Trajectory-property relationships in MOD-derived YBCO films

A study of the physical and chemical changes during processing in MOD-derived YBCO films was performed. Fully processed films were 70–85% of theoretical density. The sintering rate increased substantially in the compositional range F/Ba = 1.8–1.5. The activation energy for sintering decreased above a P(H₂O) dependent threshold temperature. XRD indicated this temperature/composition threshold also corresponded to YBCO nucleation, suggesting ex situ YBCO forms in contact with a melt. The ramp rate and P(H₂O) were used to control F/Ba trajectories, which were correlated to performance. The nucleation of YBCO was strongly dependent on processing conditions. Nucleation temperature was varied by at least 60 °C in the study. The optimal YBCO nucleation temperature in the 300–800 nm films was around 725 °C. a-axis grains dominated the microstructures of films where YBCO nucleated at <700 °C. Large second phases, but no a-axis grains, were found when the nucleation temperature was >750 °C.     

The Ti/c-Si solid state reaction III. The low-temperature reaction kinetics

Thin Ti layers (≈10nm) are grown on top of a clean Si(111) substrate. Heating these layers initiates a solid state reaction, yielding a monosilicide phase at ≈350°C and a C49 disilicide at ≈450°C. The present study concerns the growth kinetics of both phases by means of ellipsometry. A diffusion-limited growth kinetics is found for the monosilicide formation. However, two growth rates are observed, a fast initial one and a slow terminal growth rate. An enhanced Si diffusion in atomically disordered regions as compared to well ordered regions (grains or clusters) could be an explanation. From the measurements we have found a value of 2×10^-15 cm²/s for the diffusion coefficient at ≈370°C and an activation energy of 0.62 ± 0.1 eV. Both values correspond to the fast process. Subsequently increasing the temperature to ≈450°C permits the growth of the homogeneous C49 TiSi₂ phase. For this process, both planar layer growth and intermixing are observed, however, quantitative results could not be derived from the present study.     

Reproducibility of optically stimulated luminescence measurements from single grains of Al2O3:C and annealed quartz

We have measured some aspects concerning the performance of a new instrument for the measurement of optically stimulated luminescence (OSL) from single sand-sized grains. The instrument uses a solid-state laser to stimulate OSL from each grain individually. These grains are placed in a regular grid of nine-by-nine holes, which are drilled in the sample disc. We report on tests carried out to determine the precision with which the laser beam can be directed at individual grains in these holes. Single grains of aluminium oxide (Al₂O₃:C) (90–180 μm) and annealed quartz (90–120 μm) were used to test the reproducibility with which the OSL signal can be measured. These experiments suggest that the laser beam can be positioned to within 30 μm and that the reproducibility of OSL measurement is 3.5% on an average.     

Study of magnetic properties of La2/3Sr1/3MnO3 nanotubes by Monte Carlo simulation

Magnetic properties of a single nanotube whose walls are constituted by nanograins of La_2/3Sr_1/3MnO₃ are studied by means of Monte Carlo (MC) simulation. The system is considered as composed by ferromagnetic grains which couple via dipolar interaction. The grain size distribution is obtained from experimental measurements and the inter-grain distance distribution is obtained from a study of distance distribution among magnetic particles distributed in the tube walls. We show the magnetization behavior for a tube of 700 nm of diameter and 3.5 μm length. We discuss the simulation for different temperatures and external fields. As a main result, we show that the distribution of inter-granular distances has a unique behavior for tubular structures of similar diameter/length aspect ratio, independent of their sizes. This scaling relation allows us to perform the simulations using a tube of smaller dimensions. We succeed in explaining the magnetization curves, finding that dipolar interaction is necessary to explain the experimental behavior and that the grains behave as having magnetic dead layers.     

Detection of dust grains vibrations with a laser heterodyne receiver of scattered light

We present the results of measurement of grains vibrations under external action in gas and liquid with a laser heterodyne receiver of scattered radiation. For investigation of dynamic characteristics of particles we made the laser heterodyne receiver with sensitivity about 2×10⁻¹⁷ W/Hz and source of probing with radiation power 1 mW. In our pilot experiments, measurement of vibration amplitude of nanoparticles in gas (cigarette smoke) and microparticles in fluid (toothpaste in water) was made. We measured values of vibration amplitudes about 20–30 nm.     

Critical current density of polycrystalline YBa2Cu3O7−δ consisting of tin-coated grains

Tin and its oxides have been introduced into the intergrain areas of polycrystalline YBa₂Cu₃O_7−δ by coating the crystalline grains with a thin layer of tin and sintering the ceramics in flowing oxygen and argon. The transport critical current density J_c at 77 K in a magnetic field of 0−1.5 T is enhanced as a result of the coating. A probable improvement of the intergrain weak links is suggested.     

Crystal structure of YBa2Cu3O7−x thin films prepared by pulsed laser deposition with substrate bias voltage

The crystal structure of YBa₂Cu₃O_7−x thin films has been investigated by cross-section transmission electron microscopy. The samples were deposited on MgO (100) substrates at 670°C with substrate bias voltages of ±300 V. For the unbiased case, c-axis, a-axis and (103) oriented domains normal to the substrate surface were observed. In this film, the c-axis oriented domains are dominant, but the crystal often exhibits a longer c-lattice constant than that of the YBa₂Cu₃O_7−x system, so extra cationic layers are inserted in the YBa₂Cu₃O_7−x intrinsic stacking sequence. For the case of −300 V, rotated domains were dominant in the entire film; however, c-axis oriented domains also grow from the substrate surface. Small-angle semicoherent grain boundaries between them were observed. In the case of +300 V, all the grains show c-axis oriented YBa₂Cu₃O_7−x. The degree of preferential orientation of the grains is reduced at negative bias voltage of −300 V and the structure defects are reduced by applying a positive bias of +300 V.     

A step towards nanoionics

The interaction of finely focused 20–100 keV electron beam at 10–1000 A/cm² current densities with 30–150 nm films of the RbAg₄I₅-family solid electrolytes has been studied. The results obtained show that it is possible to form arrays of electrochemical devices with single elements ≈ 10 nm in size in the films. Arrays of 100×100 nm structures consisting of a solid electrolyte film on C-, Au-and Ag-thin supports are demonstrated.     

Radioluminescence (RL) behaviour of Al2O3:C-potential for dosimetric applications

The radioluminescence (RL) of carbon doped aluminium oxide (Al₂O₃:C) TL dosimeter material (TLD-500) was investigated using a ¹³⁷Cs conversion electron source (which also emits β and γ) for simultaneous irradiation and luminescence excitation. Furthermore, RL dosimetry characteristics of this material were studied. The main RL emission occurs at 420 nm. That matches the known main TL and OSL emissions for this material as well as an emission that was investigated in earlier RL studies, excited at higher energies (4 MeV electrons) and very high pulse delivered doses (≈800 kGy·s⁻¹). Furthermore, the saturation dose for the main peak is reached at the dose level of ≈80 Gy as known from TL and earlier RL investigations. Other peaks at 700 and 790 nm and broad emission bands at photon energies higher than 3.00 eV and others between 2.00 and 2.50 eV were observed. The 700 nm emission shows growth also at higher dose levels, and saturates at an estimated dose of ≈800 Gy. The 790 nm emission reaches its maximum intensity at ≈10 Gy absorbed dose. The reported results give an outlook to the usability and the potential of Al₂O₃:C combined with RL measurements for radiation dosimetry as well as for beta source calibration, using radioluminescence.     

The pH dependence of fluorescein fluorescence

Fluorescence quantum yields Φ_f and corrected fluorescence spectra were determined for fluorescein over a wide pH range (10 M H₂SO₄ to 0.01 M NaOH) in aqueous solution. The results were interpreted by comparison with those obtained for the very similar dye 6-hydroxy-9-phenyl-fluoron (HPF) which lacks the fluorescein carboxyl group. We find for the fluorescein cation Φ_f = 0.9−1, for the neutral molecule Φ_f = 0.20−0.25, and for the monoanion Φ_f = 0.25−0.35. The neutral molecule and monoanion have identical fluorescence spectra: an emission with maximum at 515 nm, extending to about 700 nm. (The dianion also has a maximum at 515 nm but has a more narrow emission band.) The fluorescein cation dissociates in the excited state at an acidity corresponding to that of ≈3 M H₂SO₄. A detailed scheme of the protolytic reactions of fluorescein in the excited state is presented.     

Cosmic history of the Bragin pallasite: evidence from the fission-track analysis

Chronology is rather a weak point in the investigation of pallasites, the stony-iron meteorites. No chronological data are known for the Bragin pallasite. Our attempt to reconstruct its cosmic history was based on the interpretation of fission-track analysis data. To apply this method only uranium-rich phosphates can be used. Extremely rare grains of stanfieldite were extracted from the silicate sawing residue and from the pallasite sample directly.

The researches pursued by us made it possible to find two populations of fossil tracks in stanfieldite grains. The tracks of these populations strongly differed both in size, shape and character of distribution. The first population, consisting of short (L2–6 μm instead of L8–12 μm for induced fission tracks), round-shaped tracks irregularly distributed, as we suppose, suffered an intense heating process, which caused a significant amount of partial annealing. The second population, consisting of longer (L8–12 μm), rhombic-shaped tracks homogeneously distributed, occurred after this thermal event. Only the second population track density was used for the fission-track age calculation.

After correction of the fossil track density, consisting of the second population tracks, for other possible track sources, the revealed tracks were unequivocally identified as those due to the spontaneous fission of ²⁴⁴Pu and ²³⁸U. The largest part of them was attributed to the spontaneous fission of ²⁴⁴Pu; ρ_Pu/ρ_U≈3. The model fission-track age of the studied pallasite turned out to be 4.20 Gyr. This value fix the time of the last shock/thermal event in the cosmic history of the Bragin pallasite, which had caused the partial annealing of tracks presented to that time and “fission-track clock” reset.     

Bi-axial texture in Ca0.1Y0.9Ba2Cu4O8 composite wires made by metallic precursors

High filament count, silver-sheathed composite wires of Ca_0.1Y_0.9Ba₂Cu₄O₈ (Y–124) were prepared by a metallic precursor route. The ductility of the metallic precursor enabled one to manufacture tapes containing up to 962 407 filaments, with filament dimensions as fine as 0.25 μm thick and 1 μm wide. By using a thermal-mechanical treatment to texture the Y–124 grains, transport critical current densities in the oxide filaments of 69 500 A/cm² at 4.2 K in self-field were obtained. Moreover, in an applied field of 0.1 T, the samples retained 39% of their self-field critical current density. A TEM investigation revealed significant bi-axial crystallographic texture: in areas viewed, c-axis alignment of adjacent grains was within 10° and oriented perpendicular to the tape face; a-axis alignment of adjacent grains was within 15° and oriented parallel to the longitudinal direction of the filaments. Furthermore, c-axis texture alone did not adequately predict the performance of these Y−124 composite conductors. Instead, performance scaled with the degree of bi-axial texture. These wires exhibited among the best reported J_c for a polycrystalline, sintered wire of YBCO in an applied magnetic field.     

Formation of epitaxial SiC nanocrystals

Epitaxial 3C-SiC grains are formed at 1190 °C in the top region of silicon, when Si wafers coated by SiO₂ are annealed in CO atmosphere. The formed SiC grains are 40-50 nm high and 100 nm wide in cross-section and contain only few defects. Main advantage of the method is that the final structure is free of voids.The above method is further developed for the generation of SiC nanocrystals, embedded in SiO₂ on Si, and aligned parallel with the interface. The nanometer-sized SiC grains were grown into SiO₂ close to the Si/SiO₂ interface by a two-step annealing of oxide covered Si: first in a CO, than in a pure O₂ atmosphere. The first (carbonization) step created epitaxial SiC crystallites grown into the Si surface, while the second (oxidation) step moved the interface beyond them. Conventional and high resolution cross-sectional electron microscopy showed pyramidal Si protrusions at the Si/SiO₂ interface under the grains. The size of the grains, as well as their distance from the Si/SiO₂ interface (peak of pyramids) can be controlled by the annealing process parameters. The process can be repeated and SiC nanocrystals (oriented in the same way) can be produced in a multilevel structure.     

Optimizing the bandwidth and noise performance of distributed multi-pump Raman amplifiers

Based on hybrid genetic algorithm (HGA), the signal bandwidth of the distributed multi-pump Raman amplifiers is optimized, and the corresponding noise figure is obtained. The results show that: (1) the optimal signal bandwidth Δλ decreases with the increase of the span length L, e.g., Δλ is 79.6 nm for L=50 km and 41.5 nm for L=100 km under our simulated conditions; (2) the relationship between Δλ and L is approximately linear; (3) the equivalent noise figure can be negative and increases with the extension of L; (4) there are one or several global maximum signal bandwidth on the determinate conditions; (5) to realize the fixed Δλ, several candidates can be obtained by means of HGA, as has important applications on the design of distributed multi-pump Raman amplifiers in practice.     

Superconducting oxide formation in the Yb---Ba---Cu---O system

Conditions for forming YbBa₂Cu₄O₈, Yb₂Ba₂Cu₃O_7−δ and YbBa₂Cu₃O_7−δ were determined in oxygen at 1.0 atm pressure by experiments with oxidized Yb---Ba---Cu---Ag alloys. YbBa₂Cu₃O_7−δ formed in less than 10 s when oxidized alloy ribbons were baked in the 805°C–890°C range. Large amounts of Ba₂Cu₃O₅ formed below 870°C. Yb₂Ba₄Cu₇O_15−δ and YbBa₂Cu₄O ₈ then formed in the 10²s–10³s range at temperatures in the 840°C–870°C and <840°C ranges, respectively. Ba₂Cu₃O₅ decomposition supplied Cu²⁺ and O²⁻ for the rapid transformation of YbBa₂Cu₃O_7−δ grains into Yb₂Ba₄Cu₇O_15−δ grains by intercalation. Intercalation was much slower in the absence of Ba₂Cu₃O₅. All of these transformation products underwent coarsening with increasing bake time. Rapid YbBa₂Cu₄O₈ and Yb₂Ba₄Cu₇O_15−δ formation, compared to the slow formation of these phase types when Yb was substituted by Y, Is due to the differing effects of Y and Yb on formation kinetics. Superconducting oxide-silver composite ribbons containing mainly YbBa₂Cu₃O_7−δ, Yb₂Ba₄Cu₇O_15−δ or YbBa₂Cu₄O₈ can be prepared from Yb---Ba ---Ba---Cu---Ag alloys.     

Sub-Doppler spectroscopy by sub-micron thin Cs vapour layer

A unique extremely thin cell (ETC) with the thickness of Cs atomic vapour layer in the range of 150–300 nm has been developed for the first time. All six hyperfine transitions of D₂ line (852 nm) of Cs, i.e. 6S_1/2(F=3)→6P_3/2(F=2–4) and 6S_1/2(F=4)→6P_3/2(F=3–5) are very well resolved in the transmission and fluorescence spectra, whereas in a cell of usual length they are not resolved due to Doppler broadening. It is demonstrated that a robust and widely used simple laser-diode technique is enough to observe separately atomic hyperfine transitions at the intensity up to 100 mW/cm² thanks to the ETC usage. We report also the first results obtained with the new ETC of 300 nm thickness filled with natural Rb. The usage of ETC allowed us to completely resolve each particular hyperfine transition of both ⁸⁵Rb and ⁸⁷Rb isotopes in D₁ line fluorescence spectrum.     

Studies on the iodine complexes of pyridine picolines and aminopyridine by constant activity method

The iodine complexes of pyridine, -, β-, γ- picolines, 2-aminopyridine and 2,2′-bipyridine in cyclohexane were studied by the constant activity method, their spectral characteristics and thermodynamic parameters were determined. The equilibrium constants, molar extinction coefficients of the charge-transfer band maxima, _CT, at 25°C and heats of complexation, ΔH°, are respectively as follows:

1. (a) pyridine-iodine, 107 dm³mol⁻¹ 24200 dm³mol⁻¹m⁻¹ and 31 KJ/mol;

2. (b) -picoline-iodine, 172 dm³mol⁻¹m⁻¹, 49700 dm³mol⁻¹m⁻¹ and 33 KJ/mol;

3. (c) β-picoline-iodine, 243 dm³mol⁻¹, 50300 dm³mol⁻¹m⁻¹ and 35 KJ/mol;

4. (d) γ-picoline-iodine, 342 dm³mol⁻¹, 55900 dm³mol⁻¹m⁻¹ and 41 KJ/m;

5. (e) 2-aminopyridine-iodine, 427 dm³mol⁻¹, 60800 dm³mol⁻¹m⁻¹ and 47 KJ/mol;

6. (f) 2,2′-bipyridine-iodine, 6.0 dm³mol⁻¹,−, 21 KJ/mol.

The values of the blue shifted iodine band maxima of the above mentioned donors and their molar extinction coefficients are, 420 nm (1450 dm³mol⁻¹m⁻¹), 419 nm (1470 dm³mol⁻¹m⁻¹), 418 nm (1640 dm³mol⁻¹m⁻¹), 417 nm (1570 dm³mol⁻¹m⁻¹), 410 nm (1574 dm³mol⁻¹m⁻¹) and 452 nm (1370 dm³mol⁻¹m⁻¹) respectively. The oscillator strengths and transition dipole moments of the blue-shifted iodine bands are characterised.     

High-resolution electron microscopy study of Ni81Fe19 film with Co33Cr67 buffer layer

The anisotropic magnetoresistance (AMR) in permalloy Ni₈₁Fe₁₉ film deposited on a 1.2 nm Co₃₃Cr₆₇ buffer layer was significantly enhanced. The high-resolution electron microscopy was used to study the microstructure of Ni₈₁Fe₁₉ film with and without Co₃₃Cr₆₇ buffer layer. It was found that Co₃₃Cr₆₇ buffer layer can induce good (1 1 1) texture, while without Co₃₃Cr₆₇ buffer layer, Ni₈₁Fe₁₉ film show randomly oriented grain structure. The Δρ/ρ enhancement is attributed to the decrease in the resistivity ρ of the Ni₈₁Fe₁₉ film due to the formation of the large (1 1 1) textured grains in Ni₈₁Fe₁₉ film with Co₃₃Cr₆₇ buffer layer. However, the surface roughness of substrate may limit the (1 1 1) textured grain size and induce additional grain boundaries in Ni₈₁Fe₁₉ film with Co₃₃Cr₆₇ buffer layer, limit the enhancement of the AMR effect.     

Study of the interfacial structure and chemistry of CVD κ-Al2O3/TiC multilayer coatings

This article describes the interfacial regions in CVD grown TiC/κ-Al₂O₃ multilayers. A number of microanalytical techniques were used including HREM, EDX and EELS. Occasionally, the first 50 nm of the alumina layers deposited on the intermediate TiC layers grew as a cubic alumina, heavily faulted, containing small amounts of sulphur (S), maybe as a stabiliser. The presence of slightly rounded TiC (111) facets may act as preferred nucleation sites for the cubic Al₂O₃ phase, with a ‘cube on cube’ orientation relationship. In this way the nucleation of κ-Al₂O₃ is less favourable. After some tens of nanometres the cubic phase cannot be stabilised any longer and the layer continues to grow as κ-Al₂O₃. A number of observations point towards the reaction zone (RZ) being η- and/or γ-Al₂O₃. The diffraction work and the FFT analysis of the HREM images show that the RZ is an fcc phase with a=7.9 Å, which matches with η- and γ-Al₂O₃. The EELS Al fine structure indicate more tetrahedral Al ions than in κ-Al₂O₃, as in η- and γ-Al₂O₃. The RZ contains small amounts of S, as has been reported for γ-Al₂O₃. Due to the structural similarities between η- and γ-Al₂O₃ it was not possible to determine which of these cubic phases is present in the RZ.