.97 crystal structure was refined from X-ray powder diffraction data. Sr₂MnGaO_4.97 is based on the Ima2 brownmillerite-type structure with apically elongated MnO₆ octahedra due to a Jahn–Teller effect. Electron diffraction and high-resolution electron microscopy showed that local ordering of the left-and right-hand chains of GaO₄ tetrahedra in Sr₂MnGaO_4.97 leads to a superstructure with a doubling of the b parameter of the orthorhombic unit cell. The formal oxidation state of Mn (V_Mn) can be varied by thermal treatments at elevated oxygen pressure (450°C, 20 bar of O₂). The oxygen insertion induces a structure transformation in oxidized Sr₂MnGaO_5.47 material with the formation of a tetragonal perovskite-like structure (aa_p, c2c_p) with oxygen vacancies located in the Ga layers. The oxidation is accompanied by a significant compression of the Mn–O apical distances and a suppression of the Jahn–Teller deformation. Both Sr₂MnGaO_4.97 and Sr₂MnGaO_5.47 can probably be treated as canted antiferromagnets with T_N=150 and 80 K, respectively.     

Development of superconducting phases in BSCCO and Ba-BSCCO by sol spray process

The effects of barium substitution for Bi or Sr sites on the growth of superconducting phases have been studied. The sol spray process has been used to synthesis the Bi-Sr-Ca-Cu-O (BSCCO) and Ba-BSCCO homogeneous ceramic powders. Thermogravimetric (TG), differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) techniques were employed to characterize the synthesized materials. The electrical resistance was measured by classical d.c. fourprobe technique. It has been observed that sol spray process has affected the physico-chemical properties of the materials and also avoid the use of chelating agent as in the case of sol gel process. In addition to the Bi₂Sr₂CaCu₂O₈ (2212) phase Ba doped specimens also contained Bi₂Sr₂Ca₂Cu₃O₁₀ (2223), BaBiO₃, BaCuO₂ and CuO phases. The results revealed that the specific effect of barium-doping on either sites (Bi or Sr) seems to avoid the formation of higher volume fraction of the low T _c phase and promoting the formation of BiBaO₃, BaCuO₂ and CuO along with formation of a high T _c 2223 phase. The substitution of Ba on either sites (Bi or Sr) lower the sintering temperature for the formation of high T _c (small volume fraction) however, the Ba doped specimens also contained non-superconducting phases.     

Nanostructured Bi2Te3 synthesized by low temperature aqueous chemical route

Chemical and physical reactions during the low temperature aqueous chemical synthesis of nanostructured Bi₂Te₃ powders were investigated in-situ by pH measurement, color observation of the solution and X-ray diffraction analysis of the powders. It was found that Bi₂Te₃ could be synthesized only in a strong alkaline solution. Bi₂Te₃ nanocapsules were synthesized by the aqueous chemical route at 65 °C with the addition of disodium ethylenediaminetetraacetate salt. High-resolution transmission electron microscopy observation indicates that the nanocapsules are hollow-structured with a wall thickness of about 6 nm. __________ Translated from CHIMICA SINICA, 2005, 63(16)(in Chinese)     

Preparation of HPEEK by Oligomer A2+B3 Approach

A series of hyperbranched poly(ether ether ketones) with different chain length between branching point (L) were prepared using a A₂+B₃ methodology, in which the A₂ is hydroxyl‐terminated PEEK oligomer. The L affects the properties of the polymers such as the inherent viscosity, the degree of crystallinity, the thermal properties of the polymers etc. The polymer with a L₂≈8 had T _g (122.4°C), T _c (200.2°C), and broad T _m (247.4°C). With the increment of L, up to the point L₂≈20 and L₂≈35, the polymers become semi‐crystalline, with a melting point of 300.9°C and 317.9°C, respectively. Their wide angle X‐ray scattering (WAXS) pattern indicated that their crystal structure is exactly the same as that of the linear homopolymer.     

Rotation dynamics of C60 molecules in organic superconductor K3C60

The rotation dynamics of C₆₀ molecules in organic superconductor K₃C₆₀ has been investigated from the viewpoint of intramolecular interaction. It is determined that the rotation of C₆₀ at mom temperature has been frozen up within a small region of rotation angle (0°–50°), and pointed out that the reason for the freeze is the physical interaction rather than the geometrical hindrance. The computations of the interactions for alkali-doped compounds A_3-x A′ _x C₆₀ (x = 1, 2, 3; A, A′ = K, Rb, Cs) other than K₃C₆₀ have also been camed out. Fmm the obtained results, it is seen that the superconducting transition temperatures T, are strongly connected with the interactions in them, and this observation is consistent with the discovery of the correlation between T_c, and lattice constants a. Project supported by the National Natural Science Foundation of China.     

Electrochemical reduction of NO and O2 on La2−x Sr x CuO4-based electrodes

A series of La_2 − x Sr _x CuO₄ (x = 0.0, 0.05, 0.15, 0.25 and 0.35) compounds was investigated for the use of direct electrochemical reduction of NO in an all-solid-state electrochemical cell. The materials were investigated using cyclic voltammetry in 1% NO in Ar and 10% O₂ in Ar. The most selective electrode material was La₂CuO₄, which had an activity of NO reduction that was 6.8 times higher than that of O₂ at 400 °C. With increasing temperature, activity increased while selectivity decreased. Additionally, conductivity measurements were carried out, and the materials show metallic conductivity behavior which follows an adiabatic small polaron hopping mechanism.