Gd-substituted Bi-2223 superconductor

The effects of gadolinium doping at calcium site on the normal and superconducting properties of Bi-2223 system were studied. The Gd-doped (BiPb)-2223 series of specimens, namely Batch I, II and III were sintered at three different sintering temperatures 830, 850 and 895°C respectively. The properties investigated are (1) the normal state resistivity with a view to study metal-to-insulator transition, (2) the XRD patterns of the specimens with a view to study the relative composition of (BiPb)-2212 and (BiPb)-2223 phases and (3) the superconducting fluctuation behaviour (SFB) with a view to determine the effect of doping, if any, on the dimensionality of the fluctuation conductivity of the system. The normal state resistivity of Gd-substituted Bi-2223 specimens shows metallic, semiconducting and insulating behaviour. The T _c (R = 0) values indicate that (BiPb)-2223 phase is responsible for the observed superconducting transitions in Batch I and Batch II specimens with Gd concentrations x ≤ 0.7. This observation is further confirmed in the analysis of XRD patterns of these specimens. Gadolinium, being a magnetic impurity, has pair breaking effect near the Fermi level and decreases T _c (R = 0). The analysis of the superconducting fluctuation behaviour (SFB) shows a 2D dimensionality without any cross-over.

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The purity of SnCl4 as monitored by 35Cl nuclear quadrupole resonance

The nuclear quadrupole resonance (NQR) spectroscopy was used to control the comparative purity of three SnCl₄ samples subjected to successive stages of deep purification. The results showed that at 77 K the samples were identical in purity degree due to the ‘freezing’ of impurities into a separate fraction not affecting the perfection of the SnCl₄ crystal lattice. The results of relaxation measurements suggest that paramagnetic impurity atoms (Fe and Cr) contained in the samples in small amounts might be embedded into the crystal lattice causing extremely long spin–spin relaxation time.     

Self-assembling conditions of 1O4Ca nanoclusters in ZnTe:(Ca,O)

Self-assembling conditions for 1O4Ca tetrahedral nanoclusters in ZnTe:(Ca, O) with Ca content up to 0.02 and with the ultradilute limit of oxygen are represented. The causes of self-assembling are a CaO and ZnTe bonding preferential over a CaTe and ZnO one and decrease of the strain energy after nanocluster formation. Self-assembling conditions were studied in the temperature range from 200 ^°C to 1305 ^°C. The occurrence of nanoclusters depends only on the Ca content and temperature. The temperature of self-assembling completion when all oxygen atoms are in 1O4Ca nanoclusters is determined by the Ca and oxygen contents.     

Effects of forced solution flow on lysozyme crystal growth

In order to study quantitatively the effects of forced solution on crystal growth, we designed a new set of experimental equipment, in particular, a microchannel mixer was used as crystallization container so that the consumption of protein samples was much reduced and thus an exact syringe pump could be used for precise control of the flow rates. Since the mixer's section was designed to be rectangular, the solution velocity in its center was steady and constant, and thus repeatable experiments were facilitated. Experimental results showed that the effects of forced solution on protein crystal growth were different under different levels of supersaturation, and new results were obtained for cases of high supersaturation. When the supersaturation is σ = 2.3, with increasing flow rates the growth rates of the lysozyme crystal's (110) face hardly change when the flow rates are lower than 1300 μm/s, and decrease quickly afterwards. When the flow rate reaches 2000 μm/s, the crystal nearly ceases to grow. When the supersaturation is σ = 2.7, with increasing flow rates the (110) face growth rates increase at the beginning then reach the maximum values at 1700 μm/s – 1900 μm/s and decrease afterwards, approaching zero or so when the flow rate reaches 12000 μm/s. The higher the supersaturation, the larger the flow rate at which the crystal ceases to grow. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Coupling of an electrodialyzer with inductively coupled plasma mass spectrometry for the on-line determination of trace impurities in silicon wafers after surface metal extraction

Understanding the properties that determine the distribution and behavior of trace impurities in Si wafers is critical to defining and controlling the performance, reliability, and yields of integrated microelectronic devices. It remains, however, an intrinsically difficult task to determine trace impurities in Si because of the minute concentrations and extremely high levels of matrix involved. In this study, we used an electrodialyzer for the simultaneous on-line removal of the silicate and acid matrices through the neutralization of the excessive hydrogen ion and selectively separation of acid and silicate ions by the combination of electrode reaction as a source of hydroxide ions with the anion exchange membrane separation. To retain the analyte ions in the sample stream, we found that the presence of moderate amounts of nitric acid and hydrazine were necessary to improve the retention efficiency, not only for Zn²⁺, Ni²⁺, Cu²⁺, and Co²⁺ ions but also for CrO₄²⁻ ion. Under the optimized conditions, the interference that resulted from the sample matrix was suppressed significantly to provide satisfactory analytical signals. The precision of this method was ca. 5% when we used an electrodialyzer equipped with an anion exchange membrane to remove the sample matrix prior to performing inductively coupled plasma mass spectrometry (ICP-MS); the good agreement between the data obtained using our proposed method and those obtained using a batchwise wet chemical technique confirmed its accuracy. Our method permits the determination of Zn, Ni, Cu, Co, and Cr in Si wafers at detection limits within the range from 2.2 × 10¹⁵ to 9.0 × 10¹⁵ atoms cm⁻³.     

The Heterogeneity of Multiwalled and Single‐Walled Carbon Nanotubes: Iron Oxide Impurities Can Catalyze the Electrochemical Oxidation of Glucose

It is well established that the heterogeneity of carbon nanotubes must be determined before the origin of the electrochemical performance can be attributed. Recently it has been diligently reported that for the case of multiwalled carbon nanotube modified electrodes, copper oxide impurities are responsible for the electrochemical activity facilitating a nonenzymatic sensing strategy towards glucose. We have explored both commercially available multiwalled and single‐walled carbon nanotubes for the sensing of glucose and find that iron oxide impurities remaining from the fabrication process are the electroactive sites facilitating the nonenzymatic detection of glucose. Given that the multiwalled carbon nanotubes in this work are purchased from the same leading supplier as that used recently, discrepancies in the fabrication process exist which clearly has implications in the commercialization of electrochemical sensors based on multiwalled carbon nanotubes.     

Development and validation of an HPLC method for the determination of process-related impurities in pridinol mesylate, employing experimental designs

A simple high performance liquid chromatographic method for the determination of process-related impurities in bulk drug of the central anticholinergic compound pridinol mesylate, has been developed and validated. Spectroscopically characterized synthetic impurities were used as standards. The chromatographic separation was optimized employing an experimental design strategy, and was achieved on a C₁₈ column with a mobile phase containing 50 mM potassium phosphate buffer (pH 6.4), MeOH and 2-propanol (20:69:11, v/v/v), delivered at a flow rate of 1.0 mL min⁻¹. UV detection was performed at 245 nm. The optimized method was thoroughly validated, demonstrating to be selective, when the chromatogram was recorded with a diode-array detector and peak purities were evaluated (>0.9995). The method is robust and linear (r² > 0.99) over the range 0.05-2.5% (5-250% with regards to the 1% specification limit for both process-related impurities); it is also precise, regarding repeatability (RSD ≤ 1.5% for all of the analytes) and intermediate precision aspects and LOQ values for the impurities are below 0.01%. Method accuracy, evidenced by low bias of the results and analyte recoveries in the range of 99.1-102.7%, was assessed at five analyte concentration levels. The usefulness of the determination was also demonstrated through the analysis of different lots of pridinol mesylate bulk substance. The results indicate that the method is suitable for the quality control of the bulk manufacturing of pridinol mesylate drug substance.     

Luminescence quantum yield and multiplication of electronic excitations in the corundum crystals

The excitation spectra of luminescence in irradiated and nonirradiated corundum crystals are investigated by means of highly polarised synchrotron radiation in 5 to 30 eV region. In the fundamental absorption region the double-exciton peaks are observed in the region 8.5-9.2 eV for irradiated (especially by neutrons) crystals at temperature 90 K. At 9.5 eV sharp drops appeared, in the luminescence spectrum space which were interpreted as nonirradiative near-surface recombination, the probability of which sharply increased at high absorption coefficients. The enhancement of the luminescence efficiency in the high-energy region was connected with the decay effect of electron excitations as well as with the influence of volumetric excitations leading to the enhancement of recombination glow. Received 16 October 1998 and Received in final form 20 January 1999     

Study of a set of micrometeorites from Antarctica using magnetic and ESR methods coupled with micro-XRF

A collection of iron-rich micrometeorites from Antarctica have been investigated using electron spin resonance (ESR) and conventional magnetic methods to establish a complete magnetic codification of their specific characteristics. Due to the high selectivity of the ESR, the spectra show that the amount and nature of the magnetic impurities contained in these tiny-sized samples, mainly Ni and Cr ions, significantly modify their ESR responses. This result provides a criterion, the Ni/Cr content (identified by spectroscopy), useful for a faithful classification of this class of extraterrestrial particles with close magnetic properties. We attempt to separate the contribution of the different magnetic ions in the ESR response. This method can be easily extended to other magnetic impurities.     

XPS analysis of aluminum nitride films deposited by plasma source molecular beam epitaxy

Ten samples of crystalline aluminum nitride (AlN) film were deposited on sapphire and silicon substrates by a plasma source molecular beam method. The samples were analyzed using X‐ray photoelectron spectroscopy (XPS) depth profiling and high‐resolution X‐ray diffraction. Oxygen levels were observed to decrease exponentially from the surface into the bulk film. Aluminum, nitrogen and oxygen peaks were fitted with subpeaks in a consistent manner and the subpeaks were assigned to chemical states. AlN subpeaks were observed at 73.5 eV for Al2p and 396.4 eV for N1s. An N1s subpeak at 395.0 eV was assigned to N? N defects. No direct N? O bonds are assigned; rather it is proposed that an N? Al? O bond sequence is the source of higher binding energy N1s subpeaks. The observations in this study support a model in which oxygen is bound only to aluminum in the form of Al? O octahedral complexes dispersed or clustered throughout the main AlN matrix or as Al? O bonds on the crystal grain boundaries. The data also suggest that the AlN lattice parameters are related to oxygen content, since the c‐axis is observed to increase with increasing oxygen content. Copyright © 2008 John Wiley & Sons, Ltd.