Comparison of the Efficiency of the One and Two-Step Process for the Production of BSCCO (2212) Powders by Means of Analytical Techniques

 The efficiency of the production of the high temperature superconducting powders Bi₂Sr₂CaCu₂O_8+x (BSCCO 2212) using the solid state reaction in one or two step processes under different thermal treatment was compared by means of different modern analytical techniques. Through the same techniques the optimization of the production of the production of Bi-2212 powder produced by the two step process, was achieved. X-ray diffraction analysis (XRD) and Raman spectroscopy were used to characterize the products for their stoichiometry and phase-purity. The grain size of the powders was observed by scanning electron microscopy (SEM), while their superconducting properties were tested by electrical DC-resistivity and magnetic susceptibility measurements using a superconducting quantum interference device (SQUID). It resulted that the two step process gives a high quality BSCCO 2212 superconducting powder with T _c = 85 K, in a shorter time and with a greater recovery rate than the one step process. Received May 3, 1999. Revision April 27, 2000.     

High temperature Ho<Subscript>2</Subscript>O<Subscript>3</Subscript>–ZrO<Subscript>2</Subscript> insulation coatings on AgMg sheathed Bi-2212 superconducting tapes by sol–gel technique for magnet technology

High temperature 0, 5, 8 and 12 mol % Ho₂O₃–ZrO₂ insulation coatings were successfully deposited on Ag and AgMg/Bi-2212 superconducting tapes using sol–gel technique for magnet technologies. With this purpose, transparent solutions were prepared from Ho and Zr-based precursor materials and then Ho₂O₃ effect on thermal, structural and microstructural properties were observed and discussed in the present study. It was found that Ho₂O₃ additive has a propensity to generate tetragonal ZrO₂ and help to stabilize it. It was observed that insulation coatings with a mosaic structure having cracks were fully compatible with Ag/AgMg sheathed Bi-2212 tape substrates because of oxygen permeability, high and low actual temperatures and W&R process in comparison with the conventional insulation process. In addition, surface roughness decreased with increasing Ho₂O₃ content, thereby decreasing the grain size. Although porosity values vary considerably from one porosity mesurement expression to another, porosities of the insulation coatings can be estimated to be in the range of 3 and 30 vol %.     

Galena/(NR+SBR) rubber composites as gamma radiation shields

Different concentrations of the lead ore mineral (Galena) were incorporated into composites of natural rubber (NR) and styrene — butadiene rubber (SBR-1502). By using ¹³⁷Cs as a gamma radiation source, the composites were investigated to determine to what extent these materials could be used as a gamma radiation shield. It was found that the linear attenuation coefficient μ (m⁻¹) increases markedly with the increase of galena content up to a value of about 29 m⁻¹ for 500 phr of Galena in the rubber matrix. The thermal properties (thermal diffusivity a, specific heat Cp, and thermal conductivity λ) were also measured for these composites.     

Some remarks on heat capacity measurements by temperature-modulated calorimetry

In temperature-modulated calorimetry, the condition in sample amount, especially thickness, required for high-accuracy heat capacity measurement should be made clear. We propose the condition of maximum thickness of a sample for measuring heat capacity within an accuracy of 1%. The other important factor for high-accuracy heat capacity measurement is thermal contact conductance between a sample and a sample pan and also that between a pan and a base plate of an apparatus. The conditions in these thermal contact conductances required for high-accuracy heat capacity measurement are discussed. Among them, if only thermal contact conductance between a pan and a base plate is significant, there is an ingenious method to measure heat capacity with high accuracy. Furthermore, if the thermal contact conductance between a pan and a base plate is infinite, we offer a simple method to obtain complex heat capacity.     

Internal electrolyte temperatures for polymer and fused-silica capillaries used in capillary electrophoresis

Polymers are important as materials for manufacturing microfluidic devices for electrodriven separations, in which Joule heating is an unavoidable phenomenon. Heating effects were investigated in polymer capillaries using a CE setup. This study is the first step toward the longer-term objective of the study of heating effects occurring in polymeric microfluidic devices. The thermal conductivity of polymers is much smaller than that of fused silica (FS), resulting in less efficient dissipation of heat in polymeric capillaries. This study used conductance measurements as a temperature probe to determine the mean electrolyte temperatures in CE capillaries of different materials. Values for mean electrolyte temperatures in capillaries made of New Generation FluoroPolymer (NGFP), poly-(methylmethacrylate) (PMMA), and poly(ether ether ketone) (PEEK) capillaries were compared with those obtained for FS capillaries. Extrapolation of plots of conductance versus power per unit length (P/L) to zero power was used to obtain conductance values free of Joule heating effects. The ratio of the measured conductance values at different power levels to the conductance at zero power was used to determine the mean temperature of the electrolyte. For each type of capillary material, it was found that the average increase in the mean temperature of the electrolyte (DeltaT(Mean)) was directly proportional to P/L and inversely proportional to the thermal conductivity (lambda) of the capillary material. At 7.5 W/m, values for DeltaT(Mean) for NGFP, PMMA, and PEEK were determined to be 36.6, 33.8, and 30.7 degrees C, respectively. Under identical conditions, DeltaT(Mean) for FS capillaries was 20.4 degrees C.     

Metal-organic deposition of YBa2Cu3Ox and Bi2Sr2Ca1Cu2Ox films on various substrates starting from different fluorine-free metallorganic compounds

YBa₂Cu₃O_x (Y-123) and Bi₂Sr₂Ca₁Cu₂O_x (Bi-2212) films on various substrates have been prepared by Metal-Organic Deposition starting from different metallorganic fluorine-free compounds and using a very simple instrumentation. The processing conditions include a rapid pyrolysis step in air and an annealing step in oxygen for Y-123 and in air for Bi-2212. The films obtained have been characterized by X-ray diffraction (XRD) and the formation of a superconducting phase of Y-123 or Bi-2212 was confirmed measuring the critical temperature (T _c) with Ac-susceptibility and resistive measurements. Microstructure and final cationic ratios have been studied by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS).     

Formation of SrSnO3 shell-like inclusions in the Bi2Sr2CaCu2O8+x superconductor via chemical reaction

Superconducting composites Bi-2212–SrSnO₃ have been prepared by reacting between the Bi–Sr–Ca–Cu–O precursor and Sr₂SnO₄ or Ca₂SnO₄ at 800–950°C, followed by crystallisation of Bi-2212 from the partial melt at decreasing temperature. The samples have been characterised by powder X-ray diffraction, scanning electron microscopy and magnetic measurements. The materials consist of large Bi-2212 lamellae and complex-shaped fine inclusions of SrSnO₃. The composite obtained using Sr₂SnO₄ contains almost all the SrSnO₃ phase in the form of micron-sized spherical shells, which are partly included in Bi-2212 lamellae, partly agglomerated in-between. The shells are perforated, thus allowing the Bi-2212 crystals to grow through them. It has been found that the shell-like grains form at an early stage of the precursor thermal treatment between 800 and 850°C. A mechanism of the SrSnO₃ shell formation is proposed. The composites exhibit T_c in the range of 82–87 K and reveal up to five times better magnetic flux pinning at T≥30 K in comparison with the undoped Bi-2212 sample prepared using the same experimental procedure.     

Effect of some metallic additives (Ag, Cd, and Sn) on thermal transport properties of a-Se

In this study, we have studied the effect of elements Ag, Cd, and Sn as chemical modifiers on some thermal transport properties (thermal conductivity, diffusivity, and specific heat per unit volume) of amorphous Se. Concurrent measurements of thermal transport properties such as effective thermal conductivity (??_e), thermal diffusivity (??_e), and specific heat per unit volume (??C _v) are used at room temperature for twin pellets of pure Se- and Se-based binary Se₉₈M₂ (M?=?Ag, Cd, and Sn) alloys using transient plane source technique. We have also determined the thermal inertia I _T using the experimental values of thermal conductivity and specific heat per unit volume for present amorphous alloys. The increasing sequence of measured thermal transport properties is also discussed.     

Relative molar response factors for thermal conductivity detectors

This paper describes an investigation into the universal nature of relative molar response factors for thermal conductivity detectors. Relative molar response factors are measured on multiple gas chromatographs equipped with thermal conductivity detectors, and the values are compared with values in the literature. As was observed previously, relative molar responses obtained on a single instrument for a homologous series vary linearly with respect to the number of carbon atoms in the hydrocarbon chain. However, significant differences are observed for the slope of this line depending on the instrument studied. This contradicts previous literature results that demonstrated an indepedence of the relative molar response with regard to the detector. The current results show that the calibration of thermal conductivity detectors using literature values for relative molar response factors could produce significant errors in the concentrations measured by the laboratory chromatograph.     

Dependency of thermal and electrical conductivity on temperature and composition of Sn in Pb–Sn alloys

The variations of thermal conductivity with temperature for Pb–Sn alloys were measured using a radial heat flow apparatus. The variations of electrical conductivity with the temperature for same alloys were determined from the Wiedemann–Franz law by using the measured values of thermal conductivity. According to present experimental results, the thermal and electrical conductivity of Pb–Sn alloys linearly decrease with increasing temperature but exponentially increase with increasing the composition of Sn. The enthalpy of fusion and the change of specific heat for Pb–Sn alloys were also determined by means of differential scanning calorimeter (DSC) from heating trace during the transformation from eutectic liquid to eutectic solid.     

Transport Properties of Bi2−xInxSe3 Single Crystals

The paper reports on the temperature dependence of the electrical and thermal conductivity, Hall constant, and Seebeck coefficient of Bi_2−xIn_xSe₃ (x=0, 0.2, 0.4) single crystals measured over the temperature range from 2 to 300 K. One single-valley conduction band model is used to interpret relations among transport coefficients. The data analysis relies on the use of a mixed carrier scattering mechanism consisting of acoustic scattering and scattering on ionized impurities. The effect of In incorporation into the Bi₂Se₃ crystal lattice on the individual components of thermal conductivity is evaluated and discussed.     

Estimating the thermal properties of soils and soft rocks for ground source heat pumps installation in Constanta county,Romania

The main objective of ThermoMap project was to develop a methodology for estimating the thermal conductivity and heat capacity in the first 10 m of the ground, in order to identify areas favourable for installation of ground heat source pumps. Based on best available data regarding climate, soil type, soil texture, geology and water table depth, maps of the thermal parameters were computed in test areas from partner countries. Three depth layers were investigated: 0–3, 3–6 and 6–10 m, each one characteristic for different types of ground source heat pumps. In order to check the computed values, samples were collected in test areas and measured in the laboratory. This paper presents the results of the validation performed for Constanta county test area (Romania). Samples of soil and Quaternary formations collected in the Danube terraces and the Black Sea high shores were analyzed in the laboratory for determining the bulk density, soil texture, thermal conductivity and heat capacity. The measurements were performed on samples simulating the three possible system conditions: unsaturated (arid or humid) and saturated conditions. The values determined by laboratory measurements were interpolated in order to obtain the appropriate thermal conductivity values for the defined bulk density values used by ThermoMap for each depth layer. The comparison between ThermoMap computed data and the laboratory measurements of thermal conductivity showed that out of three samples, at least two are within the specified error range of ±25 %. The best fit occurs for layer 3–6 m, whose assigned density is closer to the mean of measured bulk density values.     

Systematic errors in the measurement of heat by flow microcalorimetry

It is shown that a number of systematic errors must be considered when performing heat measurements by flow microcalorimetry because the nature of the flow technique is such that substantial heat loss can be incurred. The conventional procedure of electrical calibration is found to be an inadequate correction parameter. Equations to account for the effects of thermal disequilibrium are derived from the basic principles incorporated in the Tian equation. The predicted relationships are tested by simple experiments and shown to be correct. The various correction parameters are measured for a wide range of flow rate and heat input conditions. A composite equation is presented which allows for the correction of heat loss while deconvoluting electrical heat from a heat of reaction. The total heat output rate from a flow calorimeter can be calculated for most experimental conditions by reference to this equation and to the tabulated correction values.     

An improved method for determining zeta potential and pore conductivity of porous materials

An improved method based on streaming potential and streaming current was proposed to determine zeta potential and surface conductance of porous material simultaneously. In the electrokinetic generation mode, a resistor is connected to the generator and by measuring the voltage drop across resistors with different resistance, a true streaming current can be determined. The zeta potential and surface conductivity can be obtained simultaneously from their relation to streaming potential and streaming current. The electrode and ion concentration polarization effects during the measurement were also discussed. The resistance from channel ends to electrodes, which has typically been ignored in the literature, was shown to have a significant influence on the calculated zeta potential and surface conductance. Ignorance of this resistance would lead to underestimation of both zeta potential and surface conductance values.     

Survey of the quasi-ternary system La0.8Sr0.2MnO3–La0.8Sr0.2CoO3–La0.8Sr0.2FeO3

An overview on the variation of the thermal expansion, the electrical conductivity as well as non-stoichiometry of the oxide content as a function of composition within the quasi-ternary system La_0.8Sr_0.2MnO_3−δ–La_0.8Sr_0.2CoO_3−δ–La_0.8Sr_0.2FeO_3−δ in air is presented. The various powders were synthesized under identical conditions. The DC electrical conductivity values of the compositions at 800 °C in air vary in a wide range from 15 to 1338 S cm⁻¹. The magnitude of electrical conductivity of the perovskites is mainly determined by the percentage of cobalt in the compositions. A similar behaviour was observed for the measured thermal expansion coefficients between room temperature and 1000 °C in air, increasing from 10.9 to 19.4 × 10⁻⁶ K⁻¹ as a function of cobalt content. Changes in the oxygen stoichiometry of the materials were characterized by temperature-programmed oxidation measurements.     

Thermal stability of an explosive detonator

Mercuric 5-nitrotetrazole is a possible replacement for lead azide. The thermal decomposition peak maximum ranged from 185 to 270°C as the heating rate increased from 0.1 to 100°C min⁻¹. The activation energy and frequency factor for thermal decomposition were determined from dynamic and isothermal DSC and isothermal TG data; the average values were 38.8 kcal mol⁻¹ and 3.56×10¹⁴ s⁻¹. A half-life experiment confirmed the kinetic constants and indicated that the decomposition reaction was first order. The heat of explosion was determined by a pressure DSC test and found to be 2587 J g⁻¹. The linear coefficient of expansion was 37±2×10⁻⁶°C⁻¹ from −60 to 160°C and indicated secondary transitions near −10 and 90°C. The specific heat was 0.0003154T+0.1339 in the region −40–90°C. The critical temperature for a slab with a half-thickness of 0.035 cm was calculated to be 232 °C.     

A computer-controlled apparatus for thermal conductivity measurement by the transient hot wire method

The aim of this paper is to review the transient hot wire method for measurement of thermal conductivity, which is based on the measurement of temporal history of the temperature rise caused by linear heat source (hot wire) embedded in a test material. If a current is passed through the wire, the rise in temperature will be dependent, among other factors, on the thermal conductivity of the medium, surrounding the wire. Here the mathematical basis, as well as main modifications of the hot wire method — cross technique, resistance modifications with potential and compensated lead methods; hot wire probe method and parallel wire technique, are described and discussed. A fully automated computer-controlled transient hot wire apparatus is presented and tested, which allows measurement of thermal conductivity of solid, powder and granular materials at high temperatures.     

Changes in induced polarization associated with the sorption of sodium, lead, and zinc on silica sands

Low-frequency dielectric spectroscopy can be measured in terms of a conductance and a phase lag between the electrical current and the electrical field. This conductance and phase lag can be written as into a complex conductivity with both an in-phase and quadrature components that are frequency dependent. In sands, the low-frequency (10 mHz-40 kHz) spectra of the complex conductivity are dominated by the polarization of the electrical double layer (especially the internal part of the electrical double layer called the Stern layer) and the Maxwell-Wagner polarization (typically above 100 Hz). We present a polarization that is able to explain the complex conductivity spectra including the grain size distribution, the porosity, and the complexation of the mineral surface with the ions of the pore water. To test this model, we investigate the sorption of various cations (Na, Pb, Zn) characterized by different affinities with the surface of silica. Sand column experiments were carried out to see the change in the complex conductivity during the advective/dispersive transport of a lead nitrate solution and a zinc sulfate solution, replacing a sodium chloride solution in the pore space of the sand. The complex conductivity model is able to explain the change of the phase over time.     

Applicability of the transient plane source method to measure the thermal conductivity of low‐density polyethylene foams

The thermal conductivity at constant pressure of a collection of crosslinked, closed‐cell polyethylene foams were measured at room temperature with the transient plane source (TPS) method. The experimental results were compared with those determined by a standard steady‐state technique. The results showed that the values measured by the TPS method follow the same trends as those measured by a heat‐flow meter. Therefore, with the TPS technique it is possible to observe the influence of structural characteristics such as cell size, black carbon content in foams, density, and so forth on thermal conductivity. However, the values obtained by the transient method were approximately 20% higher than those given by the standard method. Possible reasons for these variations are discussed. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 1226–1234, 2004     

Thermal properties measurement of cut tobacco based on TPS method and thermal conductivity model

Drying process of biomass porous media is widely involved in agricultural products processing. Accurate measurement of thermal properties and prediction of thermal conductivity variation at different conditions is the key of heat transfer simulation and optimization for drying process. The present work measured the thermal properties of cut tobacco in a constant temperature experimental platform by transient plane source method (TPS method), and developed a model to predict thermal conductivity of cut tobacco at different conditions. The results showed that there was a high test precision for thermal properties measurement of cut tobacco by TPS method. Thermal conductivity of cut tobacco increased significantly with the increase of temperature and moisture content at the range of 25–65 °C and 12.5–25 %. Volume heat capacities showed a similar trend. The model predictions of thermal conductivity showed strong correlation coefficient with experimental values. The deviation of model predictions is less than 10 %, which indicated that the established model had a good prediction precision for thermal conductivity of cut tobacco.