Dr. Petre BADICA

By experiment we evaluated the longitudinal magnetostriction on cylindrical samples of MnZn ferrite. Starting from the idea that the magnetostriction phenomenon is closely related to the magnetization phenomenon of the ferromagnetic sample, by plotting the magnetostriction curve it is possible to extract the magnetization curve of the ferromagnetic material and to evaluate the saturation magnetization of the material and the demagnetizing factor of the sample. At the same time, the paper suggests a way to study the dynamics of the movement of the magnetic domain walls in the sample, by examining the resonance curve at each point on the magnetization curve.

A multiphase high-entropy diboride (Ti0.25Ta0.25Hf0.25Zr0.25)B2 is obtained by spark plasma sintering from a mixture of single-metal diborides. The as-prepared material at the microscale can be defined as a composite where grains of a Ta-rich/Ti-poor complex diboride phase are the reinforcement and grains of Ta-poor/Ti-rich complex diboride are the matrix. However, at the nanoscale, the grains are heterogeneous, composed of regions with a multitude of complex diboride compositions. The interface between nanoregions is compositionally graded and has an irregular shape. The four-metal diboride shows a deformation-resistant mechanism under bending load. A strengthening process is active, increasing the room temperature bending strength (326 MPa) by approximate to 50% at 1800 degrees C (488 MPa). A ductile behavior with a deformation strain of approximate to 7.5% is observed at 2000 degrees C while bending strength (407 MPa) is approximate to 25% above the value at room temperature. At 2000 degrees C, observation of dislocations propagating from one compositional nanoregion to another and with a different density suggests dislocation contribution, first of all, to plasticity. The peculiar heterogeneity of this material at nano- and microscales is considered the reason for the remarkable mechanical response to bending load at different temperatures.

The precise control of the magnetic compensation temperature (theta c) in ferrimagnetic garnets is essential for the development of cutting-edge ultrafast customizable spintronic devices. In this work we demonstrate how fine variation in stoichiometry and cation distribution in iron gadolinium garnets significanty influences theta c. Two samples of Gd3Fe5O112 garnets synthesized via a new hydrothermal method and a conventional solid-state reaction, respectively, were considered. The complex study was carried out using a complex approach combining X-ray diffraction, magnetometry, and M & ouml;ssbauer spectroscopy. Atomic-scale analysis revealed with unprecedent accuracy a cationic inversion between Fe3+ ang Gd3+ at octahedral and dodecahedral sites in both samples, and their chemical compositions were determined as Gd2.70Fe4.76O11.9 and Gd2.96Fe4.68O11.5, respectively. These local rearrangements have been shown to have a consistent influence on theta c (290 K and 317 K, respectively) around room temperature, emphasizing the high sensitivity of exchange interactions to internal atomic order. Results clearly illustrate the strong correlation between the processing, atomic configuration and macroscopic magnetic behavior, establishing a new paradigm for the design of garnet-based materials with tunable theta c. The strategy for the accurate determination of cation inversion illustrated in this work exhibits great potential in guiding material innovations for next-generation spintronics.

The Ni49+xMn32-2xGa19+x (x = 0; 2) Heusler ferromagnetic shape memory alloys were prepared using spark plasma sintering using raw flake-type powders obtained by soft grinding melt-spun ribbons. Samples were characterized using x-ray diffraction, electron microscopy, thermal analysis, and bending tests. Although the properties of ribbons and corresponding powders show similar properties' tendencies, they are opposite in the bulk sintered alloys when compared with precursor powders. Namely, Ni49Mn32Ga19 bulk shows a higher enthalpy (5.8 J g-1), an increased martensitic transformation (MT) temperature (by 9 K), and a reduced hysteresis span (5 K). Conversely, for the Ni51Mn28Ga21 sintered sample, a lower enthalpy (2 J g-1), a significant decrease (by 40 K) in the MT starting temperature, and a broadening of the hysteresis range (26 K) were observed. This difference is analyzed versus specific features of the microstructure. Moreover, the activation energy and the pre-exponential factor of the MT, extracted through kinetic analysis within two non-isothermal models, Kissinger and Friedman, complement and sustain these findings. Fractography details of the sintered samples are discussed in relation to the stress-strain curves from the bending tests. The Ni49Mn32Ga19 bulk sample exhibits a higher bending strength (260 MPa) and a lower strain (0.55%) than the Ni51Mn28Ga21 sample (177 MPa and 0.61%). The observed dependence of functional characteristics on preparation enables the possibility of property control required for various applications and suggests that the proposed route is promising in this regard for further investigations.

Bulk MgB2 disks (20 mm in diameter and 3.8 mm in thickness) added with 0, 1.5, 3.0, 4.5, 6.0, and 9.0 wt% silver are obtained by in situ spark plasma sintering. Samples are characterized by structural, microstructural, magnetic, and magnetic levitation zero-field-cooling and field-cooling measurements. Superconducting transitions are sharp with critical temperatures being in the range of 36.5-37.9 K. The vertical (F z,ZFC) and lateral (F x) levitation force show maximum values for samples added with 1.5 or 3 wt Ag%. At 20 K they are +17.78 N and 6.37 N, respectively. A maximum for zero field critical current density and pinning force is found for the sample added with 3 wt%. Roughly, as expected, levitation force correlates with zero-field critical current density, but other details influence this dependance. Results indicate that silver is an effective addition to MgB2 for enhancement of levitation performance.

Superconducting bulk disks, of 20 mm in diameter and similar to 3.5-mm thickness of MgB2 were prepared by spark plasma sintering. Samples are co-added with 10 wt. % hexagonal BN (h-BN) or graphene (G) and other additives (B4C, Te, cubic BN, fullerene C-60, or Repa-C6H10O7Ge2 (GEP)), where h-BN and G are introduced in the composite to provide full machinability by chipping of the composite and the other additives to modify microstructure and superconducting characteristics. Measurements of trapped magnetic field B-tr for a fixed rate of the applied magnetic field decrease (0.00015 T/s) indicate that samples with G show less flux jumps, but a higher thermomagnetic stability is accompanied by lower values of B-tr than for samples with h-BN. The highest maximum B-tr at 12 K for samples added with h-BN or graphene was recorded for MgB2(Te)(0.01) + 10wt.% h-BN (3.48 T) and MgB2(B4C)(0.01) + 10wt.% G (2.73 T), respectively. These values of maximum trapped field were determined for an applied field of - 2.5 and - 1.8 T. Results suggest that machinable MgB2-based composites show potential for bulk superconducting magnet applications.

MgB2 is a perspective superconductor for many power applications. How this potential refers also to microwave or radiofrequency applications is still to be determined. Although its ultimate surface resistance in zero field is not competitive with conventional metallic superconductors, its strong pinning properties can favor RF applications in a dc magnetic field. Nonetheless, the RF response in the vortex state has been relatively less studied, as well as the effect of artificial pinning centers on the microwave surface resistance in the mixed state. In this paper we study the surface resistance of spark-plasma-sintered MgB2, with and without Te and cubic-BN (cBN) addition, in a dc magnetic field up to 1.2 T. We summarize previous results on pure MgB2, and we present new data on Te-and cBN-added MgB2. We use a two-tone dielectric-loaded resonator to measure the field-dependent surface resistance at 16.5 and 26.7 GHz in the temperature range from 10 K to T. By exploiting the simultaneous measurements at two frequencies, we extract the flux-flow resistivity, the pinning constant kp and the depinning frequency fp. The two-band nature of MgB2 affects the field dependence of the flux-flow resistivity. The microscopic superconducting state is not affected by the addition of artificial pinning centers, indicating that Te and cBN do not affect interband or intraband scattering. Pinning shows a measurable trend towards an increase in the Te-and cBN-added samples at higher temperatures and fields. We finally compare the results to those obtained in bulk Nb3Sn, also in view of possible in-field RF applications such as microwave cavity-based haloscopes.

We explored the possibility to guide the forming process in a Ta/TiO2/Pt memristive device using an X-ray nanopatterning procedure, which enables the manipulation of the oxygen content at the nanoscale. The irradiation of selected areas of the sample by a 65 x 58 nm2 synchrotron X-ray nanobeam locally generated oxygen vacancies which resulted in the formation of a conductive filament in the desired position in the material. The subsequent application of an electric field between the electrodes was exploited to achieve reversible bipolar resistive switching. A multitechnique characterization was then performed, highlighting a local increase in the height of the crystal and the formation of a dislocation network, associated with the presence of Wadsley defects. Our results show that X-ray nanopatterning could open new avenues for a more deterministic implementation of electroforming in oxide-based memristive devices. We tuned the oxygen content in a Ta/TiO2/Pt memristive device at the nanoscale by a synchrotron X-ray nanobeam. We obtained a conductive filament of oxygen vacancies in the desired position in the material to achieve a controlled resistive switching.

Dense samples of MgB2, with a relative density of 98.3-99.1 %, were prepared by ex-situ spark plasma sintering using a raw powder supplied by Alfa Aesar. Samples were added with Ge-based organometallics (repagermanium/RGe, propagermaniu/PGe, linear Ge-based organometallic/GeSP, and Na-doped octamer/8THGP-Na) for the starting composition (MgB2)(Ge-based organometallics)0.0014. Except for the 8THGP-Na, they have a similar chemical composition in respect to Ge and C, while the crystal structure differs. Below 20 K, all studied additions increased the critical current density, Jc, and the irreversibility field, Hirr. Samples added with GeSP and 8THGPNa have marginal differences regarding superconducting characteristics. The best Jc and Hirr are obtained for the sample added with RGe. This sample has the highest amount of carbon in the crystal lattice of MgB2. Results point out that there is a complex influence of the additive on carbon behaviour. Although in general it is accepted that a higher amount of carbon produces higher Jc and Hirr, a comparison with the literature indicates that C-rich raw MgB2 powders (e.g. the C-enhanced MgB2 nanopowder produced by Pavezyum) are not suitable to promote strong superconductivity enhancement in the samples added with indicated organometallics, and the origin, states, and evolution of carbon should to be carefully assessed.

Fabrication and extensive characterization of hard-soft nanocomposites composed of hard magnetic low-temperature phase LTP-MnBi and amorphous Fe70Si10B20 soft magnetic phase for bulk magnets are reported. Samples with compositions Mn55Bi45 + x center dot(Fe70Si10B20) (x = 0, 3, 5, 10, 20 wt.%) were prepared by spark plasma sintering of powder mixtures. Characterization has been performed by X-ray diffraction, scanning and transmission electron microscopy, magnetometry and Fe-57 Mossbauer spectroscopy. It was shown that samples contain crystallized and nanometric LTP-MnBi phases with various elemental compositions depending on the degree of Bi clustering. Complex correlations between starting compositions, processes during fabrication, and functional magnetic characteristics were observed. Unexpected special situations of the relation between microstructure and magnetic coupling mechanisms are discovered. Exchange spring effects of different strengths occur, being very sensitive to morpho-structural and compositional features, which in turn are controlled by processing conditions. An in-depth analysis of related microscopic characteristics is provided. Results of this work suggest that fabrication by powder metallurgy routes, such as spark plasma sintering of hard and soft magnetic powder mixtures, of MnBi-based composites with exchange spring phenomena have a high potential in designing and optimization of suitable materials with tunable magnetic properties towards rare-earth-free permanent magnet applications.

Fabrication aspects of PdO thin films and coatings are reviewed here. The work provides and organizes the up-to-date information on the methods to obtain the films. In recent years, the interest in Pd oxide for different applications has increased. Since Pd can be converted into PdO, it is instructive to pay attention to the preparation of the pure and the alloyed Pd films, heterostructures, and nanoparticles synthesized on different substrates. The development of PdO films is presented from the early reports on coatings' formation by oxidation of Pd foils and wires to present technologies. Modern synthesis/growth routes are gathered into chemical and physical categories. Chemical methods include hydrothermal, electrochemical, electroless deposition, and coating methods, such as impregnation, precipitation, screen printing, ink jet printing, spin or dip coating, chemical vapor deposition (CVD), and atomic layer deposition (ALD), while the physical ones include sputtering and cathodic arc deposition, laser ablation, ion or electron beam-induced deposition, evaporation, and supersonic cluster beam deposition. Analysis of publications indicates that many as-deposited Pd or Pd-oxide films are granular, with a high variety of morphologies and properties targeting very different applications, and they are grown on different substrates. We note that a comparative assessment of the challenges and quality among different films for a specific application is generally missing and, in some cases, it is difficult to make a distinction between a film and a randomly oriented, powder-like (granular), thin compact material. Textured or epitaxial films of Pd or PdO are rare and, if orientation is observed, in most cases, it is obtained accidentally. Some practical details and challenges of Pd oxidation toward PdO and some specific issues concerning application of films are also presented.

Accelerator Mass Spectrometry (AMS) and cosmogenic nuclides techniques are used in quantitative geomorphological studies on large time scale. In order to accurately date surface exposure to cosmic rays, the amount of pure quartz taken into account, needs to be well determined. Depending on the particularity of the rocks, sometimes the presence of feldspar in geological samples hinders the accurate determination of 26Al and 10Be by AMS. To overcome this problem, our paper proposes the assessment of quartz purity by SEM-EDX analysis, in an objective and facile way, compared to ICP-MS method. The proposed methodology is not only effective, but it shows features that save time and excessive consumption of reagents that often are not environment and health friendly.

Bulk MgB2 discs were prepared by an in situ route from mixtures of magnesium and boron powders. The boron powders were produced by two methods. The first one consisted of a self-propagating high tem-perature magnesiothermic synthesis (SHS) process followed by acid and fluorine cleaning and a heat treatment in inert atmosphere. This approach produced boron with purities between 86 % and 97 %, where the main impurity was Mg. Depending on the final heat treatment, these boron powders were amorphous or crystalline. In the second route, high purity nano powders (99 %) of boron were obtained by a diborane pyrolysis process. Bulks of MgB2 were characterized by structural, microstructural, and magnetic mea-surements. Critical current density, pinning force aspects and levitation force (including guiding force) details were assessed. Amorphous lower purity boron (86-97 %) obtained by the first processing route was found to promote the largest levitation forces of the MgB2 bulks and, among these samples, the best le-vitation results were recorded when using boron with a purity of 95-97 %. Use of a lower purity boron that decreases the cost of MgB2 promotes large scale production at industrial level of bulk MgB2 super-conducting magnets for levitation applications and enhances the applicability potential of MgB2 super-conductor. The relationship between levitation force and specific features of the samples such as pinning force details are discussed.& COPY; 2023 Elsevier B.V. All rights reserved.

Currently, the treatment of wounds is still a challenge for healthcare professionals due to high complication incidences and social impacts, and the development of biocompatible and efficient medicines remains a goal. In this regard, mesoporous materials loaded with bioactive compounds from natural extracts have a high potential for wound treatment due to their nontoxicity, high loading capacity and slow drug release. MCM-41-type mesoporous material was synthesized by using sodium trisilicate as a silica source at room temperature and normal pressure. The synthesized mesoporous silica was characterized by using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), N2 absorption-desorption (BET), Dynamic Light Scattering (DLS) and Fourier transform infrared spectroscopy (FT-IR), revealing a high surface area (BET, 1244 m2/g); pore diameter of approx. 2 nm; and a homogenous, ordered and hexagonal geometry (TEM images). Qualitative monitoring of the desorption degree of the Salvia officinalis (SO) extract, rich in ursolic acid and oleanolic acid, and Calendula officinalis (CO) extract, rich in polyphenols and flavones, was performed via the continuous recording of the UV-VIS spectra at predetermined intervals. The active ingredients in the new composite MCM-41/sage and marigold (MCM-41/SO & CO) were quantified by using HPLC-DAD and LC-MS-MS techniques. The evaluation of the biological composites' activity on the wound site was performed on two cell lines, HS27 and HaCaT, naturally involved in tissue-regeneration processes. The experimental results revealed the ability to stimulate collagen biosynthesis, the enzymatic activity of the main metalloproteinases (MMP-2 and MMP-9) involved in tissue remodeling processes and the migration rate in the wound site, thus providing insights into the re-epithelializing properties of mesoporous composites.

High density samples (92-94.5 %) of MgB2 were prepared by Spark Plasma Sintering (SPS). The on-off pulsed current patterns of SPS processing were 8-4, 12-2, 24-2, 99-1. Patterns with more on pulses favor formation of a higher amount of the secondary MgB4 phase through the decomposition of MgB2. They also promote enhancement of larger MgO crystallites without a strong increase in the amount of this phase. Densification rate and pressure in the SPS chamber show a similar behavior, but their amplitude varies and the temperatures defining different stages present some shifts. As-revealed differences induced by pulsed patterns impact superconducting properties in a complex manner. An attempt to assess correlations between the pattern and different superconducting parameters is presented.

We present the multifrequency measurements of the surface resistance of spark-plasma-sintered MgB2 performed through a dielectric loaded resonator operating at 16.5 and 26.7 GHz. By normally applying magnetic fields <= 1.2 T to the sample surface, we drove it in the mixed state. By means of data-rooted analysis, we found that the sample vortex dynamics could be fully described within a single-component approach. Pinning phenomena were present and characterized by a depinning frequency smaller than the measurement ones. The multiband nature of the superconductor emerged in the flux-flow resistivity, whose field dependence could be interpreted well within theoretical models. By exploiting them, the upper critical field was extracted in the low-temperature range, which exhibited a consistent temperature trend with the values obtained at the onset of the resistive transition near Tc, and was well in line with literature data on other polycrystalline samples.

High density (99.5%) ceramic composite composed of titanium boride and boron carbide (70/30 vol%) was obtained by spark plasma sintering and was tested by 3-point bending test in Ar atmosphere at 1800 degrees C. Bending strength was high, around 1.1 GPa. The strength-strain curve presents a peculiar shape composed of three regions where elastic and plastic deformations are active with a different weight. Based on transmission electron microscopy observations we propose a process of mechanical energy absorption driven by shear stress in the boron carbide crystals: stacking faults with (1-11) and (011) stacking planes and twins with (1-11) twinning plane rearrange into nano-twins with (10-1) twinning planes, orthogonal but equivalent to the initial ones. This rearrangement mechanism provides in the first instance a plastic signature, but further contributes strengthening.

Romula (today Resca, Dobrosloveni Village, Romania) was the largest urban and economic center of Dacia Inferior (Malvensis), a Roman province located in the north of the Lower Danube region. In this context, the city market included workshops for the production of ceramic, metal, stone, bone, and glass objects. In 2013, 2015, and 2018, during excavations of the former Roman city, two rectangular glass furnaces were discovered. One has only one chamber, the other has two chambers. A melted glass layer was found on the walls of furnace no. 1, as well as in one room of furnace no. 2. Broken fragments of glass were also found in both. The furnaces are located in the central area of the Roman city. The evidence suggests that the furnaces belong to secondary glass workshops. The glass may have arrived in raw form, where it was remelted and processed. The discovery of these furnaces contributes to the growing body of evidence for Roman glass production around the empire.1

Mo matrix composites (MMC) with Mo-9Si-8B inclusions were fabricated by pressure-less sintering (PLS) and spark plasma sintering (SPS) techniques at temperatures between 1200-1500 degrees C using 1 wt.% Ni sinter additive. The positive impact of the addition Ni addition on the sinterability and formation of a continuous Mo matrix of MMC with randomly distributed Mo3Si and Mo5SiB2 inclusions was determined. The Ni addition increased the shrinkage of MMC during PLS by almost a third. The continuous Mo matrix of MMC and a relative density of more than 98% was obtained after SPS at 1400-1500 degrees C. The composite with the maximum relative density of 98% showed a Vickers hardness of 482 +/- 9 (HV20). The potential of using Ni-activated PLS and SPS to produce high-density MMC is shown.

Twenty years passed since the discovery of superconductivity in MgB2. Although there is much progress, the use of superconductors, in general, and of MgB2 in particular, remains limited. On the other hand, in the last 10 years MgB2 became a material of great interest for emergent applications, such as propellants, batteries, and catalysis, as a source material to obtain 2D borophene-like materials (e.g. BH borophane), biomedical field (taking advantage of its promising antimicrobial, antitumoral, biodegradable, and biocompatible features), heritage and ecology being the latest trends. These new directions place MgB2 as a material well integrated with nature cycles that can promote the concept of one eco- and health-friendly, with many envisioned practical purposes. This type of material is at the core of a clean and sustainable economy promoting new developments, boosting the older ones (e.g. superconductivity) and minimizing the costs for the transition to new and modern materials and technologies. In this work, we review recent trends and new directions of MgB2 applications and discuss their potential impact.

The use of superconducting (SC) materials is crucial for shielding quasi-static magnetic fields. However, the need for space-saving solutions with high shielding performance requires the development of a three-dimensional (3D) modelling procedure capable of predicting the screening properties for different orientations of the applied field. In this paper, we use a 3D numerical model based on a vector potential formulation to investigate the shielding ability of SC screens with cylindrical symmetry and a height/diameter aspect ratio close to unity, without and with the superimposition of a ferromagnetic (FM) circular shell. The chosen materials were MgB2 and soft iron. First, the outcomes of the calculations were compared with the experimental data obtained with different shielding arrangements, achieving a notable agreement in both axial field (AF) and transverse field (TF) orientations. Then, we used this validated modelling approach to investigate how the magnetic mitigation properties of a cup-shaped SC bulk can be improved by the superimposition of a coaxial FM cup. Calculations highlighted that the FM addition is very efficient in enhancing the shielding factors (SFs) in the TF orientation. Assuming a working temperature of 30 K and using a layout with the FM cup protruding over the SC one, SFs up to eight times greater than those with a single SC cup were attained at applied field up to 0.15 T, reaching values equal to or higher than 10(2) in the inner half of the shield. In the AF orientation, the addition of the same FM cup incurs a modest worsening at low fields, but at the same time it widens the applied field range where SF > 10(4) occurs near the close extremity of the shield to over 1 T.

This paper reports the synthesis and characterization of Cu2ZnSnS4 (CZTS) absorber films, prepared by a two-step electrodeposition of a ZnS (zinc sulfide) binary and a CZT (copper, zinc and tin) ternary precursors on Mo/Ti/Si substrates. The as-electrodeposited ZnS/CZT and CZT/ZnS stacks were thermally treated in a tubular furnace in sulfur environment at 550 degrees C. The role of the ZnS buffer layer is to provide a zinc and sulfur reservoir, needed to complete the formation of kesterite phase. X-ray diffraction and Raman analyses revealed the formation of the CZTS phase. The surface morphology and chemical composition of the films were studied using a scanning electron microscope. The bandgap values inferred from diffuse reflectance data, are discussed with respect to the stoichiometry which is considerably affected by the order of the stacks. Room-temperature photoluminescence of the CZT/ZnS sample showed a board PL band of 1.51 eV. It was found that the film with a ZnS layer on top is preferred for the formation of a Zn-rich single CZTS phase.

Sesquipedalian mud and burnt bricks (second to third century AD) were excavated from the Roman city of Romula located in the Lower Danube Region (Olt county, Romania). Along with local soils, bricks are investigated by petrographic analysis, X-ray fluorescence (XRF), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR), electron microscopy (SEM/EDX), X-ray microtomography (XRT), thermal analysis (DTA-TG), M.ssbauer spectroscopy, magnetometry, colorimetry, and mechanical properties assessment. The results correlate well with each other, being useful for conservation/restoration purposes and as reference data for other ceramic materials. Remarkably, our analysis and comparison with literature data indicate possible control and wise optimization by the ancient brickmakers through the recipe, design (size, shape, and micro/ macrostructure), and technology of the desired physical-chemical-mechanical properties. We discuss the Roman bricks as materials that can adapt to external factors, similar, to some extent, to modern "smart" or "intelligent" materials. These features can explain their outstanding durability to changes of weather/climate and mechanical load.

Two unreacted commercially available Nb3Sn precursor wires with different architecture were subject to a two-temperature heat treatment in vacuum at 650 degrees C for 72 h and at 700 degrees C for 168 h. Evolution of wires towards formation of the superconducting phase was assessed by the non-invasive X-ray computed microtomography (micro XRT) with a spatial resolution of similar to 2 mu m on the samples before and after the heat treatments. Statistical image analysis quantified the defects and quantitatively revealed the deviation of the geometrical perfection of the wire components comparative to designed parameters depending on the wire architecture and heat treatment conditions. Our results position XRT as a tool to evaluate the quality of Nb3Sn, also promoting it as a method capable for providing new insights that could be used in the optimization processes of Nb3Sn wires design, technology, and during operation.

High density (94-98% of the theoretical density) MgB2 samples added with C6H10Ge2O7 and cubic BN with compositions (MgB2)(1-x)(Ge2C6H10O7)(0.0028)(cBN)(x) (x = 0.003, 0.005, 0.007, 0.01) and (MgB2)(1-y)(Ge2C6H10O7)(y)(cBN)(0.005) (y = 0.0014, 0.0028, 0.005, 0.0075) were obtained by spark plasma sintering technique. For optimum doped samples with x = 0.005-0.007 and y = 0.0028-0.005, a weak enhancement of zero-field critical current density J(c0), irreversibility field H-irr, and volume pinning force F-p,F-max was determined. This behavior is very different from similar samples added with a single additive for which H-irr has a large enhancement. Consequently, it suggests the presence of opposite structural and microstructural effects induced by the additives. These effects, on the one hand, are discussed to decrease the sensitivity of MgB2 superconducting properties in the co-added samples comparative to samples added with C6H10Ge2O7, and, on the other hand, they contribute to anomalies that were found when assessing the pinning force-related parameters by the universal scaling law.

Zr0.8Sn0.2TiO4 powders synthesized by solid state reaction route have been consolidated by conventional and spark plasma sintering methods. Single-phase ceramics with various microstructures and, consequently, different extrinsic absorption were investigated by terahertz time-domain spectroscopy. The results showed that the terahertz spectroscopy can be used for tailoring in the " synthesis - microstructure - properties" cycle.

Polycrystalline MgB2 bulk samples were produced by ex-situ spark plasma sintering (SPS) using the oxygen-free preceramic polymer additive poly(dimethylsilane) as a source for carbon doping and as a sintering aid. Two major effects were identified. One is the significant enhancement of the densification kinetics during sintering for all tested compositions. The second one is the improvement of the high field critical current density for a certain level of the poly(dimethylsilane) addition.

Zr0.8Sn0.2TiO3 (ZST) powders synthesized by solid-state reaction were subject to processing by spark plasma sintering (SPS). A single-phase ceramic with a high relative density of 95.7% and 99.6% was obtained for sintering temperatures of 1150 degrees C and 1200 degrees C, respectively, and for a dwell time of 3 min. In order to reduce the oxygen vacancies, as-sintered discs were annealed in air at 1000 degrees C. The dielectric loss of the annealed samples, expressed by the Q x f product, measured in the microwave (MW) domain, varied between 35 THz and 50 THz. The intrinsic losses (Q x f ~ 60 THz) were derived by using terahertz time-domain spectroscopy (THz-TDS).

Bulk high density MgB2 and a composite material made of a PLA matrix and MgB2 powder inclusions were in vivo tested as candidates for biodegradable materials for orthopedic implants. A rat model was used. Implants were introduced into femoral bone, in transversal and longitudinal directions. Assessment of the implant-tissue interaction was performed by X-ray imaging, X-ray computer tomography, electron microscopy, cytology, and histopathology on samples at 40 and 90 days after surgery. Both materials are biocompatible, bone and adjacent soft tissue showing good tolerance of implants. Biodegradation of MgB2 is faster than for PLA-MgB2 composite, but in both cases, it is accompanied by bone regeneration. Results suggest that use of MgB2-containing composites can promote space and time control of degradation and promotes MgB2 as a promising material for fracture repair. (c) 2022 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

The consumer market requests infrared (IR) optical components, made of relatively abundant and environmentally friendly materials, to be integrated or attached to smartphones. For this purpose, three new chalcogenides samples, namely Ge23.3Zn30.0Se46.7 (d_GZSe-1), Ge26.7Zn20.0Se53.3 (d_GZSe-2) and Ba4.0Ge12.0Zn17.0Se59.0I8.0 (d_GZSe-3) were obtained by mechanical alloying and processed by spark plasma sintering into dense bulk disks. Obtaining a completely amorphous and homogeneous material proved to be difficult. d_GZSe-2 and d_GZSe-3 are glass-ceramics with the amount of the amorphous phase being 19.7 and 51.4 wt. %, while d_GZSe-1 is fully polycrystalline. Doping with barium and iodine preserves the amorphous phase formed by milling and lowers the sintering temperature from 350 degrees C to 200 degrees C. The main crystalline phase in all of the prepared samples is cubic ZnSe or cubic Zn0.5Ge0.25Se, while in d_GZSe-3 the amorphous phase contains GeSe4 clusters. The color of the first two sintered samples is black (the band gap values are 0.42 and 0.79 eV), while d_GZSe-3 is red (E-g is 1.37 eV) and is transparent in IR domain. These results are promising for future research in IR materials and thin films.

Pure and Er-doped hematite (alpha-Fe2O3) nanorods were prepared by a two-step method involving hydrothermal synthesis and calcination of pure and Er-doped goethite (alpha-FeOOH) nanorods. Substitution of Fe3+ by Er3+ in the crystal structure of hematite caused morpho-structural changes such as expansion of the unit cell and gradual shortening and rounding of hematite nanorods towards formation of nanoellipsoids. These changes induced modification of magnetic and optical properties suggesting the possibility of a systematic control of physical properties via rare earth substitution. A decrease in the hyperfine magnetic field, coercive field and Morin transition temperature, as well as an increase of the magnetic susceptibility and a narrowing of the optical band gap were observed by substitution. Intimate mechanisms related to the formation of more and more defect-like hematite phases with decreased temperatures for the transition to the low temperature antiferromagnetic phase at increased doping level were evidenced via temperature dependent Mo center dot ssbauer spectroscopy.

We report the mechanical behavior of a bulk boron ceramic prepared by spark plasma sintering of commercially available beta-boron powder. In order to fabricate polycrystalline boron ceramic, we used a protective tantalum foil reacted with carbon from the graphite die or graphite foil forming a thin layer of TaB2 and TaC covering the boron specimen. This is the first study to show the high-temperature flexural strength, toughness, and Young's moduli of boron up to 1400 degrees C. At 1600 degrees C and above, boron will react with testing environment forming an outer shell. The flexural strength and fracture toughness at room temperature reached an average of 340 MPa and 4.1 MPa m (1/2) , respectively. Despite showing clear signs of plastic deformation on the strain-stress curves, the yield strength of the monolithic boron ceramic exceed 1 GPa at 1200 degrees C. It was determined that fracture at elevated temperatures follows a quasi-transgranular mechanism, where the sub-grains of the boron fracture as plate-like structures. An interpretation for the observed fracture behavior was proposed.

Boron powders with Mg were coated with polytrifluorochloroethylene (PCTFE, fluorine content is 52.6 wt%) and perfluoropelargonic acid (PFPA, fluorine content is 69.6 wt%). They were used to fabricate propellants that were burnt in a reaction chamber designed and fabricated in our lab. Combustion products were studied by Raman spectroscopy, powder agglomeration analysis, electron microscopy, and thermal analysis. Results indicate that surface modification of the initial powder by fluorine-containing components decrease the agglomeration of the combustion products and the strongest effect is for PCTFE. Powders microstructural features and thermal stability of the coatings are discussed as being at the origin of different behavior during combustion of the propellants.(c) 2021 The Combustion Institute. Published by Elsevier Inc. All rights reserved.

The chemical precipitation was used to obtain carbon fibers (CF) with surface modified by magnetite particles (Fe3O4). Processing was carried out by employing up to three subsequent coating stages of ultrasonic treatments. After each sonication stage, the coating was 17, 33, and 47 wt. % of the total weight of the modified fibers. Raman spectroscopy indicates the presence in the coating of a mixture of iron II and III states. As-decorated fibers were used to fabricate composites with an epoxy resin (ED-20) matrix cured with PEPA. The quantity of the carbon fiber filler was of 1, 3, and 6 wt %. At room temperature, the saturation magnetization of the soft magnetic samples was 0.37, 0.83, and 1.72 emu/g for the indicated compositions. Carbon fiber reinforced polymer materials with extra functions such as magnetic in this case, are expected to be useful in applications from the power and energy industries.

The paper presents fabrication and characterization of spark plasma sintered textured (001) MgB2 with a record degree of orientation of about 40% and 16% by high-energy ultra-sonication and slip casting in high magnetic field (12 T) and 0 T magnetic field, respectively. Structural characterization was performed by X-ray diffraction, and electron microscopy. The analysis revealed unexpected preferred orientation also in the MgO secondary phase due to the epitaxial growth of (111) MgO on (001) MgB2. The influence of oriented microstructure on the superconducting characteristics expressed by critical current density (Jc), irreversibility field ( H irr), and on the pinning properties were assessed. High anisotropy versus sample orientation in applied magnetic field, H , was observed for Jc, Hirr, pinning activation energy ( U *) extracted from relaxation measurements. The zero-field critical current, Jc0 and Fp,maxare weakly or not dependent on the direction of H , while the other indicated parameters are significantly influenced. Results enable control of superconducting parameters by further optimization of microstructure through MgB2 texturing as a novel and viable strategy for development of bulk MgB2 with enhanced properties when taking advantage of its anisotropy.(c) 2021 Chongqing University. Publishing services provided by Elsevier B.V. on behalf of KeAi Communications Co. Ltd. This is an open access article under the CC BY-NC-ND license ( http://creativecommons.org/licenses/by-nc-nd/4.0/ ) Peer review under responsibility of Chongqing University

We report for the first time on the antimicrobial activity of MgB2 powders produced via the Reactive Liquid Infiltration (RLI) process. Samples with MgB2 wt.% ranging from 2% to 99% were obtained and characterized, observing different levels of grain aggregation and of impurity phases. Their antimicrobial activity was tested against Staphylococcus aureus ATCC BAA 1026, Enterococcus faecalis ATCC 29212, Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853, and Candida albicans ATCC 10231. A general correlation is observed between the antibacterial activity and the MgB2 wt.%, but the sample microstructure also appears to be very important. RLI-MgB2 powders show better performances compared to commercial powders against microbial strains in the planktonic form, and their activity against biofilms is also very similar.

Commercial nanopowders of MgB2 were characterized from the viewpoint of granulometric distribution, structure, microstructure, and pH behavior in water. The powders are very different: a higher amount of the MgB2 phase with a lower tendency for agglomeration determines a higher rate of pH-increase. A higher rate of pH-increase usually produces a stronger antimicrobial activity against Staphylococcus aureus, Enterococcus faecium, Escherichia coli, Pseudomonas aeruginosa, Candida albicans, and Candida parapsilosis reference strains. The variation of the pH-increase rate suggests the possibility of temporo-spatial control of MgB2 bioactivity, although the contribution of other factors should not be neglected. Remarkably, the efficiency of the MgB2 powders is higher against biofilms than on microbes in the planktonic state. Further, our experiments confirm the antimicrobial efficiency of MgB2 in the in vitro tests against 29 methicillin resistant clinical S. aureus isolates and 33 vancomycin resistant E. faecium/faecalis strains, but in this case the biofilms are more resistant than planktonic cells. The MgB2 treatment of infected mice led to a significant decrease of E. coli colonization in liver, spleen and peritoneal liquid and it also caused changes in the intestinal microbiota. The activity of powders on HeLa and HT-29 tumor cell lines was assessed by inverted microscopy, flow cytometry, and evaluation of the cellular cycle. MgB2 inhibits tumor cell growth influencing DNA synthesis (S-phase). The obtained results indicate that the tested powders could provide promising solutions for the development of large-spectrum multifunctional antimicrobial and anti-biofilm agents, and/or for anti-cancer therapies. (C) 2021 The Authors. Published by Elsevier B.V.

The 17th-19th century wooden and stone churches are an iconic symbol for the Romanian national heritage, raising urgent needs for the development of efficient and ecofriendly restoration and preservation solutions. Nanotechnology has a great but largely unexplored potential in this field, providing new tools and methods to achieve higher consolidation and protection efficiency, mainly due to the ability of nanoparticles to inhibit the growth and metabolic activity of different biodeteriorating agents, including fungi. The purpose of the present study was to report for the first time on the efficiency of MgB2 materials, mainly prized for their practical superconducting properties, against a large collection of filamentous fungal strains recently isolated from biodeteriorated wooden and stone heritage objects. Four types of MgB2 powders, with a crystallite size of 42-113 nm, were tested by qualitative (on 149 strains) and quantitative (on 87 strains) assays. The cytotoxicity was evaluated by the microscopic analysis of SiHa cells morphology and Hep2 cell cycle analysis and the ecotoxicity by the Allium test. The tested filamentous fungal strains belonged to 11 different genera, and those isolated from mural paintings and wooden objects exhibited the best capacity to colonize the inert substratum. All MgB2 powders exhibited similar and relatively low minimal inhibitory concentrations (MIC) values against the Aspergillus and Penicillium isolates, which were predominated among isolates. From the tested powders, PVZ and CERAC proved to be more efficient against the strains isolated from stone and wood materials, while LTS was active against the fungal strains colonizing the mural paintings and museum objects. The cytotoxicity results indicated that the tested powders are toxic for the human cells at concentrations higher than 50 mu g/ml, but, however, the very short lifetime of these NPs prevents their accumulation in the natural environment and, thus, the occurrence of toxic effects. The tested powders proved to be ecofriendly at the active antifungal concentrations, as suggested by the phytotoxicity test results. Taken together, our results suggest the potential of the MgB2 materials for the development of environmentally safe antifungal substances, which can be used in the control of the material cultural heritage biodeterioration process.

An analysis of the field dependence of the pinning force in different, high density sintered samples of MgB2 is presented. The samples were chosen to be representative for pure MgB2, MgB2 with additives, and partially oriented massive samples. In some cases, the curves of pinning force versus magnetic field of the selected samples present peculiar profiles and application of the typical scaling procedures fails. Based on the percolation model, we show that most features of the field dependence of the critical force that generate dissipation comply with the Dew-Hughes scaling law predictions within the grain boundary pinning mechanism if a connecting factor related to the superconducting connection of the grains is used. The field dependence of the connecting function, which is dependent on the superconducting anisotropy, is the main factor that controls the boundary between dissipative and non-dissipative current transport in high magnetic field. Experimental data indicate that the connecting function is also dependent on the particular properties (e.g., the presence of slightly non-stoichiometric phases, defects, homogeneity, and others) of each sample and it has the form of a single or double peaked function in all investigated samples.

Pottery vessels made of kaolin clay from the Roman Period (2nd, 3rd centuries CE) found in Romula (Re?ca village, Olt County, Romania) from Dacia Inferior (Malvensis) were investigated by petrographic, X-ray diffraction, X-ray fluorescence, thermal analysis, electron microscopy, and mechanical tests. Our results are compared with available data on kaolin clays and pottery vessels from other sites located along the lower course of Danube river and near the Black Sea, namely in Moesia Superior, Moesia Inferior, and Thracia. Archeological and geographical contexts are addressed. Results of our analysis suggest a local production of ceramics in Romula, by using raw materials from the north of Lower Danube, in opposition to the idea that kaolin ware was imported from the provinces south of the Danube.

Three commercial powders of MgB2 were tested in vitro by MTS and LDH cytotoxicity tests on the HS27 dermal cell line. Depending on powders, the toxicity concentrations were established in the range of 8.3-33.2 mu g/ml. The powder with the lowest toxicity limit was embedded into polyvinylpyrrolidone (PVP), a biocompatible and biodegradable polymer, for two different concentrations. The self-replenishing MgB2-PVP composite materials were coated on substrate materials (plastic foil of the reservoir and silicon tubes) composing a commercial urinary catheter. The influence of the PVP-reference and MgB2-PVP novel coatings on the bacterial growth of Staphylococcus aureus ATCC 25923, Enterococcus faecium DMS 13590, Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853, in planktonic and biofilm state was assessed in vitro at 6, 24, and 48 h of incubation time. The MgB2-PVP coatings are efficient both against planktonic microbes and microbial biofilms. Results open promising applications for the use of MgB2 in the design of anti-infective strategies for different biomedical devices and systems.

Pristine high-density bulk disks of MgB2 with added hexagonal BN (10 wt.%) were prepared using spark plasma sintering. The BN-added samples are machinable by chipping them into desired geometries. Complex shapes of different sizes can also be obtained by the 3D printing of polylactic acid filaments embedded with MgB2 powder particles (10 wt.%). Our present work aims to assess antimicrobial activity quantified as viable cells (CFU/mL) vs. time of sintered and 3D-printed materials. In vitro antimicrobial tests were performed against the bacterial strains Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853, Staphylococcus aureus ATCC 25923, Enterococcus faecium DSM 13590, and Enterococcus faecalis ATCC 29212; and the yeast strain Candida parapsilosis ATCC 22019. The antimicrobial effects were found to depend on the tested samples and microbes, with E. faecium being the most resistant and E. coli the most susceptible.

Partially-oriented MgB2 bulk discs (13 and 9 %) with the starting compositions of (MgB2)(0.99)(B4C)(0.01) and (MgB2)(0.99)(c-BN)om were fabricated by slip casting under an H-0 = 12 T magnetic field (perpendicular to the disc surface) and subsequent spark plasma sintering. The maximum critical current density and irreversibility field are for H//H-0 (H=applied field). These values are higher or similar to the randomly-oriented samples with the same composition. The maximum volume pinning force (F-p) is lower in the partially-oriented ones than in the randomly-oriented samples. The pinning-force-related parameters depend on the additive and orientation. Assessment of the major pinning mechanism within the scaling and percolation models considering these parameters shows significant limitations. A method to scale F-p is proposed; for the randomly and partially-oriented samples (that show an extra peak in F-p), the single and double Gaussian functions fit well. The results suggest an anisotropic influence of carbon substituting for boron in the MgB2.

Dense samples (94-96%) with starting composition (MgB2)(0.99)(X-acac)(0.01) (X-acac denotes Ga or In acetylacetonate) were obtained by spark plasma sintering. The resulting material is a superconducting composite, where carbon substitutes for boron in the crystal structure of MgB2. Added samples show enhanced critical current density at high magnetic fields and this is reflected in high values of irreversibility field (H-irr) at temperatures below 25 K when compared to a pristine sample. More efficient is In-acac addition and it promotes a H-irr of similar to 12.4T (100 A/cm(2) criterion) at 5 K. Carbon substitution for boron in the crystal structure of MgB2 has a strong influence on the pinning force and its related parameters and promotes in the added samples a grain boundary pinning mechanism as the dominant one, whereas the pristine sample with a low amount of carbon shows a major mechanism of point pinning type. However, our analysis indicates on the synergetic effects of the carbon substituting for boron and of the microstructural details on pinning and critical current density. The result strongly emphasizes the significantly different behavior of the additive during processing of the MgB2 samples, although thermal analysis experiments on both additives show very similar decomposition patterns. (C) 2020 The Authors. Published by Elsevier B.V.

Nanocrystalline PdO films have been characterized by X-ray diffraction, scanning electron microscopy, and electron probe microanalysis. The results demonstrate that thermal oxidation in an O-2 atmosphere causes similar to 35-nm-thick nanocrystalline Pd films on SiO2/Si(100) substrates to undergo a sequence of phase transformations resulting in PdO formation, followed by PdO decomposition into metallic Pd atT > 1120 K. In the range 670-970 K, theaandctetragonal cell parameters of the nanocrystalline PdO films increase monotonically with increasing temperature. The present and previously reported data have been used to construct a model for the unit cell in the crystal structure of palladium(II) oxide. Based on the quasi-chemical approach, we propose a model that accounts for the observed increase in the tetragonal cell parameters and thep-type conductivity of the nanocrystalline PdO films in terms of the formation of excess interstitial oxygen atoms.

The second magnetization peak (SMP) in the fourfold symmetric superconducting single crystals (such as iron pnictides and tetragonal cuprates) has been attributed to the rhombic-to-square transition (RST) of the quasi-ordered vortex solid (the Bragg vortex glass, BVG). This represents an alternative to the pinning-induced BVG disordering as the actual SMP mechanism. The analysis of the magnetic response of BaFe2(As1-xPx)(2) specimens presented here shows that the SMP is not generated by the RST. However, the latter can affect the pinning-dependent SMP onset field if this is close to the (intrinsic) RST line, through the occurrence of a "shoulder" on the magnetic hysteresis curves m(H), and a maximum in the temperature variation of the DC critical current density. These features disappear in AC conditions, where the vortex system is dynamically ordered in the RST domain, emphasizing the essential role of vortex dislocations for an efficient accommodation of the vortex system to the pinning landscape and the SMP development. The m(H) shoulder is associated with a precipitous pinning-induced proliferation of dislocations at the RST, where the BVG elastic "squash" modulus softens. The DC magnetization relaxation indicates that the pinning-induced vortex system disordering continues above the RST domain, as the basic SMP mechanism.

Almost six decades ago, in Romania a small group of physicists begun to study chalcogenide compositions, motivated primarily by the desire to understand the phase-change phenomenon in these materials, discovered recently, at that time, by Stanford R. Ovshinsky. It took not too long for them to realize the challenges these materials set to the research. With newcomers to the field, the research was broadened. In some cases just for basic research, to model, and to understand the chalcogenide materials, whereas in other cases, the applicative potential was revealed and used. Herein, the evolution of the field of these somewhat exotic materials is followed, listing the main contributions done in Romania, both in basic and applied research.

MgB2 has great potential for many applications, thanks to its relatively high critical temperature and low fabrication cost. Large efforts are done to improve the current carrying capabilities of bulks and tapes in view of different application fields, e.g. with the addition of Te and cubic-BN to MgB2. To elucidate the vortex pinning physics exploiting a different dynamic regime, we present here a microwave study of the pinning properties of spark plasma sintered bulk MgB2 with and without the addition of 0.01 % at. Te or cubic-BN. We show the surface resistance R-s of the MgB2 samples measured with a dielectric-loaded resonator at similar to 16.5 GHz and similar to 26.7 GHz in the 10 K-Tc temperature range at fields up to 1.0 T. Then, the MgB2 R., is studied with high frequency vortex motion models in order to obtain the pinning constant (Labusch parameter) and the depinning frequency. Finally, the microwave behavior of MgB2 in the mixed state is compared with the recent results obtained on Nb3Sn.

MgB2 bulk superconductors are expected to be utilized as rare-earth-free and lightweight trapped field magnets. However, the flux jumps frequently happen during the magnetizing processes, and heavily degrade the field-trapping performances. We have investigated the effect of additives to the MgB2 bulk samples prepared by spark plasma sintering process, and observed various flux jumps during the pulsed field magnetizing processes, which were carried out at 14 K which was obtained by the 2-stage GM cryocooler. The authors classified the flux motions as three categories as "no flux flow", "fast flux flow", and "flux jump" regions, and investigated the conditions where the flux jumps happen. We observed some drastic flux jumps in the pristine and clarified the effect of graphene addition to the flux jumps. The experimental results showed us a possible expansion of no flux jump region, and suggested us the improvement of field trapping capability.

Eutectic particles of B4C-TiB2 were reinforced with Ti by spark plasma sintering (SPS) or infiltration. The SPSed samples with 20, 30 and 40 wt. % Ti consisted of ceramic phases, and had a bicontinuous macrostructure formed by the Ti-rich region and the eutectic particles region, while the infiltrated sample was a complex composite comprised of a 3D Ti-rich continuous network, composite in nature, that contained Ti-metal and in which are embedded isolated ceramic (eutectic) particles. The SPSed samples are brittle with the maximum bending strength of 300 MPa for the 30 wt. % Ti, higher than for a reference sample produced by SPS from directionally solidified eutectic particles. A higher amount of added Ti results in a higher displacement in the bending test suggesting a higher fracture toughness. Simultaneous strengthening and toughening of the composite was realized. The infiltrated sample was ductile, while its bending strength (220 MPa) was comparable to the values measured for the brittle as-introduced reference sample and the sample with 20 wt. % Ti, both produced by SPS. In the SPSed and infiltrated samples at the interface between the Ti-rich region and B4C-TiB2 eutectic particles, a local 'pull-out' intergranular fracturing mechanism mainly involving Ti-B 1D-grains was observed. This local micromechanism together with a 'pull out' macromechanism of the eutectic grains from the Ti-rich component are considered important for the bridging/anchoring behavior responsible for the strengthening and toughening processes in our novel hierarchical composites.

Bulk discs (20 mm diameter and 4.3 mm thickness) of MgB2 added with Ge2C6H10O7 were obtained by Spark Plasma Sintering. Six samples with composition Mg B 2 (Ge2C6H10O7)(0.0014) and one undoped sample were fabricated under similar conditions and were magnetically characterized in order to determine the scattering of properties and reproducibility. The main source of the scattering of the properties is the decomposition of the additive due to elimination of the organic part in gas form, which occurs stepwise with intensive vacuum drops at around similar to 560 and similar to 740 degrees C. A third drop, which is sometimes not well resolved being part of the second peak at 740 degrees C, occurs at similar to 820 degrees C. The critical temperature at the midpoint of the transition, T-C, shows only a relatively small variation between 37.4 and 38 K, and the irreversibility field at a low temperature of 5 K takes values between 8 and 10 T. The pinning force and pinning force related parameters do not correlate with the carbon substituting for boron in MgB2 and suggest a synergetic influence of the microstructural details and carbon. Overall, despite the superconducting properties scattering, the samples are of high quality. Stacked into a column of six samples, they can trap at the center and on the surface of the column a magnetic field of 6.78 and 5.19 Tat 12 K, 5.20 and 3.98 Tat 20 K and 2.39, and 1.96 Tat 30 K. These promising values, combined with facile fabrication of the samples with relatively high quality and reproducibility, show the feasibility of their use in building complex and large compound arrangements for bulk magnets and other applications.

This work involves the synthesis and characterization of Cu2ZnSnS4 (CZTS) layers. The films were prepared on Mo/glass substrates by single-step electrodeposition method followed by sulfurization at 500 degrees C under argon flow. The effect of boric acid concentration on the crystallographic structure, compositional and morphological properties of CZTS films was investigated, with the objective to understand the growth behavior and to enhance the film properties. Cyclic Voltammetry was used in order to estimate the adequate deposition potential for the CZT alloy. The x-ray diffraction analysis showed the formation of the kesterite phase in all the samples. The Raman and x-ray photoelectron spectroscopy studies confirmed the existence of the CZTS phase. The scanning electron microscopy was employed to inspect the films structure. The results indicated that increasing the concentration of boric acid affects the physico-chemical properties of the films.

Grain boundaries, twins, and defects are considered to influence the thermomechanical behavior of any covalent ceramic, as a result, monolithic B4C samples show different curve shapes of bending strength vs temperature and the present theoretical models fail to fit them over the entire temperature range. To overcome these issues, we fabricated a novel high-density boron carbide and evaluated its high-temperature bending strength. The as-obtained ceramic is composed of boron carbide grains and a fine grain-boundary metal Pt framework. The material shows a decreased strength, which is due to a non-linear increase in the volume expansion coefficient of the B4C. Recovery in strength above 1000 degrees C is due to the presence of twins, their growth and rearrangements. We consider twins rearrangements are the pieces of evidence for a novel 'micro' mechanism of high-temperature stress accommodation for the boron carbide bulks.

Superconductors are key materials for shielding quasi-static magnetic fields. In this work, we investigated the shielding properties of an MgB2 cup-shaped shield with small aspect-ratio of height/outer radius. Shape and aspect-ratio were chosen in order to address practical requirements of both high shielding factors (SFs) and space-saving solutions. To obtain large critical current densities (J(c)), which are crucial for achieving high magnetic-mitigation performance, a high-purity starting MgB2 powder was selected. Then, processing of the starting MgB2 powder into high density bulks was performed by spark plasma sintering. The as-obtained material is fully machinable and was shaped into a cup-shield. Assessment of the material by scaling of the pinning force showed a non-trivial pinning behaviour. The MgB2 powder selection was decisive in enlarging the range of external fields where efficient shielding occurs. The shield's properties were measured in both axial- and transverse-field configurations using Hall probes. Despite a height/outer radius aspect ratio of 2.2, shielding factors higher than 10(4) at T = 20 K up to a threshold field of 1.8 T were measured in axial-field geometry at a distance of 1 mm from the closed extremity of the cup, while SFs > 10(2) occurred in the inner half of the cup. As expected, this threshold field decreased with increased temperature, but SFs still exceeding the above mentioned values were found up to 0.35 T at 35 K. The shield's shape limits the SF values achievable in transverse-field configuration. Nevertheless, the in-field J(c) of the sample supported SFs over 40 at T = 20 K up to a field of 0.8 T, 1 mm away from the cup closure.

Solid-state reaction synthesized Zr0.8Sn0.2TiO3 powders have been compacted by spark plasma sintering. In order to reduce the oxygen vacancies, the sintered samples were annealed ex-situ in air. Single-phase ceramics with different amount of oxygen vacancies and, consequently, different extrinsic absorption were investigated by terahertz time-domain spectroscopy. The results showed that the terahertz spectroscopy could be a suitable technique for tailoring the absorption properties of the spark plasma sintered materials.

We report on a combined experimental and modelling approach towards the design and fabrication of efficient bulk shields for low-frequency magnetic fields. To this aim, MgB2 is a promising material when its growing technique allows the fabrication of suitably shaped products and a realistic numerical modelling can be exploited to guide the shield design. Here, we report the shielding properties of an MgB2 tube grown by a novel technique that produces fully machinable bulks, which can match specific shape requirements. Despite a height/radius aspect ratio of only 1.75, shielding factors higher than 175 and 55 were measured at temperature T = 20 K and in axially-applied magnetic fields mu H-0(appl) = 0.1 and 1.0 T, respectively, by means of cryogenic Hall probes placed on the tube's axis. The magnetic behaviour of the superconductor was then modelled as follows: first we used a two-step procedure to reconstruct the macroscopic critical current density dependence on magnetic field, J(c)(B), at different temperatures from the local magnetic induction cycles measured by the Hall probes. Next, using these J(c)(B) characteristics, by means of finite-element calculations we reproduced the experimental cycles remarkably well at all the investigated temperatures and positions along the tube's axis. Finally, this validated model was exploited to study the influence both of the tube's wall thickness and of a cap addition on the shield performance. In the latter case, assuming the working temperature of 25 K, shielding factors of 10(5) and 10(4) are predicted in axial applied fields it mu H-0(appl) = 0.1 and 1.0 T, respectively.

Polycrystalline In2S3 thin films have been grown on SnO2/glass substrates by chemical bath deposition technique and irradiated at different high gamma doses 3, 7, 15 and 40 kGy. X-ray diffraction, Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy (EDS), Spectrophotometer, Photoluminescence and Thermoluminescence were used to investigate physical properties of In2S3 thin films induced by gamma irradiation. After being irradiated, structural properties of In2S3 thin films have shown that preferred orientation has been moved from (4 0 0) plan at 2 theta(1)=33.42 degrees to a new created orientation at 2 theta(2)=38.06 degrees for 40 kGy gamma dose. EDS analysis has shown that atomic percentage (S/In) has been strongly varied for 40 kGy which indicate significant changes in stoichiometry. Thermoluminescence of irradiated In2S3 thin films has revealed a good sensitivity toward absorbed gamma dose. After irradiation, optical transmittance of In2S3 thin films has been increased from 50% to a maximum value of 70% in the visible range for 15 kGy dose. Band gap energy E-g has been slightly decreased. Other optical parameters such absorption and extinction coefficients, refractive index and permittivity have been determined. These experimental results show that gamma radiations can be used for tuning physical properties of In2S3 thin films for photovoltaic applications.

Mixtures of B4C, alpha-AlB12 and B powders were reactively spark plasma sintered at 1800 degrees C. Crystalline and amorphous boron powders were used. Samples were tested for their impact behavior by the Split Hopkinson Pressure Bar method. When the ratio R = B4C/alpha-AlB12 >= 1.3 for a constant B-amount, the major phase in the samples was the orthorhombic AlB24C4, and when R < 1 the amount of AlB24C4 significantly decreased. Predictions that AlB24C4 has the best mechanical impact properties since it is the most compact and close to the ideal cubic packing among the Al-B-C phases containing B-12-type icosahedra were partially confirmed. Namely, the highest values of the Vickers hardness (32.4 GPa), dynamic strength (1323 MPa), strain and toughness were determined for the samples with R = 1.3, i.e., for the samples with a high amount of AlB24C4. However, the existence of a maximum, detectable especially in the dynamic strength vs. R, indicated the additional influence of the phases and the composite's microstructure in the samples. The type of boron does not influence the dependencies of the indicated mechanical parameters with R, but the curves are shifted to slightly higher values for the samples in which amorphous boron was used.

Boron carbide added with 0-20 wt% carbon fibers was subject to Si infiltration. Samples mainly consist of B13C2, beta-SiC and unreacted Si. Some amount of SiB6 and alpha-SiC was also detected, while formation of B-12(B,C,Si)(3) phase was suppressed due to short infiltration time. The carbon fibers react with Si and result in formation of a composite core-shell fiber with SiC-shell and C-core. Theoretical estimations suggest that these composite fibers have a strong influence on the enhancement of the bending strength. Although apparently in good agreement with experimental data showing an increase of bending strength up to 510 +/- 27 MPa in the sample with 10 wt% carbon fiber, the implications of phase changes with the carbon fiber amount has to be carefully considered. At higher amounts of carbon fibers, bending strength decreases.

Plates of NiTi chemically etched, electro-polished, and sol gel coated with XO2 (X =Ti, Si, Zr), or coated with oxides and dip-coated polymers of Dextro-Levo-lactide-co-glycolide (DL-PLG, 0.4 mu m thickness), Dextro-Levo-lactic acid (DL-PLA, 1.3 mu m) or poly methyl methacrylate polymer (PMMA, 1.7 mu m) were obtained. Smooth and uniform NiTi surfaces without significant pitting, as revealed by AFM, were prepared for chemical etching of 120 s in HF:HNO3:H2O = 1:5:4, followed by electropolishing 120 s in H2SO4:CH3OH:H2O = 1:4:5 electrolyte and using a potential of 9 V. Dip-coated layer of PMMA has shown cracks and large pores and was eliminated from further experiments. Samples of pristine and coated NiTi were in vivo implanted into rabbits and extracted after 10 and 60 days. Clinically, all implants are biocompatible; all rabbits survived and a recovery process was observed for all cases. NiTi covered with SiO2, DL-PLG and SiO2/DL-PLG have shown the best healing evolution. For 10 and 60 days good recovery was found also for NiTi coated with TiO2. Coatings of ZrO2 and ZrO2/DL-PLG have shown the poorest results. The oxide coating and the roughness R-ZJIS that contains information on the 'deep' large areas in the coatings show the strongest influence on the healing processes. Work indicates the possibility of space- and time- scale controlled variation of the functional properties. (C) 2018 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda.

The work demonstrates growth by the Verneuil method of SrTiO3 single crystals of 30 mm in diameter. Experiments are performed under an industrial environment. Growth was for 4.75 h, i.e., within one production shift. The optimum growth conditions for which the length of the region with bubbles D is zero and the effective length EL (i.e., the crystal length of commercial value) is maximized are for the amount of SrCO3 additive of similar to 3 wt % and for H-2 outer flow rate of similar to 35 L/min. These two parameters show the strongest influence on the bubble-free growth, but other growth parameters (H-2 inner flow rate, O-2 flow rate increase, rotation speed) were also optimized. Selected crystals are characterized from the structural, microstructural, optical, and THz spectroscopy viewpoints, and they are compared with a commercial substrate and with crystals reported in the literature. This work opens the possibility for the industrial growth of large SrTiO3 single crystals and commercialization of large area substrates.

MgB2 green bodies were prepared by magnetic field slip casting in ethyl alcohol with added polyethyleneimine dispersing agent under a high magnetic field, mu H-0(0) = 12 T. Samples were further processed by spark plasma sintering (SPS) and characterized for superconducting properties. Slip casting provides texturing of MgB2 (the degree of c-axis orientation is approximately 3.5%), which is further increased significantly (to about 21%) in the SPSed sample. The critical current density (J(c)) displays anisotropy relative to the orientation of the measuring magnetic field. Specific features of J(c)(H, T) and of the pinning force extracted from magnetic measurements with the field parallel and perpendicular to H-0 are discussed.

This research work is dedicated to study structural, morphological, optical and photoluminescence properties of samarium doped calcium sulfate (CaSO4) thin films after exposure to high gamma radiations. Polycrystalline doped CaSO4 thin films have been grown on glass substrates by spray pyrolysis technique and irradiated at different high gamma doses 3, 7, 15 and 40 kGy. Physical characterization of irradiated thin films has been made by X-ray diffraction, Spectrophotometer, Scanning Electron Microscope, Energy Dispersive Spectroscopy, Fluorescence Spectrometer and Thermoluminescence. The most remarkable result, as shown by structural analysis, is the increase of grain size from 52 to a maximum value of 93 nm for 15 kGy gamma dose which indicates a clear enhancement in crystal structure by gamma irradiation. Moreover, the preferred orientation has been immediately changed from (102) plan to (100) just after the first 3 kGy gamma dose. SEM micrographs of irradiated thin layers show deep modifications in surface morphology. Optical transmission spectra have shown a sharp and intense peak at 350 nm wavelength. Band gap energy has been slightly decreased from 3.9 eV before irradiation to 3.6 eV for 40 kGy. A new and strong energy level noted E r , has been emerged and created due to high gamma irradiations in addition to the principal one relative to band gap energy. Other parameters like absorption and extinction coefficients and refractive index have been determined. Thermoluminescence data show a high sensibility to gamma radiations doses which offer opportunities for dosimetry applications. These experimental results suggest the use of irradiated samarium doped calcium sulfate as optical window for space photovoltaic devices where gamma rays are abundant. These results are also helpful for researchers using CaSO4 thin films near nuclear apparatus (nuclear reactors and particle accelerators) or those interested in studying interaction between radiations and condensed matter.

Thin films of (117) Bi2Sr2Ca2CuO8+ (Bi-2212) were grown by Molecular Organic Chemical Vapor Deposition (MOCVD) on (110) SrTiO3 and (110) LaAlO3 substrates. Substrates were vicinal with off angles up to 20 degrees. Films are 3D epitaxial and X-ray diffraction phi- scans demonstrate that, while the films grown on a flat substrate are composed of twinned grains, the films on vicinal substrate are twin-free. A higher quality is obtained if growth is performed at two temperatures: Growth starts at 550-600 degrees C and continues at 700-750 degrees C. The twin-free film grown by the two-temperature method shows a zero-resistance critical temperature of 37 and 32 K when the measuring current is applied in-plane parallel and perpendicular to [001] direction of the substrate. Twin-free non c-axis thin films are promising for fabrication of novel planar THz devices.

We explored in-gap states (IGSs) in perovskite oxide heterojunction films. We report that IGSs in these films play a crucial role in determining the formation and properties of interfacial two-dimensional electron gas (2DEG). We report that electron trapping by IGSs opposes charge transfer from the film to the interface. The IGS in films yielded insulating interfaces with polar discontinuity and explained low interface carrier density of conducting interfaces. An ion trapping model was proposed to explain the physics of the IGSs and some experimental findings, such as the unexpected formation of 2DEG at the initially insulating LaCrO3/SrTiO3 interface and the influence of substitution layers on 2DEG.

Short powder-in-tube tapes of MgB2 in the Fe sheath were fabricated by ex situ route from a commercial powder containing some free Mg and MgO impurity phases. The final heat treatment was performed by spark plasma sintering (SPS). Tapes were with open (OT) or closed (CT) endings. Closed endings were made by folding and pressing. The MgB2 core of the OT sample has shown a higher low-field critical current density, a higher maximum pinning force, a slightly higher disorder, smaller average MgB2 crystallite size, a weak contact between Fe and MgB2 core, and more macro-flux jumps. The upper and irreversibility fields were similar for OT and CT samples. In the center of the MgB2 cores, the detected impurity phase is MgO, while at the interface with Fe, MgB4 also occurs. Impurity phases found at interface, MgO and MgB4, are present in the center of the bulk SPSed samples. Reactions and pinning-force-related parameters are discussed with respect to Mg behavior influenced by condition of endings. It is inferred that the presence of free Mg in the raw MgB2 powder has an important contribution to observed differences, and its removal or control is recommended.

Four Ge-based organometallic (OM = C6H10 Ge2O7) polymers with similar chemical composition were used as additions for MgB2. MgB2 (OM) 0.0014 dense samples with a relative density higher than 97% were obtained by ex situ spark plasma sintering. The critical current density and the irreversibility magnetic field of the added samples are slightly improved at high magnetic fields by repagermanium (Alfa Aesar) addition when compared to the pristine reference sample. Addition of Ge-straight-chain polymer shows some improvement of the maximum volume pinning force, F-p (max). There is no significant Ge substitution in the crystal lattice of MgB2, while C substitutes for B. Pinning mechanism is mainly of a point pinning type, with the grain boundary pinning mechanism strengthening at lower temperatures and when additives are not used. A relatively high amount of carbon in the samples washes out the Ge effects on pinning-force-related parameters. The structure and morphology of the polymer additive play an important role in dispersion when mixing, impacting the quality of the superconducting properties. The nanosize dimension of the pristine MgB2 powder shows also some drawbacks in mixing and sintering.

Co-doped CeO2 thin films were grown from a bulk target with starting composition Ce0.95Yb0.04Er0.01O2 by pulsed laser deposition (PLD) on a p(+)-n-n(+) single crystal silicon diode. The PLD laser fluence was varied between 1.7 J/cm(2) and 3.7 J/cm(2). The device with the film grown for a laser fluence of 2.3 J/cm(2) delivers the highest performance taking advantage of the up conversion (UC) effect provided by this film. Namely, the increase in the relative power conversion efficiency of the device is 12.1% and 39.2% for illumination under 1 and 2.1 sun, respectively, and its relative external quantum efficiency is 8.2% when illuminated with 980 nm light. The film grown for the optimum 2.3 J/cm(2) fluence shows good target-film composition transfer and a granular morphology with a low roughness. The UC mechanism consists of efficient energy transfer between spatially separated Yb3+ and Er3+ ions, i.e. the absorption of infrared light photons by the Yb3+ ions (F-2(7/2) -> F-2(5/2) transition) is followed by a two-step energy transfer process to neighboring Er3+ ions and by their characteristic luminescent emissions ((H-2(11/2), S-4(3/2)) -> I-4(15/2)) and (F-4(9/2) -> I-4(15/2)).

Samples of MgB2 with relative density above 95% were obtained by spark plasma sintering (SPS) at 1150 A degrees C for a heating time of 100 A degrees C/min and a maximum pressure of 95 MPa. Dwell time was of 1, 4, 7, 10, and 20 min. Samples show that dwell time has a low influence on superconducting characteristics. However, small differences were observed and they are discussed from the viewpoint of density, structural, microstructural, critical current density, irreversibility field, and pinning type. The dominant contribution for all investigated samples is given by point and delta T (c) pinning.

Pristine and (SiC + Te)-added MgB2 powders, green and spark plasma sintered (SPS) compacts were investigated from the viewpoint of quasi-static and dynamic (Split-Hopkinson Pressure Bar, SHPB) compressive mechanical properties The amount of the additive (SiC + Te) was selected to be the optimum one for maximization of the superconducting functional parameters. Pristine and added MgB2 show very similar compressive parameters (tan delta, fracture strength, Vickers hardness, others) and fragment size in the SHPB test. However, for the bulk SPSed samples the ratio of intergranular to transgranular fracturing changes, the first one being stronger in the added sample. This is reflected in the quasi-static K-IC that is higher for the added sample. Despite this result, sintered samples are brittle and have roughly similar fragmentation behavior as for brittle engineering ceramics. In the fragmentation process, the composite nature of our samples should be considered with a special focus on MgB2 blocks (colonies) that show the major contribution to fracturing. The Glenn-Chudnovsky model of fracturing under dynamic load provides the closest values to our experimental fragment size data.

Fabrication methods are important way to improve structural and superconducting properties of MgB2 such as critical current, magnetic levitation force (MLF) and magnetic field trapping capability. Although the graded fabrication technique has been used for single-grain bulk YBCO superconductor to improve critical current and bulk superconducting properties, similar technique as regional doping has not been used for bulk MgB2, until now. In this study, nanoparticle silver doping was carried out in to the bulk MgTi0.06B2 superconductor by using in-situ solid state reaction and partial graded (regional) doping method together, to improve the radius independent uniform bulk current density and the magnetic levitation force as well as the structural properties of the MgB2 bulk superconductors. Both the J(c)(0) self-field critical current and F-p (mu H-0) pinning force density values enhanced in comparison with the inner region values, when the nanoparticle Ag doping is carried out in to the outer section of the sample. Addition to the enhancement of the structural and the micro electromagnetic properties as J(c)(0) and Fp (mu H-0), our study also focused on the improved of the bulk Jc and the radius of shielding current loop r, to improve bulk electromagnetic properties as the levitation force. It is seen that the structural properties enhanced and both the vertical levitation force and the lateral guidance force value increased with Ag doping to the outer section of MgTi0.06B2 sample. On the other hand, the increasing ratio of the lateral guidance force of 19.7% and the vertical levitation force of 10.8% of the sample with 3 wt% Ag-doped than the undoped one points out that the regional doping method to the outer section is very suitable for guidance force applications, which is important in the magnetic bearing application such as Maglev and magnetic energy storage systems. (C) 2017 Elsevier B.V. All rights reserved.

Additives to MgB2 can improve the superconducting functional characteristics, such as critical current density (J (c)) and irreversibility field (H (irr)). Recently, we have shown that repagermanium (C6H10Ge2O7) is an effective additive, enhancing both J (c) and H (irr). To look into details of the processes taking place during the reactive sintering, a thermal analysis study (0.167 K s(-1), in Ar) is reported. We used differential scanning calorimetry between 298 and 863 K and simultaneous thermogravimetric-differential thermal analysis between 298 and 1233 K. Samples were mixtures of powders with composition 97 mol% MgB2 and 3 mol% C6H10Ge2O7. Up to 863 K, repagermanium decomposes by multiple steps and forms amorphous phases. A reaction with MgB2 is not observed. Above this temperature, partial decomposition of MgB2 occurs. Crystalline Ge and MgO are detected before formation of Mg2Ge and MgB4, when temperature approaches the melting point of Ge (1211 K). Carbon substitution for boron in the crystal lattice of MgB2 is observed for samples heated above 863 K. The amount of substitutional C does not significantly change with temperature.

High-density (92-98% of the theoretical density) MgB2 samples added with Sb2O5 ((MgB2)+ (Sb2O5) x, x = 0, 0.0025, 0.005, 0.015) were obtained by Spark Plasma Sintering. A higher amount of additive decreases density. In added samples, grains of secondary phases are located at MgB2 grain boundaries and they are of large size. Hence, Sb2O5 does not promote effective flux pinning, connectivity is lower, and this suppresses the critical current density and the irreversibility field. Pinning force-related parameters indicate that added samples are close to the point pinning region and they show a higher grain boundary pinning contribution when compared with pristine MgB2 sample and when temperature is lower. It is speculated that for fixed processing conditions and Sb-oxide phases, a lower stability of the additive, reflected by a lower melting temperature, may promote reactive processes to start earlier leading to coarsening of the grains belonging to secondary phases.

Green compacts of B4C or B4C added with 1 vol% graphite were infiltrated with molten Si and subsequently were subject of processing by floating zone partial re-melting (FZPR). In FZPR only the low temperature fusible component, in this case Si, is melted. A fully dense B4C-based ceramic is obtained. It contains free-Si, SiC and B4C. In the center of the FZPR ceramic without graphite addition, the amount of Si is decreased when compared to the infiltrated material. Some impurity elements such as Al, Fe, or Ti detected in the raw B4C powder are preferentially gathered at the edges of the sample. In the sample added with graphite, formation of a high amount of SiC in the infiltrated material hinders Si shift from the center to the edges. The pulling rate and the particle size of the B4C raw powders are also important. It is recognized that sintering of powders larger than 10-20 gm is usually difficult: our approach is demonstrated to be suitable for processing of B4C powders with a very different particle size, from 10 to 250 gm. The FZPR ceramic had a Vickers hardness of 9-38 GPa depending on location of the indentation imprint and on the sample. A tensile strength of 114-188 MPa that is up to about 2-3 times higher than for the infiltrated material was recorded. Work indicates that the proposed processing approach offers extended control possibilities towards fabrication of new composite materials not available by traditional technologies.

Commercial MgB2 powder was loaded into a Fe-tube, by plastic deformation a tape of similar to 0.5 mm in thickness and 6.9 mm in width was obtained. Short pieces were processed by Spark Plasma Sintering (SPS) at 950, 1050 and 1150 degrees C for 3 min. The optimum sintering temperature is 1050 degrees C. From magnetic/electrical measurements, the onset critical temperature and the irreversibility field at 5 K were 38.7 / 38.9 K and 6.2 / 13.5 T, respectively. The pinning-force-related parameters indicate that the dominant flux pinning mechanism is of point pinning type. Contribution of grain boundary pinning is stronger at lower temperatures.

We investigated the evolution of the DC magnetic hysteresis curves of Nb0.89Ti0.11 alloys thermo-mechanically processed by intermediate heat treatments at 900 degrees C in vacuum and cold rolling (similar to 50% thickness reduction). Starting with a rectangular piece (similar to 0.4 mm thick) cut from the as-grown alloy, after the first thermo-mechanical treatment, the specimen exhibits over a wide temperature T interval a peak effect not far from the DC irreversibility line. With a supplemental thermo-mechanical treatment, the peak effect disappears and is substituted by a second magnetization peak ( where the characteristic fields are significantly lower) induced by pinning enhancement. The second magnetization peak was clearly seen at high temperatures only, due to the occurrence of thermo-magnetic instabilities in the low-T domain. In both cases, analysis of magnetic relaxation evidences a crossover towards plastic vortex creep accompanying the maximum in the effective critical current density. These results suggest a common nature of the observed effects, related to the disordering of the vortex system induced by pinning.

Thin films of Bi2Sr2CaCu2O8 (Bi-2212) with the non-c-axis (117) orientation were grown by MOCVD on (110) LaAlO3 single crystal substrate. XRD theta - 2 theta scans show that films contain also (119) and (011) Bi-2212 impurity grains. We propose and report characterization of the non-c-axis films by XRD phi-psi scans. By this approach, the assumed theoretical film-substrate relationship of the (117) Bi-2212 grains is demonstrated experimentally. The result also confirms twinning in the span rooflike (117) Bi-2212 grains. The impurity (119) and (011) Bi-2212 grains are also rooflike and in-plane aligned according to film-substrate relation and AFM images so that the film can be considered in-plane epitaxial.

This article reports the synthesis and characterization of several types of organic-inorganic nanocomposites based on epoxy resin/monoglycidylether-terminated poly(dimethylsiloxane) reinforced with 2, 5, or 10 wt% polyhedral oligomeric silsesquioxanes (POSS) bearing one glycidyl (1GE-POSS) or eight glycidyl(8GE-POSS) groups. The morphological features of the studied samples were established through atomic force microscopy, contact angle measurements, X-ray photoelectron spectroscopy, and scanning electron microscopy/energy-dispersive X-ray spectroscopy, and it was demonstrated that 8GE-POSS is well dispersed within the polymer matrix, while 1GE-POSS exhibits a high tendency to form aggregates. Differential scanning calorimetry (DSC) and Fourier transform infrared resonance (FTIR) measurements are used to follow the curing behavior and to study the polymerization kinetics of epoxy groups. As evidenced by DSC and FTIR results, the inclusion of 8GE-POSS within the polymer matrix leads to a lower epoxy polymerization rate of the resulted nanocomposites than those reinforced with 1GE-POSS. The dynamic mechanical analysis results revealed that the thermomechanical properties are gradually improved with increasing of 8GE-POSS content due to the higher cross-linking density.

High density monolithic boron carbide specimens with grain size of 3-5 mu m were consolidated by spark plasma sintering using identical heating conditions and Ar or N-2 atmospheres. The effect of impurities from two different raw powders on the flexural strength was revealed. The increase in flexural strength was observed up to 1600 degrees C. Specimens consolidated in nitrogen had a higher strength than that consolidated in argon. Samples had the room temperature strength ranging from 350 to 550 MPa. The high temperature strength of our samples exceeding 400 MPa is higher than that previously reported for polycrystalline monolithic B4C. The supporting cracking/strengthening mechanism was discussed and proposed. (C) 2016 The Ceramic Society of Japan. All rights reserved.

Thermal behavior of repa-germanium (C6H10Ge2O7, Ge-132) during heating in air or in argon is investigated using DSC-TGA, XRD, SEM,TEM, and FT-IR measurements. Nine domains of thermal transformations were identified from room temperature to 1200 degrees C, in air or argon. The first reversible transformation is below 220 degrees C and it was assigned to an isomerization process, based on DSC, XRD and IR measurements. The next five transformation domains (220-910 degrees C) are decompositions accompanied by weight loss. The main product of thermal decomposition is Ge. The next transformation domain (910-970 degrees C) corresponds to melting of Ge, both in argon and air. In the air, this step is followed by oxidation of Ge (970-1100 degrees C) and, finally, by melting of GeO2. Amorphous phases formed between 220 and 720 degrees C. Observed processes are discussed based on crystal chemistry and bonds dynamics considerations. (C) 2016 Elsevier B.V. All rights reserved.

Graphene nanopowder (G) with average thickness particle size of about 6-8 nm was added to MgB2 commercial powder. Starting composition was (MgB2)((1-x))(G)(x),x = 0.0125, 0.025, 0.05. Processing was performed by Spark Plasma Sintering (SPS) technique. All added samples have high density (above 95%). The critical temperature (T-c) and the lattice parameter a (c-axis lattice parameter is constant) show a small variation suggesting that carbon substitution for boron is low. TEM observations show the presence of un-reacted graphene plates supporting the T-c and structural results. It also indicates that G-addition does not modify the MgB2 microstructure. Despite this, there is an optimum doped sample (MgB2)(0.9875)(G)(0.0125) for which the critical current density at temperatures below 25 K is slightly higher at high magnetic fields than for the pristine sample. The addition of G is found as one of the least effective C-source additions enhancing J(c). We discuss results as being strongly related to variation of the residual stress. (C) 2016 Elsevier Ltd. All rights reserved.

Dense bulk samples, with relative density of 88-99%, of MgB2 added with Ge2C6H10O7 were obtained by ex situ Spark Plasma Sintering. The critical current density of the added samples is improved at high magnetic fields when compared to a pristine reference sample. The optimum composition was found for MgB2(Ge2C6H10O7)(0.0014), where J(c)(20 K) = 10(2) A/cm(2) is obtained at 5.8 T, versus 3.9 T for the reference sample. This sample has also the highest product J(c0) center dot H-irr among the added samples, and values are similar to those for the pristine MgB2 sample. There is no significant Ge substitution in the crystal lattice of MgB2, while C substitutes for B. Pinningmechanism shifts from point to grain boundary type with increasing of addition amount. The pinning shift tendency is higher at lower temperatures (5 K).

A finite element simulation of the mechanical static features for a modified short hip endoprosthesis was performed. The corkscrew-like femoral stem was modified introducing more turns of the thread. By such an approach it is expected that for some cases the mechanical fixation of the prosthesis to the bone will be improved or the use of the cement for bonding is not necessary. Our scenario was estimated for titanium and stainless steel, and both materials show good safety factors. Mechanical stress is expected to be distributed more uniform in the bone for the new design with more turns of thread.

Ex-situ spark plasma sintering (SPS) was used to obtain dense MgB2-based tapes in a Fe sheath with the starting composition (MgB2)(0.975) + (SiC)(0.025) + Te-0.01. Prior to the SPS procedure of tape formation, the samples were submitted to a series of cold working processes typical for the powder-in-tube technique. The tapes were compared with optimal doped bulk samples (having the same starting composition) and a pristine MgB2 tape. The morphology of the composite samples, the phase structure of both the core and the inner face of the metallic sheath shows the formation of a plethora of traces as a result of interaction between MgB2, additives, and the Fe sheath. Important critical parameters, like critical current density and the irreversibility field, show that there is a field and temperature range where the SiC and Te-added tapes display better critical parameters comparative to either pristine MgB2 tapes in the Fe sheath or SiC and Te doped MgB2 bulk samples.

Dense (95-98.6%) bulk boron carbide prepared by Spark Plasma Sintering (SPS) in Ar or N-2 atmospheres were subject to three-point flexural tests at room and at 1600 degrees C. Eight different consolidation conditions were used via SPS of commercially available B4C powder. Resulting specimens had similar grain size not exceeding 4 mu m and room-temperature bending strength (sigma(25) (degrees C)) of 300-600 MPa, suggesting that difference in sigma(25) (degrees C) m is due to development of secondary phases in monolithic boron carbide ceramics during SPS processing. To explain such difference the composition of boron carbide and secondary phases observed by XRD and Raman spectroscopy. The variation in intensity of the Raman peak at 490 cm(-1) of boron carbide suggests modification of the boron carbide composition and a higher intensity correlates with a higher room temperature bending strength (sigma(25) (degrees C)) and Vickers hardness (HV). Secondary phases can modify the level of mechanical characteristics within some general trends that are not dependent on additives (with some exceptions) or technologies. Namely, HV increases, sigma(25) (degrees C) decreases, and the ratio sigma(1600 degrees C)/sigma(25 degrees C) (sigma(1600 degrees C) - bending strength at 1600 degrees C) is lower when fracture toughness (K-IC) is higher. The ratio sigma(1600 degrees C)/sigma(25 degrees C) shows two regions of low and high K-IC delimited by K-IC=4.1 MPa m(0.5): in the low K-IC region, boron carbide specimens are produced in nitrogen. (c) 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

High density bulks (97%-99%) of MgB2 were prepared by spark plasma sintering (SPS) in nitrogen (N-2) atmosphere for different heating rates (10, 20 and 100 degrees C min(-1)) and compared with reference samples processed in vacuum and Ar. N-2 reacts with MgB2 and forms MgB9N along the MgB2 grain boundaries. The high-field critical current density is enhanced for the sample processed in N-2 with a heating rate of 100 degrees C min(-1). At 2-35 K, this sample shows the strongest contribution of the grain boundary pinning (GBP). All samples are in the point pinning (PP) limit and by increasing temperature the GBP contribution decreases.

High density (above 92%) superconducting bulks of MgB2 co-added with cubic BN (c-BN) and fullerenes (C-60) were obtained by the ex-situ spark plasma sintering (SPS). Compositions were (MgB2)((1-x))(C)(x)(c-BN)(0.01), x = 0.0125, 0.025, 0.05, 0.075. The co-added sample (MgB2)(0.975)(C)(0.025)(c-BN)(0.01) shows a marginally higher critical current density J(c) at intermediate magnetic fields and below 15 K than for optimum samples added with c-BN or C-60. For this sample, pinning is in the point pinning limit and the delta T-c mechanism is dominant. At high magnetic fields co-added samples are inferior to samples added with one additive, but are superior to pristine sample. Co-addition of c-BN and C-60 is not effective for vortex pinning when compared with individual addition. The result is discussed based on phase formation aspects, microstructural details and residual strain. It was found that in the presence of C-60, c-BN consumption with formation of MgNB9 is intensified with implications on different elements that influence pinning. (C) 2015 Elsevier B.V. All rights reserved.

The aim of this research is to prepare amorphous thin films of undoped gallium sulphide and doped with rare-earth sulphides, of rare-earth sulphides and to investigate their physical properties. We have prepared thin amorphous films of Ga2S3, EuS, Er2S3, Gd2S3, and Ga2S3 doped with rare-earth sulphides (Ga2S3:EuS, Ga2S3:Er2S3, Ga2S3:Gd2S3) by Pulsed laser Deposition (PLD). The corresponding targets for preparation of amorphous thin films were obtained by Spark Plasma Sintering (SPS) from commercially available powders of binary sulphides. The structural results for the undoped and doped Ga2S3 thin films indicate a packing of disordered layers similar to that of amorphous As2S3. Femtosecond laser irradiation of the Ga2S3 thin films shows a photoexpansion effect at low laser power (85-100 mW) and an ablation effect at higher laser power (above 105 mW). The threshold between low power and high power pulses is situated at higher value for Ga2S3 (100 mW) in comparison with the case of As2S3 thin films (20 mW). (C) 2014 Elsevier B.V. All rights reserved.

Powder mixtures of MgB2 and B4C with composition ((MgB2) + (B4C) x, x = 0.005, 0.01, 0.03) were consolidated by Spark Plasma Sintering at 1150 degrees C for 3 min. The average particle size of B4C raw powder was relatively high of 4 mm. Despite this, it is shown that processing processes are fast and, as in the case of the in-situ routes, for our ex-situ method carbon substitutes for the boron in the crystal lattice of MgB2. Specifics of microstructure are discussed based on electron microscopy observations. Carbon substitution and microstructure contribute to enhancement of the critical current density J(c) at high magnetic fields and of the irreversibility field H-irr. Samples are shown to be in the point pinning limit with some tendency toward the grain boundary pinning depending on B4C doping amount and temperature. An optimum composition is found for x = 0.01: for this sample, at 20 K, a J(c) of 100 A/cm(2) is obtained at 5.35 T. This value is higher than for the pristine MgB2 sample and for an optimum ex-situ nano-SiC-doped sample obtained for the same SPS processing conditions. (C) 2015 Elsevier B.V. All rights reserved.

Dense MgB2 samples with La2O3 addition were obtained by spark plasma sintering. We used two different La2O3 raw powders showing different particle sizes and shapes. The as-obtained composite samples have significant differences in microstructure and Vickers hardness. A deposited phosphate layer was obtained by immersing the samples in PBS, and drying. Formation of phosphate needles, gathered in bouquets, show a possible bioactive behavior of MgB2.

Superconducting bulks of MgB2 were obtained by the Spark Plasma Sintering (SPS) technique. Different heating rates of 20, 100, 235, 355, and 475 degrees C/min were used. Samples have high density, above 95%. The onset critical temperature T-c, is about 38.8 K. There is an optimum heating rate of similar to 100 degrees C/min to maximize the critical current density J(c0), the irreversibility field H-irr, the product (J(c0) x mu H-0(irr)), and to partially avoid formation of undesirable flux jumps at low temperatures. Significant microstructure differences were revealed for samples processed with low and high heating rates in respect to grain boundaries. (C) 2015 Elsevier B.V. All rights reserved.

The purpose of the present study is to develop novel nanocomposites based on diglycidylether of bisphenol A (DGEBA) combined with diglycidylether-terminated polydimethylsiloxane (DG-PDMS), reinforced with 10 wt.% (mono-/octa) epoxy POSS nanocages (MEP or OEP-POSS). DG-PDMS and POSS compounds were covalently incorporated into DGEBA resin via copolymerization of epoxy groups. The effect of both DG-PDMS and POSS nanoparticles on the curing reaction, glass transition temperature (T-g), thermal stability, hardness and morphology of DGEBA/DG-PDMS +/- POSS nanocomposites were studied by DSC, FTIR, DMA, TGA, SEM/EDX, AFM and contact angle measurements. SEM/EDX and AFM results prove that OEP-POSS is well dispersed within DGEBA/DG-PDMS polymer matrix, while MEP-POSS forms large POSS aggregates. The thermo-mechanical properties of POSS based nanocomposites are also in good correlation with morphology features. MEP-POSS based nanocomposite with heterogeneous dispersion of FOSS aggregates exhibits lower T-g value and thermal stability in comparison with OEP-POSS nanocomposite which exhibits a nanoscale dispersion of the PUSS cages. The obtained T-g of OEP-POSS based nanocomposite increases with 31 degrees C in comparison with the unreinforced matrix. Moreover, this nanocomposite shows the highest storage modulus (E') and hardness. (C) 2015 Elsevier Ltd. All rights reserved.

The Mossbauer spectra of a FeSe0.3Te0.7 single crystal grown by the Bridgman method were analysed across the superconducting transition by considering the interplay between the structure and electron configuration of the transition metal. The magnetically determined superconducting critical temperature is T-C similar to 14 K. The Fe-57 Mossbauer spectra collected in the temperature range from 5 to 200K mainly have an asymmetric doublet pattern, which was conveniently fitted by the full Hamiltonian method. No effective magnetic moment ascribed to the superconducting phase was observed down to 5K. The unusual behaviour observed below similar to 17K for the chemical isomer shift and quadrupole splitting may be associated with an electron reconfiguration process intimately related to an unusual lattice distortion accompanying the superconducting transition. The decreasing trend of the total absorption spectral area and second-order Doppler shift during cooling the sample below the critical temperature, point to enhanced phonon activation in the superconducting state.

Both Spark Plasma Sintering (SPS) and conventional sintering were applied to obtain bulks of ledeburitic highly alloyed steels for tools fabrication. Powder mixtures of the component elements, of com-pounds or of powders obtained through ball milling of the chips resulting from the processing of parts from steels of interest were used. When compared with traditional technologies (casting and plastic deformation), SPS and the use of milled chips resulted in the formation of microstructures with a high degree of distribution homogeneity and dimensional uniformity of the carbides. As is well known, the improvement of these param-eters leads to the maximization of the functional properties of tools.

Spark plasma sintering (SPS) was applied for fabrication of dense (relative density > 97 %) bulk MgB2 samples added with Ge. Mixtures of MgB2 and Ge powders with starting compositions (MgB2) Ge (x) , x=0.005, 0.01, and 0.03 were used. Added samples show enhancement of the critical current density at high magnetic fields when compared to a pristine reference sample. The optimum composition is for x=0.005 and for this sample J (c)(20 K) =10(2)A/cm (2) is obtained at 5 T, while for the reference sample is obtained at 3.9 T. Ge does not substitute in the crystal lattice of MgB2 and T (c,onset) or T (c,midpoint) from magnetization measurements scatter within 0.15 or 0.3 K, respectively.

Commercial wires of MgB2 with different architectures and two different heat treatments were characterized with respect to their superconducting properties (T-c, J(c), H-irr, pinning force, macro flux jumps behaviour) through magnetic measurements and were visualized by 3D x-ray micro-tomography (XRT). For a particular architecture, heat treatment conditions of 625 degrees C/3 hrs or 700 degrees C/30 min produced relatively small differences, whereas the architecture of the wires showed a strong influence on superconducting characteristics. XRT checks the integrity of the wires easily detecting in a non-invasive way 3D macro defects and shows their hidden extended shape. XRT also allows a comparative geometry analysis between similar elements (e.g. filaments or filaments-matrix interfaces) from a particular wire or from wires with different architectures. Namely, XRT shows that the geometrical perfection (defined as the degree of departure of the geometry from the designed one) of the inner MgB2 filaments from the wires with 18 elements was lower than for the outermost ones from the same wires and was also lower than for the filaments from the wires with 7 elements. It is proposed that these results of geometrical perfection correlate with better overall superconducting quality of the wires with 7 filaments (except for the stronger presence of macro flux jumps in the wires with 7 filaments).

Bulk ceramics of Ga2S3 and rare-earth sulfides (EuS, Gd2S3, Er2S3) as well as combinations thereof have been prepared by spark plasma sintering (SPS). The disk-shaped ceramics were used as targets for pulsed laser deposition (PLD) experiments to obtain amorphous thin films. The properties of these new bulks and amorphous thin films have been investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX), optical transmission spectroscopy, and atomic force microscopy (AFM). In order to test the photoexpansion effect in Gd2S3 and the possibility to create planar arrays of microlenses, the film was irradiated with femtosecond laser pulses at different powers. For low laser power pulses (up to 100mW power per pulse) a photoexpansion effect was observed, which leads to formation of hillocks with a height of 40-50 nm. EuS doped Gd2S3 thin film shows luminescence properties, which recommend them for optoelectronic applications.

Lamellar crystal objects such as straight, curved or kinked whiskers, bows and objects with missing stripes were grown in a static air atmosphere from melt-quenched substrates with starting composition Bi1.5Sr1Ca1Co0.6Oy. The average EDS composition of the objects is Bi2Sr0.75Ca1.8Co1.94Oy and the crystal structure is of the phase usually denoted in the literature as Bi-2(Sr,Ca)(2)Co2Oy (BiCO222). Objects of other phases were not found. Curvature is in the (ab)-plane. By scanning tunneling spectroscopy (STS) a semiconducting energy gap was determined at 2.41 eV.

Dense samples (relative density > 93%) of bulk MgB2 with GeO2 additions were obtained by Spark Plasma Sintering. The critical current density J(c) of the added samples is improved at high magnetic fields when compared to the pristine sample. The optimum composition is for MgB2(GeO2)(0.005). For this sample, a J(c)(20 K) = 10(2) A/cm(2) is obtained at 5.1 T versus 3.9 T for the pristine sample. Ge substitution in the crystal lattice of MgB2 can be considered negligible, and T-c,T-onset and T-c,T-midpoint from magnetization measurements scatter within 0.2 and 0.6 K, respectively. TEM investigations show some specific details at nano scale: the tendency to form secondary phases (25-100 nm) with sphere-like or irregular shapes is observed and discussed. Samples are composites and the residual strain of MgB2 is constant for pristine and GeO2-added samples. Therefore, pinning enhancement leading to improvement of Jc for the GeO2 added samples is purely a 'microstructure' effect due to the presence of secondary phases. The point pinning is determined to be the predominant mechanism. Addition of a higher amount of GeO2 is shifting the pinning mechanism toward a grain boundary pinning. (C) 2015 Elsevier Masson SAS. All rights reserved.

Thin films of Bi2Sr2CuO6 (Bi-2201) with (001) or (115) orientation were grown on SrTiO3 substrates. These films are expected to be useful as component films of heterostructures and devices (e.g. as insulators). We used two chemical routes, namely spin coating followed by thermal annealing and MOCVD. For both routes we demonstrated growth of c-axis and non-c axis thin films depending on the selected orientation of the SrTiO3 substrate. To our knowledge, films of (115) Bi2201 obtained by spin coating or MOCVD are reported for the first time.

Superconducting bulk discs, S, of 20 mm in diameter and 3.5 or 3.3 mm thickness of MgB2 (pristine or added with cubic BN, respectively) with density above 97% were prepared by Spark Plasma Sintering. Discs were combined in a pair-type sandwich-like arrangement with a permanent NdFeB axially magnetised magnet, PM (similar to 0.5 T). Measurement of the trapped field, B-tr, with temperature, time, and the reduction rate of the applied magnetic field was performed using a Hall sensor positioned at the centre between the superconductor and the permanent magnet. It is shown that the permanent magnet with certain polarity favors higher trapped field of the superconductor owing to suppression of flux jumps specific for high density MgB2 samples. The B-tr of the PM-S pair was 2.45 T (20 K) and 3.3 T (12 K). (C) 2014 Elsevier B.V. All rights reserved.

Boron carbide ceramic was prepared by reactive Spark Plasma Sintering under N-2-atmosphere and for different heating times and maximum pressure regimes. Split-Hopkinson Pressure Bar (SHPB), indentation, XRD and microscopy measurements were performed for samples characterization. It is shown that SHPB toughness control depending on SPS regime is possible and the main reason is introduction of nitrogen into B4C ceramic. Complex relationships between processing conditions, sintering mechanism, material's specifics, static and dynamic mechanical properties are discussed. Improvement of dynamic toughness is through mechanisms resembling those working for static load conditions such as cracks deflection and pull out, but there are also significant differences. (c) 2013 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

High density (above 93%) superconducting bulks of MgB2 with addition of hexagonal BN (h-BN) and cubic BN (c-BN) with compositions ((MgB2) + (BN)(x), x = 0.01, 0.03, 0.05) were obtained by ex situ spark plasma sintering. All the investigated samples have the critical temperature T-c = 38.8 K. The variation of the critical current density J(c) with the external magnetic field H for h-BN added sample is almost overlapping the J(c)(H) dependence for the pristine MgB2 sample. On the other hand, J(c) for the samples added with c-BN is larger at high magnetic fields, while the decrease of J(c) at low H is very small. At T = 20 K, a J(c) of 10(2) A cm(-2) is determined for the sample with x(c-BN) = 0.005 at H = 58 kOe, and for the sample with x(c-BN) = 0.01 at 54 kOe. Magnetic relaxation measurements indicate a significant flux pinning enhancement in MgB2 samples added with c-BN. It is proposed that the disorder at the interface caused by the convenient lattice matching relationship between the lateral plane of the MgB2 crystal prism and the face of the c-BN crystal cube is responsible for the observed vortex pinning increase.

Sintered bulks require new approaches for the control and improvement of their functional characteristics. Nanostructuring, synergy effects at interfaces in a composite, and technology specific features are essential in this regard. In this work, for a better understanding of challenges, complex relationships between materials and technology and different practical concepts such as "transferability", "composite within a composite", and "multilevel design", and "multifunctionality", a comparative analysis is proposed for very different nano structured materials such as La0.9Sr0.1Ga0.8Mg0.2O3-x x solid electrolyte, hard B4C-based materials, and doped MgB2 superconductors. Samples were obtained by reactive spark plasma sintering (SPS). SPS is reconfirmed as a powerful processing technique that generates high-density unique bulk materials impossible to fabricate by other methods. However, it is shown that SPS is not universal and its suitability should be carefully considered depending on materials and targeted applications. (C) 2014 The Japan Society of Applied Physics

Two different types of Ho2O3 powders (showing a much different morphology) were added to MgB2 in the ex-situ Spark Plasma Sintering (SPS). In the 5-25 K range, the first Ho2O3 powder type does not significantly suppress the critical current density J(c) at low magnetic fields and the second one enhances it at high fields, while their mixture simultaneously controls J(c) at both small and high magnetic fields so that the decrease is small at low fields and there is a notable enhancement at high fields when compared to pristine sample. The control of J(c)(H) is discussed versus specific characteristics of the raw powders, the resulting microstructure of the added SPS-ed samples and pinning details from magnetic relaxation measurements. (C) 2014 Elsevier B.V. All rights reserved.

A mixture of B2O3 and amorphous B with the mole ratio of 1:14 is shown to react and form B6O ceramic under in-situ spark plasma sintering (SPS) conditions. The optimum SPS temperature and time to obtain phase B6O are 1250 C and 30 min, respectively, and Rietveld refinement of the XRD patterns indicates that the oxygen occupancy of B6Ox is reasonably high at x = 0.89(99). However, to reach high density above 98%, SPS temperatures of 1700-1800 degrees C are necessary and a one-step twotemperature in-situ reactive SPS was designed and applied. As-prepared B6O dense ceramic has Vickers hardness (36.7 +/- 1.2 GPa) and fracture toughness (K-1c = 4.2 +/- 0.15 MPa. m(1/2)) comparable with the highest values reported in literature for the bulks obtained by processing routes of already reacted B6O powders (ex-situ routes).

Vortex pinning on natural and artificial defects is essential for large scale applications of superconducting materials. One of the most promising solutions for the creation of efficient pinning structures is to combine the strong pinning supplied by columnar defects (with the radius of the order of the superconducting coherence length) and the presence of random quenched disorder, which inhibits the detrimental vortex kink formation. A strong pinning is revealed by high values of the vortex activation energy in the magnetic relaxation process. We present a critical analysis of the interpretation of the relaxation data at long- and short time scales, by extracting the so called normalized vortex-creep activation energy. This allowed us to find the actual temperature interval for the characteristic vortex excitations in YBa2Cu3O7 films with embedded BaZrO3 nanorods 9preferentially oriented along the c axis), and to unambiguously determine the characteristic vortex pinning energy. The observed drastic change of magnetic relaxation at short time scales (attained in standard AC measurements) is attributed to a large contribution of the pinning enhanced viscosity to the vortex hopping activation energy.

We present the effect of single molecular magnet ([Fe(bpca) Dy-2(NO (3))(4)] a <...H (2) Oa <...4.5 CH (3) NO (2) and [Mn (2)(naften) (2)(CH 3COO)(CH 3OH)] a <...BPh (4)) thermolysis on the superconducting properties of polycrystalline MgB (2) samples when inserted and sintered by spark plasma sintering technique. As a result of pyrolysis, Fe- and Dy-magnetic compounds grow within the MgB (2) matrix and give a paramagnetic behavior in normal state, whereas the Mn-based compounds display negligible magnetic properties. We find that the magnetic critical current density of the as-obtained superconducting composites, as well as the pinning mechanism, is dependent on the magnetic background, with a noticeable advantage for the sample with magnetic compounds.

We report on the changes on the microstructural, hardness, and corrosion properties induced by carbo-chromization of 316L stainless steel prepared by Spark Plasma Sintering technique. The thermo-chemical treatments have been performed using pack cementation. The carburizing and chromization were carried out between 1153 K (880 A degrees C)/4 h to 1253 K (980 A degrees C)/12 h and 1223 K (950 A degrees C)/6 h to 1273 K (1000 A degrees C)/12 h in a solid powder mixture of charcoal/BaCO3 and ferrochromium/alumina/NH4Cl, respectively. The obtained layers were investigated using X-ray and electron diffraction, optical and scanning electron microscopies, Vickers micro-hardness, and potentiodynamic measurements. The thickness of the carbo-chromized layer ranges between 300 and 500 mu m. Besides the host gamma-phase, the layers are mainly constituted of carbides (Fe7C3, Cr23C6, Cr7C3, and Fe3C) and traces of alpha'-martensite. The average hardness values decrease smoothly from 650 HV at the sample surface down to 200 HV at the center of the sample. The potentiodynamic tests revealed that the carbo-chromized samples have smaller corrosion resistance with respect to the untreated material. For strong chromization regimes, the corrosion rate is increased by a factor of four with respect to that of the untreated material, while the micro-hardness of the layer is three times larger. Such materials are suited to be used in environments where good corrosion resistance and wear properties are required.

Dense boron carbide (above 95%) was achieved through high pressure (300 MPa) and low temperature (1600 degrees C) Spark Plasma Sintering (SPS). This approach resulted in improvement of fracture toughness and of dynamic toughness when compared to corresponding toughness values of the sample sintered by conventional SPS (2100 degrees C, 50 MPa). Dynamic toughness was extracted from Split Hopkinson Pressure Bar measurements. Results are understood based on microstructure and on very different behaviour of the samples in respect to residual B2O3 and carbon available in the raw B4C powder. (C) 2014 The Ceramic Society of Japan. All rights reserved.

Ge, GeO2 and Ge2C6H10O7 additions to MgB2 obtained by ex situ spark plasma sintering significantly enhance the critical current density J(c) in high magnetic fields. A J(c)(T = 20 K) of 102 A cm(-2) is obtained at 3.9 T in the pristine sample and at 5.8 T in the MgB2(Ge2C6H10O7)(0.0014) sample. The decrease in the critical temperature for added samples is less than 1 K and T-c(20 K, H = 0) shows a small decrease from 5.5 x 10(5) A cm(-2) in the pristine sample to 3.9 x 10(5) A cm(-2) in MgB2(Ge2C6H10O7)(0.0014) sample. Ge does not substitute into the MgB2 lattice. (C) 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Nano- or micropowders of Eu2O3 were added to MgB2, resulting in a composition of (MgB2)(0.975)(EuO1.5)(0.025). Pristine and doped samples were prepared using spark plasma sintering and tested for (i) Vickers hardness, (ii) pH evolution in phosphate-buffered saline solution, (iii) corrosion resistance (Tafel polarization curves), (iv) cytotoxicity (in vitro tests), and (v) antibacterial activity. Eu2O3 addition influenced the investigated properties. Solutions of MgB2-based samples show a relatively high saturation pH of 8.5. This value is lower than that of solutions incubated with Mg or other Mg-based biodegradable alloys reported in the literature. MgB2-based samples have lower electro-corrosion rates than Mg. Their Vickers hardness is 6.8-10.2 GPa, and these values are higher than those of biodegradable Mg-based alloys. MgB2 has low in vitro biocompatibility, good antibacterial activity against Escherichia coli, and mild activity against Staphylococcus aureus. Our results suggest that MgB2-based materials deserve attention in biomedical applications, such as implants or sterile medical instruments. (C) 2014 Elsevier B.V. All rights reserved.

Ex situ spark plasma sintering was used to obtain dense MgB2 co-doped with SiC and Te. The composition (MgB2) + (SiC)(0.025) + Te-0.01 shows critical current densities J(c)(20 K, 5 T) of 3.5 x 10(2) A cm(-2) and J(c)(5 K, 9 T) of 2 x 10(3) A cm(-2). These values are higher than for pristine samples or those separately doped with Te or SiC. They are also comparable at high fields and temperatures with the best reported values for the co-doped MgB2 bulks produced by conventional in situ methods. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Tetragonal alpha-FeSe flakes were fabricated by a simple method. Enhancement of superconductivity was observed in the quenched samples. The properties were characterized by X-ray diffraction, a superconductivity quantum interference device, and physical property measurement system. It is interesting that the superconducting transition temperature of the quenched samples is about 2 K higher than that of unquenched samples, but after reannealed, the enhancement of superconductivity disappeared. The reduction of the c/a ratio might be responsible for the enhancement of superconductivity in the quenched FeSe flakes.

Bi2O3 and Bi-metal powders were mixed with MgB2 powder. Starting compositions were (MgB2)(Bi2O3) x, x = 0.0025, 0.005, 0.015, and (MgB2)(Bi)(y), y = 0.01. Mixtures were processed by Spark Plasma Sintering (SPS) technique. As obtained composite samples show high density, above 94 % of the theoretical density. Samples with Bi2O3 for x = 0.0025 and 0.005 show higher critical current densities, J(c), at high fields and at 20 K than for the pristine sample. Their irreversibility field, H-irr, is also higher. On the other hand, sample added with Bi-metal has lower J(c) and H-irr at any temperature than for the pristine sample.

In the last years oxide materials for electronics show significant progress. However, many details regarding technology control of the properties have to be solved. For electronics, thin films and heterestructures are important taking advantage of integration and synergetic concepts leading to new types of devices and functionalities. It is notable that, while fabrication of new devices and materials showing new phenomena are booming, the growth principles and concepts are somehow developing slowly within this general trend. This is because in many cases, growth of materials is very personalized. Understanding of the bi-directional relationship between the general and particular principles deserves attention. The immediate benefit is that knowledge on growth for one material can be transferred to another one. In our work we have analyzed such relationships for some oxide multicomponent perovskites. Materials used in our examples are Bi-Sr-Ca-Cu-O and YBa2Cu3O7, (Ca, Sr)CuO2, (Ca, Ba)CuO2 and Bi4Ti3O12. Presented thin films or heterostructures are with c-axis and non-c-axis orientations and based on these examples we discuss some of the growth principles.

Directionally solidified B4C-TiB2 eutectics doped with different Si contents were prepared by floating zone method. Silicon doping (up to 3 vol.%) promotes a more coherent interface between B4C matrix and TiB2 inclusions, a decrease of the spacing between TiB2 (when solidification rate is constant), and formation of a more uniform morphology with thinner inclusions. These features lead to simultaneous enhancement of Vickers hardness (HV), fracture toughness (K-1c) and bending strength (sigma) when compared with Si-free B4C-TiB2 eutectics. For our materials, the average HV, K-1c and sigma were 45.2 GPa, 7.04 MPa m(1/2), and 460 MPa at room temperature or 487 MPa at 1600 degrees C, respectively. The values of sigma at indicated temperatures are approximately twice higher than for the Si-free B4C-TiB2 eutectic composites. (C) 2013 Elsevier B.V. All rights reserved.

We review, based on our results, the problems and solutions for the growth of thin films and composite heterostructures emphasizing the general growth aspects and principles vs specifics for each material or heterostructure. The materials used in our examples are Bi2Sr2Ca2Cu3O10, Bi2Sr2CaCu2O8, YBa2Cu3O7, (Sr, Ca)CuO2, (Ba, Ca) CuO2, and Bi4Ti3O12. The growth method was metal organic chemical vapor deposition (MOCVD). The presented thin films or heterostructures have c- and non-c-axis orientations. We discuss the implications of the film-substrate lattice relationships, paying attention to film-substrate lattice mismatch anisotropy and to film-film lattice mismatch, which has a significant influence on the quality of the non-c-axis heterostructures. We also present growth control through the use of vicinal substrates and two-temperature (template) and interrupted growth routes allowing significant quality improvements or optimization. Other key aspects of the growth mechanism, that is, roughness, morphology, and interdiffusion, are addressed. It is concluded that the requirements for the growth of non-c-axis heterostructures are more severe than those for the c-axis ones. (C) 2012 The Japan Society of Applied Physics

We were successful in synthesizing non-linear YBa(2)Cu(3)Ox whiskers, i.e. half loops or kinked shapes, which are promising candidates for solid-state devices based on the intrinsic Josephson effect and with improved electrical connections. We report on a complete characterization of their structural properties via a synchrotron nanoprobe as well as laboratory single-crystal diffraction techniques. This investigation allowed us to fully disclose the growth mechanism, which leads to the formation of curved whiskers. The superconducting properties are evaluated in comparison with their straight counterpart, revealing a strong functional analogy and confirming their potential applicability in superconducting electronic devices.

We have obtained by Spark Plasma Sintering (SPS), dense samples of MgB2 added with Ho2O3. Starting composition was (MgB2)(0.975)(HoO1.5)(0.025) and we used addition powders with an average particle size below and above 100 nm. For Mg, pristine and added MgB2 samples we measured potentiodynamic polarization curves in Phosphate Buffered Saline (PBS) solution media at room temperature. MgB2 based composites show corrosion/degradation effects. This behavior is in principle similar to Mg based alloys in the same media. Our work suggests that the different morphologies and phase compositions of the SPS-ed samples influence the interaction with corrosion medium; hence additions can play an important role in controlling the corrosion rate. Pristine MgB2 show a significant improvement of the corrosion resistance, if compared with Mg. The best corrosion resistance is obtained for pristine MgB2, followed by MgB2 with nano-Ho2O3 and mu-Ho2O3 additions.

Boron carbide B4C powders were subject to reactive spark plasma sintering (also known as field assisted sintering, pulsed current sintering or plasma assisted sintering) under nitrogen atmosphere. For an optimum hexagonal BN (h-BN) content estimated from X-ray diffraction measurements at similar to 0.4 wt%, the as-prepared BaCb-(BxOy/BN) ceramic shows values of Berkovich and Vickers hardness of 56.7 +/- 3.1 GPa and 39.3 +/- 7.6 GPa, respectively. These values are higher than for the vacuum SPS processed B4C pristine sample and the h-BN -mechanically-added samples. XRD and electronic microscopy data suggest that in the samples produced by reactive SPS in N-2 atmosphere, and containing an estimated amount of 0.3-1.5% h-BN, the crystallite size of the boron carbide grains is decreasing with the increasing amount of N-2, while for the newly formed lamellar h-BN the crystallite size is almost constant (similar to 30-50 nm). BN is located at the grain boundaries between the boron carbide grains and it is wrapped and intercalated by a thin layer of boron oxide. BxOy/BN forms a fine and continuous 3D mesh-like structure that is a possible reason for good mechanical properties.

A methodology is proposed to investigate in detail shrinkage kinetics under isothermal spark plasma sintering (SPS) conditions applied to ceramic nano powders such as Y2O3 stabilized ZrO2. To do so, mild SPS conditions were used (low temperatures and pressure, long dwell times). The extracted experimental activation energy has the value of 246 +/- 37 kJ mol(-1) and the slope of the curves on the intense densification stage is around 0.33. Results are in agreement with densification by a grain-boundary diffusion mechanism as for conventional sintering and the contribution from the specific pressure-assisted mechanisms as for hot pressing is insignificant. This result suggests that exploration of mild SPS might prove rewarding in separation and control of the sintering mechanisms leading to production of specific ceramic with new or improved functionality. (C) 2011 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

The tunnel-diode resonator (TDR) technique for accurate measurements of the magnetic penetration depth is used to measure the London and Campbell penetration depths of polycrystalline SiC doped (10wt.%) MgB2. The Campbell length was used to investigate the field and temperature dependence of the critical current density. The as determined critical current density provides values as high as 6x10(6) A/cm(2) at 4.2K, 1T, which is higher than values estimated by Bean method.

Superconducting bulks of MgB2 with addition of Sb2O3 and Sb with different stoichiometric compositions ((MgB2) + (Sb2O3) (x) , x = 0.0025, 0.005, 0.015, and (MgB2) + (Sb)(y), y = 0.01) were obtained by the Spark Plasma Sintering (SPS) technique. All added samples have high density, above 95% and critical temperature, T (c), of 38.1-38.6 K. This result and XRD data suggest that Sb does not enter the lattice of MgB2. Impurity phases are Mg3Sb2, MgO, and MgB4. The optimum addition is Sb2O3 for x = 0.005. This sample shows the critical current density, J (c)(5 K, 0 T) = 4 x 10(5) A/cm(2) and J (c)(5 K, 7 T) = 6 x 10(2) A/cm(2), while the irreversibility field, H (irr) (5 K, 100 A/cm(2)) = 8.23 T. Indicated values of J (c) and H (irr) are higher than for the pristine sample. The mechanism of J (c) and H (irr) increase in the Sb2O3 added samples is complex and composed of opposite effects most probably involving morphology elements, the presence of nano metric MgB4 and the indirect influence of oxygen or oxygen and Sb. Crystallite size of MgB2 is decreasing when Sb-based additions are introduced and the effect is stronger for the Sb-metal addition. The sample with Sb-metal addition does not improve J (c) and H (irr) when compared with pristine sample.

A simple and reproducible fabrication process for the synthesis of FeSe superconductors has been developed. The properties were characterized by X-ray diffraction, scanning electron microscope, superconductivity quantum interference device, and physical property measurement system. It showed a zero resistance superconducting critical temperature of similar to 7.9 K and an onset critical temperature of similar to 13.9 K. The upper critical magnetic field at zero temperature was estimated to be 31 T. The growth mechanism of FeSe flakes was also discussed.

Mixtures of MgB2 and metal or oxide additions with starting compositions of (MgB2)(M2O3)(x), x = 0.0025, 0.005, 0.015, and (MgB2)(M)(y), y = 0.01, M = Bi, Sb, were processed by spark plasma sintering (SPS). As-obtained samples are composites with high density exceeding 94% of the theoretical values. Secondary phases indicate similar reactions for samples with Bi- or Sb-based additions. However, samples show very different superconducting characteristics depending on the addition type and amount. A direct correlation with the melting temperature of the addition could not be revealed, although some aspects will be discussed. From the critical current density (J(c)) and irreversibility field (H-irr) enhancement viewpoints, optimum additions are oxides for x = 0.0025; 0.005. Both oxides improve Jc at high fields, but Sb2O3 is effective up to 10 K, whereas Bi2O3 is effective up to 30 K. Metal additions decrease J(c) and H-irr when compared with a pristine MgB2 sample. (C) 2012 The Japan Society of Applied Physics

High-temperature superconducting objects of Bi2Sr2CaCu2O8 and YBa2Cu3O7 highly curved in the ab-plane, such as curved/ kinked whiskers, bows and ring-like structures, were obtained within a solid-liquid-solid (SLS) grass-like growth mechanism. As-grown objects are crystals with three-dimensional epitaxy similar to conventional single crystals: they can be viewed as crystal parts 'cut' from a conventional rectangular crystal. Between our curved objects and conventional crystals, whiskers or thin films there are some differences in the superconducting properties induced only by the shape factors and no new physics is observed. Some details of the growth mechanism are discussed, emphasizing curved-line formation.

Te metal or TeO2 were added to MgB2 ((MgB2) (A)(x), x = 0.005, 0.01, 0.03, A = addition). The mixtures were processed by spark plasma sintering. The critical current density J(c), of the samples containing the Te/TeO2 additions is enhanced at high fields and at temperatures up to 20K. The curve of J(c)(5 K, H) for the sample with optimum x(Te) = 0.01 shows no accelerated decrease up to 8 T (J(c)(5 K, 8 T) = 1.8 x 10(3) A cm(-2)). The irreversibility field of the samples containing the Te/TeO2 additions is also enhanced. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Unconventional in situ synthesis of MgB2 undoped and doped with fullerene (C-60) was performed by using a single-mode microwave (MW) furnace. Structural properties suggested that C substitutes for B in the crystal lattice of MgB2, while the J(c) showed typical enhancement at high magnetic fields when C chemical doping occurred. This behavior was similar to published results for another field-activated unconventional method of processing, i.e., spark plasma sintering, and it was opposite to the conventional powder-in-tube method for which chemical substitution was not realized when using addition of C-60. Certain morphologically unique features such as the occurrence of needlelike grains were revealed in the MW samples. Our MW samples showed higher relative density (<= 83%) than previously reported data. Magnetic relaxation experiments suggested the presence of microscopic flux jumps in the MW samples, while macroscopic flux jumps were not observed.

Superconducting bulks of MgB2 were obtained by an ex-situ two-temperature route applied to spark plasma sintering (SPS). Processing of samples was performed at lower temperatures than previously reported. Samples produced by the two-temperature route show a higher morphological uniformity, a higher density (above 98%), a higher Vickers hardness, and undesirable stronger microscale flux jumps, as indicated by magnetic relaxation measurements when compared to a sample obtained by the one-temperature route (95.3% relative density). At the same time, all sintered samples show approximately constant crystallite size, critical current density, irreversibility field, critical temperature, weight fraction of impurity phases (MgB4 and MgO), and the amount of carbon accidentally introduced during SPS processing. (C) 2012 Elsevier B.V. All rights reserved.

We present the magnetic and transport properties of superconducting composites fabricated by admixing carbon-encapsulated Fe nanospheres and MgB2 powder. The addition of nanoparticles is expected to enhance the critical current density by carbon-doping the MgB2 matrix and by providing artificial pinning sites. Three samples with estimated amounts of 0.35, 0.6, and 1.0 wt. % metallic Fe were prepared using the spark plasma sintering technique. The average size of these nanoparticles is comparable to the superconducting coherence length of MgB2 at approximately 5 nm. We found that the additions do not significantly alter the critical temperature which is very high, close to that of the pure MgB2 samples. We have also observed improved current densities, as high as 1100 kA/cm(2) for the samples with 0.35 wt. % metallic Fe at 5 K and 1 T. A core-shell model for explaining the transport data is presented. The field and temperature dependence of the reduced pinning force is described in terms of pinning on grain boundaries and/or on point defects. (C) 2011 American Institute of Physics. [doi: 10.1063/1.3672820]

It is proposed a processing route to obtain dense (>= 90%) nanometric La0.9Sr0.1Ga0.8Mg0.2O3-x (LSGM) electrolyte ceramic by reacting under spark-plasma-sintering (SPS) conditions a relatively poor mixture of intermediate powdered La/Sr- and Ga/Mg-based products synthesized separately by precipitation and hydrothermal methods, respectively. Samples with particle size of 9-20, 37-93, and 120-240 nm were measured from the electrical conductivity viewpoint. A fast transport path along grain boundaries was not observed and, a higher nano particle size improves total conductivity in our samples. Results suggest that it is necessary to make a clear distinction between particle size from microscopy observation and crystallite size from structural (e.g. XRD) measurements when looking at the general conductivity - grain size dependence. This dependence is complex and the use of an unconventional, far from equilibrium technique such as SPS might influence it. Currently, a good understanding is missing, but pending on materials, technology specifics and the complex relationship between them, some of the usually promoted ideas from literature such as the necessity of high mixing levels in the precursor powders, of high pressure application during sintering, of low particle size (nano) in the sintered ceramic for a higher conductivity, of high purity phase and so on require careful consideration. (C) 2010 Elsevier B.V. All rights reserved.

Superconducting Y123 thin films with (001), (100/010) and (103/110) orientations were obtained by molecular-organic- source MBE (MOMBE) for optimum growth temperatures of 600, 515 and 600 degrees C, respectively, using a Ba(DPM)(2)(phen)2 source material and ozone atmosphere. Superconductivity was obtained without post processing. According to the literature, use of a Ba(DPM)(2)(phen)(2) precursor was expected to yield a lower optimum growth temperature, but there were no significant differences between the use of this source and a Ba(DPM)(2) precursor. For our c-axis oriented Y123 film, the optimum growth temperature was higher than the reported record-low growth temperature (500 degrees C by MOCVD using Ba(DPM)2(phen)2) but it was lower than the values for other growth techniques. This can have a positive impact on fabrication of layered devices or integration through the decrease of inter-diffusion between the layers. Results also suggest that processes are complex and other details than the source type should be carefully considered.

We investigated the relaxation of the irreversible magnetization in a series of 200 nm thick YBa2Cu3O7/PrBa2Cu3O7 [(YBCO)(n)/(PrBCO)(m)] superlattices, where the thickness m of the nonsuperconducting PrBCO layer (measured in unit cells) was kept to m = 4 (sufficient to decouple the superconducting YBCO layers), whereas the thickness n of the YBCO layer was varied between 2 and 20 unit cells. The analysis of standard zero-field-cooling dc magnetization relaxation data obtained in the low temperature T region with the applied magnetic field H oriented along the c axis reveals the occurrence of a crossover elastic (collective) vortex creep at low T-plastic vortex creep at high T, generated by the T dependent macroscopic currents induced in the sample during measurements. For thin superlattices (n < 20) the creep crossover temperature T-cr proportional to n, and T-cr decreases linearly with increasing ln(H) for a fixed n. This crossover represents an alternative to the elastic vortex glass behavior reported for superlattices, as well as to 'quantum vortex creep' at unexpectedly high T inferred for thin films. We also discuss the absence of an increase of the magnetically determined critical current density with decreasing YBCO thickness in our superlattices, which apparently contradicts the collective pinning theories.

Superconducting materials have contributed significantly to the development of modern materials science and engineering. Specific technological solutions for their synthesis and processing helped in understanding the principles and approaches to the design, fabrication and application of many other materials. In this review, we explore the bidirectional relationship between the general and particular synthesis concepts. The analysis is mostly based on our studies where some unconventional technologies were applied to different superconductors and some other materials. These technologies include spray-frozen freeze-drying, fast pyrolysis, field-assisted sintering (or spark plasma sintering), nanoblasting, processing in high magnetic fields, methods of control of supersaturation and migration during film growth, and mechanical treatments of composite wires. The analysis provides future research directions and some key elements to define the concept of 'beautiful' technology in materials science. It also reconfirms the key position and importance of superconductors in the development of new materials and unconventional synthesis approaches.

The relaxation of the irreversible magnetization in optimally doped YBCO films with natural and artificial pinning centres was measured in zero-field cooling conditions using SQUID magnetometry. The external magnetic field H was oriented along the c axis. An appropriate method for the determination of the characteristic vortex pinning energy from the normalized vortex-creep activation energy is discussed. This is based on the existence of a crossover elastic (collective) vortex creep at low temperatures T - plastic vortex creep at high T, caused by the T dependent macroscopic currents induced in the sample during magnetization measurements.

The temperature T variation of the normalized magnetization relaxation rate S in high-temperature superconductors (HTS) with strong vortex pinning exhibits a maximum in the low-T range. This was reported for various HTS, and the origin of the faster relaxation at low T appearing in standard magnetization relaxation measurements was usually related to specific pinning properties of the investigated specimens. Since the observed behaviour seems to be characteristic to all HTS with enhanced pinning (generated by random and/or correlated disorder), we show that the S(T) maximum can be explained in terms of classic collective vortex creep. The influence of thermo-magnetic instabilities in the low-T range is also evidenced. The collective (elastic) creep regime is generated by the T dependent macroscopic currents induced in the sample during standard magnetization measurements. (C) 2010 Elsevier B.V. All rights reserved.

Superconductor MgB2 has a significant potential for practical applications, but undesirable flux jumps in magnetization curves at low temperature and at moderate or intermediate magnetic fields prevent its widespread use. In the present work, we analyzed the flux-jumps tendency in MgB2 bulk doped with SiC, B4C and metallic Mg. Samples were prepared by field-assisted-sintering (FAST) as composites with up to three intercalated Fe-foils. Samples produced by FAST showed quite different phase structures clearly influencing pinning and thermo-magnetic instability features due to inhomogeneous materials structure or due to dopants. The largest flux jumps are observed in samples with high critical current density, as usually observed in conventional MgB2 bulks. However, jumps patterns are different and do not perfectly follow the jumps critical current dependence, especially for the samples with Mg-addition.

We report on magnetization data obtained as a function of temperature and magnetic field in Li-2(Pd0.8Pt0.2)(3)B and Li2Pd3B non-centro-symmetric superconductors. Reversible magnetization curves were plotted as M-1/2 versus T. This allows study of the asymptotic behavior of the averaged order parameter amplitude (gap) near the superconducting transition. Results of the analysis show, as expected, a mean field superconducting transition for Li2Pd3B. By contrast, a large deviation from the mean field behavior is revealed for Li-2(Pd0.8Pt0.2)(3)B. This is interpreted as due to the strength of the non-s-wave spin-triplet pairing in this Pt-containing compound which produces nodes in the order parameter and, consequently, phase fluctuations. The diamagnetic signal above T-c(H) in Li2Pd3B is well explained by superconducting Gaussian fluctuations and agrees with the observed mean field transition. For Li-2(Pd0.8Pt0.2)(3)B the diamagnetic signal above T-c(H) is much higher than the expected Gaussian values and appears to be well explained by three-dimensional critical fluctuations of the lowest-Landau-level type, which somehow agrees with the scenario of a phase mediated transition.

We investigated the influence of fullerene (C-60) addition on the superconducting parameters of MgB2 bulk samples obtained by spark plasma sintering (SPS). It was found that 1.5 wt% C-60 addition leads to the reduction of the critical temperature by a few K, whereas the magnetically determined critical current density increases by approximately one order of magnitude in an applied magnetic field H = 70 kOe at temperature T = 10 K. This indicates substitution of B by C in C-60 added MgB2 processed by SPS, contrary to some data reported in the literature obtained using conventional methods. For our relatively large specimens, the occurrence of macroscale flux jumps was observed over a wide (H, T) domain. The relaxation of the irreversible magnetization suggests that the macroscale flux jumps transform into microscale flux jumps with increasing H and T

Non-centrosymmetric superconductor Li-2(Pc1-xPtx)(3)B, x = 0-1 was synthesized from mixtures of the elements. A simple semi-open method is proposed using endings-pressed stainless steel tubes placed in a high-vacuum furnace. Heating regime employed a short-time overheating at 900 degrees C and a slow cooling step between T-s and 550 degrees C within 3 h. To adequately compensate Li-losses and attain maximum critical temperature, the optimum T-s and starting Li-content were found to change from 720 to 740 degrees C and from Li-2.4 to Li-2.6, respectively, when x was changing from 0 to 1. It was shown that placing Li separately in the tube also produces superconducting samples. Li being supplied to the (Pd,Pt)-B mixture through the vapour transport. This result enables the possibility of thin films growth using a (Pd,Pt)-B precursor film heat treated in a Li-vapour atmosphere. Preliminary results on thin films growth are introduced. (C) 2009 Elsevier B.V. All rights reserved.

Commercial wires of Nb3Sn and NIgB2 were inspected through X-ray cone-beam micro-tomography (mu CT). Details of the architecture of the wires of different topologies were visualized. In the case of MgB2 wires this allowed to compare the geometrical perfection of the component elements between the wires with 18 and 7 superconducting sub-elements heat treated for different conditions. Defects such as 3D voids and interruption of the diffusion barriers were also visualized. High resolution 3D-mu CT observations of the Nb3Sn wire architecture allowed also direct and non-invasive determination of the twist-pitch parameter. 3D tomography shows important advantages over 2D traditional microscopy methods.

In order to study the mechanism of the small n-value for Bi2212, E - J characteristics were measured carefully for various kinds of Bi2212 tapes and round wires in high magnetic fields. Some of wires were heat-treated in a magnetic field of 5 T. We found that the n-values of all the samples increase by the in-field heat-treatment at 5 T. In addition, we analyzed the E - J properties by the combination of the percolation model based on the local J(c) distribution and the two directional J(c) distribution model. The improvement of the n-value by the in-field heat treatment can be understood by the change of the aspect-ratio of the grains. Therefore, the aspect-ratio of the grains plays an important role in the current transport influencing not only J(c) but also n-value.

We attempted to grow non-c axis heterostructures of substrate-IS type with S = BSCCO and I = (Sr, Ca)CuO(2). A careful selection of the films-substrate relationship is revealed as a key condition toward growth of layered heterostructures with different orientations. However this powerful principle, that is also a mandatory condition, is not sufficient in order to obtain high quality structures. The reasons are discussed looking for further solutions. Our comparative analysis is expanded to other heterostructures we reported in other works trying to reveal some of the more general problems of the non c-axis heterostructures growth.

Thin films of (001) Bi2Sr2Ca2Cu3O10 With high zero-resistance critical temperature T(c)0 = 75-95.1 K and low roughness up to three half-c-axis unit cells were grown by metal-organic chemical vapor deposition (MOCVD) on substrates with large film-substrate lattice mismatch and different film-substrate mismatch anisotropy. Comparative analysis of the films on (001) and (110) MgO and NdGaO3 suggests that Bi-2223 films can easily accommodate large mismatch film-substrate differences, while mismatch on different directions, that is, mismatch anisotropy, has a strong influence on the quality of the film. The highest quality (low roughness, high uniformity, and high T-c0(R=O)) is obtained when mismatch anisotropy, taken as the mismatch ratio (r), is given only by compressive or only by tensile mismatch stress, and it is around 1, that is, it is as for the (001) MgO substrate. Mismatch anisotropy (value and sign) is an important parameter and can be used to tune superconducting properties of the film.

Four-cation nanograined strontium and magnesium doped lanthanum gallate (La0.8Sr0.2) (Ga0.9Mg0.1)O3-delta (LSGM) and its composite with 2 wt% of ceria (LSGM-Ce) were prepared. Morphologcally homogeneous nanoreactors, i.e., complex intermediate metastable aggregates of desired composition were assembled by spray atomization technique, and subsequently loaded with nanoparticles of highly energetic C3H6N6O6. Rapid nanoblast calcination technique was applied and the final composition was synthesized within the preliminary localized volumes of each single nanoreactor on the first step of spark plasma treatment. Subsequent SPS consolidations of nanostructured extremely active LSGM and LSGM-Ce powders were achieved by rapid treatment under pressures of 90-110 MPa. This technique provided the heredity of the final structure of nanosize multimetal oxide, allowed the prevention of the uncontrolled agglomeration during multicomponent aggregates assembling, subsequent nanoblast calcination, and final ultra-rapid low-temperature SPS consolidation of nanostructured ceramics. LaSrGaMgCeO3-delta nanocrystalline powder consisting of similar to 11 nm crystallites was consolidated to LSGM-Ce nanoceramic with average grain size of similar to 14 nm by low-temperature SPS at 1250 degrees C. Our preliminary results indicate that nanostructured samples of (La0.8Sr0.2)(Ga0.9Mg0.1)O3-delta with 2 wt% of ceria composed of similar to 14 nm grains can exhibit giant magnetoresistive effect in contrast to the usual paramagnetic properties measured on the samples with larger grain size.

Superconducting SiC and B4C-doped MgB2 samples containing up to three layers of pure Fe have been prepared by Field-Assisted-Sintering Technique (FAST). The adhesion between the Fe and doped-MgB2 layers is excellent due to the enhanced local interdiffusion and increased solubility of Fe into MgB2 grains that are typical for the non-equilibrium processes. Magnetic measurements showed the largest irreversibility, hence, the largest critical current density in the B4C-doped sandwich with one Fe foil. Additionally, the drawback of flux jumps at low temperatures is almost absent for one Fe-layer sandwiches. However, the irreversibility is smaller than in pure MgB2 and SiC-doped MgB2 samples prepared by the same technique, but without the insertion of Fe foil. When the number of Fe foils is increased to three and an excess of 5 % wt. Mg is added, the SiC-doped sandwiches show almost similar irreversibility values and field dependence (at 5 K and at 20 K) as the pristine MgB2 samples without Fe. But, the flux jump is recovered at the same level found for the pristine MgB2 without Fe. An explanation in terms of doping dependence of the ratio between the thermal and magnetic diffusion constants is proposed.

The relaxation of the irreversible magnetization of MgB2 bulk samples obtained by electric-field assisted sintering was investigated using the SQUID magnetometry for a magnetic field H up to 50 kOe applied in zero-field-cooling conditions. We observed a crossover plastic creep at high temperatures T-elastic creep at low T, described by H alpha T-2 in the low T range, which appears to be caused by the macroscopic currents induced in the sample during magnetization measurements. By decreasing T below this line the determined creep exponent rapidly overcomes the widely accepted theoretical values for elastic (collective) pinning. This behaviour can easily be explained through the occurrence of micro flux jumps, leading to a finite magnetization relaxation rate in the low-T limit. (C) 2008 Elsevier B.V. All rights reserved.

Field-assisted-sintering technique (FAST) has been employed to obtain polycrystalline MgB2 samples, pristine and doped with 5 mol % SiC and B4C, using commercial MgB2 powder. The mass density of the samples is around 90% of the theoretical value. The response in magnetic field shows that the upper critical field and the irreversibility field are depressed by comparison with pristine MgB2. The latter has an upper critical field H-c2=14.37 T close to the values reported for the single crystals. Scaling analysis of the field dependence of the pinning force suggests that both addition of SiC and B4C stabilizes two well defined pinning regimes in FAST-processed MgB2. At low temperatures, T < 24 K (H <= 5T), the pinning occurs at the grain boundaries whereas at higher temperatures there is a mixed pinning. These effects are supposed to be the combined result of relatively low level of C diffusion into the lattice of MgB2, specific features in formation of the grain boundaries during FAST processing and the influence of the added materials on morphology. At high fields (above 8.5T) and 4.2K, doped samples are superior to the pristine one from the critical current density viewpoint.

Materials may show anisotropic properties on different crystal directions and this is also the case of High Temperature Superconductors (HTS). To take advantage of the materials anisotropy one concept of interest is "orientation engineering" in thin films. This can be realized through the control of the film-substrate lattice relationship. Some examples in this regard are presented in this work and through comparative analysis we try to evaluate the viability of this approach and of he entcountered problems. It is expected that in the future this approach will generate new nano composite materials with new properties and effects leading to development of new devices with new or improved functionality.

Recently, MgB2 was discovered to be a superconductor with a surprisingly high critical temperature of about 39 K and with significant potential for applications. This material is usually prepared from a mixture of Mg and B in sealed tubes with excess Mg. As-prepared samples usually are very porous and mechanically weak. High density superconducting samples of MgB2 undoped and doped with SiC and B4C were produced by Field Assisted Sintering Technique (FAST) (T-c = 38.5 K). Samples are relatively large of 1.9 cm in diameter, apparently uniform, and can be easily extracted from the die. Processing times are short for easily attainable and relatively low temperatures. The effects of FAST consolidation on crystalline morphology revealed by microtomography and Scanning Electron Microscopy (SEM) and bulk density were investigated. Most samples have bulk density above 90% of the theoretical one. Despite such high bulk density, microtomography in combination with SEM revealed that in the samples there are some regions of low and high density. High density regions are not the consequence of FAST processing and they were observed in the raw material.

Room temperature mechanical treatment consisting of multiple torsion loadings (named pre-torsion) was applied to Nb3Sn composite wires with different architecture to reduce thermal residual compressive strain experienced by the superconducting Nb3Sn filaments. Due to this effect all investigated wires have shown enhancement of the critical current density, I-c up to 56% at 15T and 4.2K. Enhancement of I-c was larger for the reinforced wires than for the wires without reinforcement suggesting that reinforcement is useful in strain relaxation during pre-torsion. The best results were obtained when the position of the reinforcement was located in the outer region of the wire. Pre-torsion is similar or more efficient than cycles of bending loadings (named pre-bending). For pre-torsion important parameter is rotation angle per length of the wire and optimum conditions for short wires are valid for long wires. Uniformity of Ic along the length of a 99cm wire after pre-torsion was within +/-2.1A.

Superconducting c-axis thin films of Bi2Sr2Ca2Cu3O10 (Bi-2223) were grown by MOCVD on (001) and (110) MgO substrates. Films on both substrates show, as revealed by AFM investigations, similar morphology composed of regular rectangular grains and relatively low roughness of about two or three half c-axis unit cell order. AFM images also suggest that films might have in-plane epitaxy. The films have zero resistance critical temperatures of 95.1K for the (001) MgO substrate and 75K for the (110) MgO substrate, respectively. Considering very large films-substrate lattice mismatch between (110) MgO and (ab)-plane of the superconducting phase the growth of indicated films is a surprise.

Bulks and tapes of MgB2 with 5 wt.% SiC were prepared from Mg, B and SiC. Mixing of the raw powders was performed in Ar atmosphere by high energy milling using a planetary mill. Number of balls (10 or 20), size (10 mm or 7 mm, respectively), rotation speed (200 rpm or 400 rpm) and milling time (up to 3 h) were varied. Powders were compared through XRD and SEM. From the as-prepared powders, bulk and tape samples were prepared and investigated by magnetic (SQUID) and transport (four-probe method) measurements. Results suggest that through variation of the milling conditions such as rotation speed, size and number of balls it is possible to control the value of the critical current density, J(c) and the slope of the J(c)(B) curve, For different heat treatment conditions milling with 400 rpm and using 20 balls of 7 mm always resulted in lower J(c)(B) than for the tapes or bulks produced from hand-milled mixture. Use of 10 balls of 10 mm keeping all the other conditions constant changed the slope of the J(c)(B) curve possibly improving J(c) above a crossover at 4 T. Mild milling with a rotation speed of 200 rpm (20 balls x 7 mm) resulted in enhancement of J(c) in the entire investigated region B 14 T leading to lower J(c)-values. The best samples had at 4.2 K J(c) = 3.6 x 10(-2) A center dot cm(-2) at 14 T and J(c) = 5 x 10(3) A center dot cm(-2) at 10 T.

Well-compacted MgB2 specimens with the density higher than 90 % of the theoretical value were obtained by electric-field assisted sintering. This method assures a good grain connectivity, which leads to the appearance of efficient pinning centres at the grain boundaries. We measured the DC magnetization curves and the relaxation of the irreversible magnetization using the SQUID magnetometry for a magnetic field H up to 50 kOe applied in zero-field-cooling conditions. The critical current density is of the order of 1010 A/m(2) at H = 20 kOe and T = 10 K. A crossover plastic creep at high temperatures T - elastic creep at low T described by H proportional to T-2 in the low T - high H domain was observed. This is caused by the macroscopic currents induced in the sample during magnetization measurements. By decreasing T below this line the determined creep exponent rapidly overcomes the widely accepted theoretical values for elastic (collective) pinning. This behaviour can be explained through the occurrence of micro flux jumps, which seem to be responsible for the finite magnetization relaxation rate in the low-T limit. The relaxation of the irreversible magnetization allowed us the precise determination of the characteristic pinning energy barrier.

It is shown that x-ray microtomography (XRT) is a powerful technique to observe on extended volumes the morphology, alignment and local bulk density in MgB2 tapes, thin films and especially bulk specimens. For the bulk samples obtained from mechanically milled powders for different conditions, several types of the 3D microstructural patterns were observed. These significant differences between the samples were not revealed by SEM. Microtomography can be a useful additional technique to characterize the samples and to obtain unique information, e. g. on local bulk density, but it cannot replace the existing methods: advantages and limitations are discussed. It is concluded that the method is promising and further developments are expected to be helpful for a better understanding of the complex processing-microstructure-properties relationship in the MgB2 superconductor.

In this work we focus on the microstructural and magnetic characterization of CuNb/Nb3Sn wires with different architectures (design and reinforcement). The microstructural characterization was performed using scanning electron microscopy. AC magnetic susceptibility was measured with field applied both parallel and perpendicular to the wire axis. The heat treatment performed to form the A-15 superconducting phase leads to partial spheroidization followed by coarsening of the Nb filaments in the reinforcement material. The differences concerning the microstructure of the reinforcement material among the investigated wires were reflected in the broadening of the superconducting transition of Nb, more evident for a field applied parallel to the wire axis. From the magnetic data the wires were also compared in terms of the superconducting volume fraction.

We study the superconducting order parameter in the non-centrosymmetric compounds Li-2(Pd1-xPtx)(3)B (x = 0, 0.3, 0.7 and 1) by measuring magnetic penetration depth lambda(T). The low temperature lambda(T) shows a linear temperature dependence for x >= 0.3, but follows exponential-like behavior for lower Pt contents. These findings suggest that a spin-triplet state might gradually develop with increasing x due to the broken inversion symmetry. Published by Elsevier B.V.

The tensile strain dependence of the upper critical field B-c2 for Nb3Sn wires was measured using a new apparatus for applying tension at low temperature. The critical current I-c calculated from the strain-dependent B-c2 measurements is the almost consistent with the measured I-c. In the measurements by a new apparatus, the axial and the lateral applied strains were examined by the strain gauges attached onto the wire. The deviatoric strain epsilon(dev) and the hydrostatic strain epsilon(hyd) were estimated by the axial and the lateral strain. We found the deviatoric strain dependence of B-c2 is different between the tensile and compressive strain states. This means that the hydrostatic strain also should be taken into account in order to understand the strain effects on the superconducting properties of Nb3Sn.

Sr2FeMoO6 was synthesizes by soft chemistry route using citric and/or oxalic acid as complexing agents. This method provides good compositional control with promising results as a base for further improvements. The material shows complex temperature- and field(magnitude and orientation) dependent electro-magnetic behavior as probed by magnetic and transport measurements. The zero-field cooling curves of magnetization versus temperature taken at different magnetic fields, show two temperature regions separated by a transition temperature T-cups(ZFC). When H increases, T-cups(ZFC) values decrease. At 5 K and 5 T the saturation moment is 3.55 JIB per formula unit, and the coercitive force is 0.021 T. The relative value of the magnetoresistive effect (i.e. 100 (rho(H)-rho(0))/rho(H), %, with rho being resistivity) at 5 K is 68% and 36% when applied field H is parallel and perpendicular the measuring current I, respectively. The results are discussed in relation to magnetic sublattices and the interaction that produces anti-site defects and spin-dependent electron anisotropy. (C) 2006 Elsevier B.V. All rights reserved.

Relaxation of the thermal residual strain in Nb3Sn wires is realized through cycles of multiple torsion loadings ('pre-torsion') at room temperature. As a consequence, the critical current, I-c, is enhanced. This effect is stronger than previously reported mechanical treatments of multiple bending ('pre-bending'). The maximum I-c is attained for complex mechanical treatments of pre-torsion and pre-bending. Complex treatments allow efficient and relatively independent control of residual strain relaxation over all three directions of the wire, resulting in enhancement of I-c towards the theoretical limit of the material. Our findings have an immediate positive impact on the performance of Nb3Sn wires and, hence, on their applications (e.g. react-and-wind coils).

Critical temperature T-c of the Li-2(Pd1-xPtx)(3) B was reported to be 7-8 K for x = 0 and 2.2-2.8 K for x = 1. In this article we present our preliminary results on behavior of magnetization-temperature curves with starting composition of Pd-B precursor, y-Li concentration in LiyPd3B and post-annealing of the Pd-end compound. Results suggest that to maximize T-c ratio Pd: B should be close to 3: 1, while y-Li has to be optimum. The lowest T-c for LiyPd3B was 4.4-4.6 K, while post-annealings at 560 degrees C allowed enhancement of T-c up to 8.2-8.4 K. Compositions Li(2)Z(3)B with Z = Ni, Ru, Rh, Re, Ag are not superconducting down to 1.8 K. Exception is composition with Re showing superconductivity due to Re3B compound. All samples were prepared by arc melting. (c) 2007 Elsevier B.V. All rights reserved.

Samples of (Bi,Pb)(2)Sr2Ca2Cu3O10 (Bi(Pb)-2223) phase have been fabricated from two different oxide precursors with the same stoichiometry, synthesized by solid state reaction in the air at 815 degrees C for 20 h. The first precursor was prepared by mixing Bi2O3, PbO, SrCO3, CaCO3 and CuO powders, while the second one through mixing Bi2O3 and PbO with Sr2Ca2Cu3Ox produced from SrCO3, CaCO3 and CuO powders. Pellets from the two precursors were prepared in the same conditions; heat treatment time was varied and intermediate grindings were applied. Although the maximum attained Bi(Pb)2223 phase amount was about 50% and above 90% in the samples from the two precursors, respectively, the samples from the first precursor have generally shown better superconducting properties such as the critical temperature from resistivity measurements and intragrain critical current J(cg) from magnetic susceptibility measurements. For our particular case the influence of the final heat treatment is relatively low and at the same time the precursor plays a major role in controlling growth processes and final superconducting properties. Lower room-temperature Seebeck coefficient of the thermoelectric power for the samples fabricated from the first precursor suggests that one mechanism through which this control is realized might be the modification of the oxygenation level in the samples produced from different precursors. It was also found that for the samples prepared from the two precursors, intermediate grinding after 110h or more of heat treatment enhances density, almost does not influence J(cg) (or slightly improves it), decreases T-c, and does not influence significantly the amount of Bi(Pb)-2223 phase.

Field Activated Sintering Techniques (FAST) are increasingly used to consolidate metal and ceramic powders. They combine application of a pulsed electrical current with external pressure to activate the densification process. The nature of electrical field/current interaction with powder systems is not clear yet. In this regard, in-situ transport measurements and microstructural analyses were carried out during pulsed current application in the FAST processing of Ni powders. Our experimental results were compared with existing electrical conduction theories and observed effects were relatively well explained qualitatively within these theories. Under electrical field it was confirmed that no voltage-current phase-shift occurs at elevated operating interfacial temperatures. For the field situation a higher applied pressure is decreasing the contact instability among particles contacts and of the sintering onset temperature. Microstructural investigations of the FAST-sintered samples indicate rather distribution of the higher density regions and a considerable increase of neck formation above 340 degrees C.

Field Assisted Sintering Technique (FAST) is currently used to consolidate ceramic, metal and composite powders. This method combines a pulsed electrical current with simultaneous application of an external pressure. In this article we report fabrication by FAST of high density MgB2 ceramic with addition of 5% SiC and 5% B4C. The influence of sintering conditions such as temperature and time on bulk density, morphology and superconducting properties of the samples was investigated. All samples had bulk density of more than 90% of the theoretical one and the same critical temperature T-c = 38.5 K from magnetisation measurements. These preliminary results suggest that FAST is a promising method for processing of MgB2 superconductor.

First-order branched tree structures of MoO3 belts on sillimanite fibers (refractor wool) were grown by a vapor transport method. At longer growth times, MoO3 micro-belts on micro-belts form a flower-like structure. Most belts are of alpha-MoO3, and they grow in the two opposite directions along the c-axis. They show a high level of crystal quality, clean surfaces, sharp edges, and a triangular-shape tip with certain angles. The most frequent are angles of 47 degrees and 94 degrees. The growth mechanism is of vapor-solid type. In the initial stages of growth, elements specific for spontaneous spread and island formation on the surface of the sillimanite fibers described in the literature are observed. Significant enhancement of the thickness suggests that a layer-by-layer 2D growth is also probable. It is thought that responsible for such growth is direct vapor deposition of the Mo-O vapors on the already formed belts, this being similar to thin film growth. Curved surfaces of the substrate (in our case of the sillimanite fibers), on which the MoO3 belts are growing, are important and can be used for the directional growth control of the belts and formation of hierarchical structures. The vapor transport method allows the formation of beta-MoO3 belts that grow in the b-axis direction.

Six practical composite wires of Nb3Sn (Furukawa Electric Co, Ltd) with different architectures ( design and reinforcement) were compared from the normal state resistance R, critical temperatures T-c(onset), T-c(offset) and Delta T-c, upper critical field B-c2 ( at 4.2 K) and critical current density J(c) points of view. Wires were as follows: three of near-the-edge reinforcement design with Nb reinforcement of 0, 21, 50 vol% in the CuNb region, and two of central reinforcement design with Nb of 21 and 50 vol%. One wire with near the edge 50% vol Nb reinforcement had a different reinforcement/superconductor ratio. As-reacted wires show very different patterns of R, T-c(onset), T-c(offset), Delta T-c, B-c2 and J(c). For the superconducting parameters this is probably due to different 3D thermal residual strains. Data suggest that the architecture of the as-reacted wire can control residual strain values and distribution. During multiple bending of the wires at room temperature ( named pre-bending), introduction of the reinforcement improves relaxation of the 3D residual strain and especially of the lateral components. As a consequence, B-c2 and J(c) versus pre-bending strain, epsilon(pb), are enhanced to values closer to those of the Nb3Sn in the stress-free state. Relative enhancement of these critical parameters for the reinforced wires is higher than for the reinforcement-free wire. Evolution during pre-bending and maximum attained absolute values of the superconducting parameters can be grouped roughly as a function of near-the-edge or central reinforcement design. Variation of the superconducting parameters suggests that the pre-bent state may depend on the as-reacted one ( which is a function of wire architecture and processing history); when J(c) was low as in the case of as-reacted wires with central reinforcement, during pre-bending, despite a relatively high J(c) enhancement, this parameter attained lower absolute maximum values than for the other wires. Depending on the wire, when pre-bending strain epsilon(pb) = 0.8 - 1%, the enhancement of non-Cu J(c) at 4.2 K in the pre-bent wire is by up to 43.5% at 15 T compared to the as-reacted case. The maximum absolute value of J(c) is obtained for the near-the-edge reinforcement pre-bent wires with 21 and 50% vol Nb. B-c2 of these wires was lower than for the other reinforced wires and higher than for the reinforcement-free wire. Pre-bent wires with near-the-edge reinforcement are identified as new and promising candidates for fabrication of react-and-wind coils with improved performance.

Two practical Nb3Sn composite wires (short samples) were investigated from the points of view of critical current, I-c, and cracks evolution versus number of bending load cycles. Bending was applied manually at room temperature using a block-form with curved surface corresponding to applied bending strains of 0.5% and 0.8%. It was applied in plane, alternatively in one direction and in the opposite one up to 130 times. We shall use for this mechanical treatment term pre-bending. The wires had approximately the same diameter but a different architecture: one was of conventional type (standard US-Japan wire, Hitachi Cable) and the second one was CuNb reinforced wire (Furukawa Electric Co. Ltd.) with reinforcement located near-the-edge. It was found that critical current maximizes gradually with the number of bendings and the maximum value of I-c, is attained for a number of bending loadings, N-pb, of about 15. Beyond this optimum N-pb, critical current is constant. Optimum N-pb is likely not dependent on the wire, applied field or pre-bending strains. Results suggest that Cu is important in the work hardening process. Work hardening during pre-bending is imposing limitations in application of this technically convenient mechanical treatment for release of the residual strain and further enhancement of I-c. Semi-quantitative analysis of the electron microscopy observations shows that for our experimental conditions the density of cracks is approximately constant being in agreement with described I-c, behavior. Other possible consequences of our results are discussed. Among the most interesting issues is possibility of the 3D independent control of yielding and hence of residual strain release. Several new practical ideas that will need future confirmation are proposed: e.g. application of loading-unloading cycles of torsion treatment in combination with tensile or pre-bending treatments might be useful.

We investigated MOCVD growth of c-axis two-layer and three-layer stacked heterostructures on (100) SrTiO3 of SI, IS or SIS type. S denotes high temperature superconductor thin films of YBa2Cu3O7 (Y-123), Bi2Sr2Ca2Cu3O10 (Bi-2223) or Bi2Sr2CaCu2O8 (Bi-2212), while I stands for insulating thin films of (Ba, Ca) CuO2 or (Sr, Ca) CuO2. X-ray diffraction, atomic force microscopy and measurements of resistivity versus temperature were performed after the deposition of each layer. The best results, suitable for further device fabrication, were obtained for the SIS structure (100) SrTiO3/Bi-2223/(Sr, Ca) CuO2/Bi-2212. Similar structures with I = (Ba, Ca) CuO2 have shown higher impurity phases and lower superconducting quality of the top superconducting layer. For two-layer or three-layer structures, Bi-2223 as a top layer could not be obtained and, instead, a phase with Bi-2212 formed. Structures with (100) SrTiO3/Y-123/(Sr, Ca) CuO2/Y-123 or (100) SrTiO3/Y-123/(Ba, Ca) CuO2/Y-123 were also promising, but a current leak often occurred due to greater roughness. Structures with Y-123 are less sensitive to growth temperature than those with BSCCO.

High density (more than 90% of the theoretical density) bulk samples with relatively large size (2.0 cm in diameter) of MgB2, pristine and doped with 5 mol% SiC and B4C were obtained by the field-assisted sintering technique (FAST) from commercial MgB2 powder. The superconducting properties in the magnetic field of the doped samples show depressed upper critical field H-c2 and irreversibility field H-irr when compared with pristine MgB2. The reason for better H-c2 and H-irr in the undoped sample is not clear. Most probable is that this is due to the limited diffusion time which restricts the substitution of carbon for boron in this short-time processing method as well as due to the way grain boundaries are formed in the FAST process. However, all our samples have shown higher values of H-c2 and H-irr than the values reported previously for FAST-MgB2 samples. The data were further investigated through scaling analysis. Data suggest that both additions of SiC and B4C stabilize two well defined pinning regimes in FAST-processed MgB2. At low temperatures, the pinning occurs at the grain border whereas at high temperatures, T >= 24 K, there is mixed pinning (H <= 5 T).

We investigate the order parameter of noncentrosymmetric superconductors Li2Pd3B and Li2Pt3B via the behavior of the penetration depth lambda(T). The low-temperature penetration depth shows BCS-like behavior in Li2Pd3B, while in Li2Pt3B it follows a linear temperature dependence. We propose that broken inversion symmetry and the accompanying antisymmetric spin-orbit coupling, which admix spin-singlet and spin-triplet pairing, are responsible for this behavior. The triplet contribution is weak in Li2Pd3B, leading to a wholly open but anisotropic gap. The significantly larger spin-orbit coupling in Li2Pt3B allows the spin-triplet component to be larger in Li2Pt3B, producing line nodes in the energy gap as evidenced by the linear temperature dependence of lambda(T). The experimental data are in quantitative agreement with theory.

High quality superconducting thin films of HTS have been grown by MOCVD on substrates with artificial steps of predefined height and width. The surface of the films grown on the steps having width equal to the 'double of the migration length' of the atomic species depositing on the substrate is totally free of precipitates: precipitates are gathered at the step edges where the free energy is lowest. The method has several advantages: it is simple, universal (it is independent of the materials, substrates, deposition technique or application) and allows control of precipitates segregates so that the quality and growth conditions of the films are the same as for the films grown on conventional substrates. The method is expected to result in new opportunities for the device fabrication, design and performance.

We report successful growth of high-quality thin films with clean and completely precipitate-free surface, suitable for device applications, by applying a new concept and method to the substrates. The concept consists in generation of artificial steps of controlled height and width, and desired shape on the surface of the substrate. The width of the step is chosen so that it is equal to the double of the migration (surface diffusion) length of the atomic species in the growth process of the film. If precipitates occur, they will be selectively gathered to the step edge where the free energy is lowest. Using this new method, we have successfully obtained by MOCVD high-quality precipitate-free Bi-2223 and Bi-2223/Bi-2212-superlattice thin films on (100) SrTiO3 substrates with artificial steps of controlled width and height. These as-grown films have been further used to fabricate patterned intrinsic Josephson junctions. Completely precipitate-free films offer a strong advantage for integration, and generate new possibilities for the device fabrication.

To eliminate precipitates-segregates that can easily occur on the thin film surfaces of the multicomponent materials for electronics, a new approach is proposed, consisting of the following aspects: first, on the substrates, artificial steps of predefined height and width are produced, and second, films are grown on such substrates. The width of the step is taken equal to the 'double of the migration length' of the atomic species depositing on the substrate. In these conditions, precipitates migrate and gather at the step edges where the free energy is lowest and the resulting totally precipitate-free surface of the film on the step is suitable for device applications or integration purposes. The method has several other important advantages and they are discussed in the text. Using this new approach we present successful fabrication of a mesa structure showing intrinsic Josephson effect. We have used thin films of Bi-2212/Bi-2223 superstructure grown by MOCVD on (001) SrTiO3 single crystal substrates with artificial steps of about 20 mu m width. (c) 2006 Elsevier B.V. All rights reserved.

In this paper we focus on supersaturation and migration of the atomic species involved in the growth of oxide films in order to search for new efficient methods for growth of flat, uniform and precipitate-free complex thin films with high quality. In this respect we have applied MOCVD to HTS thin films, 'interrupted growth' (consisting of on/off vapour deposition cycles, keeping the temperature and atmospheric conditions constant), similar to 'pulsed laser interval deposition' reported in the literature. We show that MOCVD can be easily and successfully applied to suppress island growth, contrary to the currently accepted idea that this approach is unique to PLD. This suggests that principles of supersaturation-migration-supersaturation cycles are universal for the films' growth. By this approach, high-quality Bi-2223 thin films with a uniform flat surface, having roughness less than half the c-axis unit cell, were grown by MOCVD. Using substrates with artificial steps of predefined width equal to 'twice the migration length' totally precipitate-free thin films were obtained: precipitates-segregates of impurity phases (Cu rich for HTS materials) are gathered at the step edges where the free energy is lowest. As-prepared films were used to fabricate intrinsic Bi-2223 and Bi-2212/Bi-2223 SIS-type Josephson junctions (IJJs).

Recently, a double perovskite oxide, Sr2FeMoO6, has been reported to show a very sharp magnetoresistance (MR) response at relatively small-applied fields and at high temperatures. The half-metallic state of this compound ensures a theoretical magnetic moment of 4 mu(B) per formula unit. Ordering control is expected to be influenced by the synthesis route. In this regard, in this article, perovskite samples were obtained from the liquid phase, using oxalic acid as complexing agent. Application of a field above 0.08 T increases the zero-field-cooled (ZFC) magnetization. Below this field, for the ZFC-curves measured from 2 K up to 400 K, magnetization increases, reaching a peak at T-cups(ZFC), before decreasing cups gradually to a paramagnetic state. Saturation moment is relatively low (2.1-2.2 mu(B)), probably due to anti-site defects, as suggested in the literature.

In this paper we present a penetration depth study on the newly discovered superconductors Li2Pd3B and Li2Pt3B. Surprisingly, the low-temperature penetration depth lambda(T) demonstrates distinct behavior in these two isostructural compounds. In Li2Pd3B, lambda(T) follows an exponential decay and can be nicely fitted by a two-gap BCS superconducting model with a small gap Delta(1)=3.2K and a large gap Delta(2)=11.5K. However, linear temperature dependence of lambda(T) is observed in Li2Pt3B below 03T(c), giving evidence of line nodes in the energy gap.

The cobalt oxide superconductor NaxCoO2 center dot yH(2)O is studied by angle-resolved photoemission spectroscopy. We report the Fermi surface (FS) topology and electronic structure near the Fermi level (E-F) in the normal state of NaxCoO2 center dot yH(2)O. Our result indicates the presence of the hexagonal FS centered at the Gamma point, while the small pocket FSs along Gamma-K direction are absent, similar to NaxCoO2. The top of the e(g)(') band, which is expected in band calculations to form the small pocket FSs, extends to within similar to 30 meV below E-F, closer to E-F than in NaxCoO2. We discuss its possible role in superconductivity, comparing with other experimental and theoretical results.

Magnetization M(H,T) and M(T,H) curves with magnetic field approximately parallel and perpendicular to the c-axis of Na0.35CoO2.1.3H(2)O superconducting crystals have been measured (T-c = 3.7 K). The shape of the M(H,T) loops resembles Bi-based high-T-c superconductors (HTS), but the superconducting anisotropy is below that of Bi-system; this parameter is as for HTS with middle or moderately high anisotropy. (c) 2006 Elsevier Ltd. All rights reserved.

We review the current status of the growth, characterization and applications of Bi-Sr-Ca-Cu-O (BSCCO) whiskers from the materials science point of view. Our analysis leads to the conclusion that reconsideration of the importance of the whisker studies is necessary; whiskers can play a major role in studies of the growth mechanism and defects, properties control and their understanding, and new devices and applications. Arguments favourable to the idea that BSCCO whiskers can possibly have a significant impact on future synthesis of nano-objects in this system or other high-T-c superconducting systems, as well as in investigation and understanding of the growth processes under elevated magnetic fields, are discussed. Emphasis is made on superconducting whiskers, but non-superconducting ones are also briefly addressed.

Thin films of MgB2 on r-cut Al2O3 substrates have been grown by pulsed-laser deposition (PLD) using a Nd-YAG laser (fourth harmonic-266 nm) instead of the popular KrF excimer laser. The growth window to obtain superconducting films is laser energy 350-450 mJ and vacuum pressure with Ar-buffer gas of 1-8/10 Pa (initial background vacuum 0.5-1 x 10(-3) Pa). Films were deposited at room temperature and post-annealed in situ and ex situ at temperatures of 500-780 degrees C and up to 1 h. Films are randomly oriented with maximum critical temperature (offset of resistive transition) of 27 K. SEM/TEM/EDS investigations show that they are mainly composed of small sphere-like particles (<= 20 nm), and contain oxygen and some carbon, uniformly distributed in the flat matrix, but the amount of Mg and/or oxygen is higher in the aggregates-droplets (100-1000 nm) observed on the Surface of the film's matrix. Some aspects of the processing control and dependences on film characteristics are discussed. The technique is promising for future development of coated conductors.

Fe-sheathed tapes of MgB2 with addition of SiC have been prepared by the powder-in-tube (PIT) method using a powder mixture mechanically milled in an argon or hydrogen atmosphere. The reactivity of the component powders in the mixtures, Mg, B and SiC, was significantly enhanced by mechanical milling, so that MgB, formed faster than in tapes fabricated from a hand-milled mixture. At the same time the number of impurity phases was higher, and the impurity phases of Mg2Si and Fe2B were observed only in these tapes. Mechanical milling also induced a lower quality of MgB2, especially for tapes produced from powders milled in a hydrogen atmosphere, with a significant influence on the values of the critical temperature T-C and critical field, J(C). (c) 2005 Published by Elsevier B.V.

Several articles report two-layer c-axis heterostructures of Bi4Ti3O12 on BiSrCaCuO. However in some applications, or for integration purposes, multi-layer geometries composed of alternating c-axis or non c-axis thin films might be useful. From this perspective we investigated growth of c-axis and non c-axis BiSrCaCuO on Bi4Ti3O12 structures. The paper mainly focuses on evaluation of the structures from the growth, stability/interdiffusion, uniformity/morphology points of view based on structural and microstructural data.

Recently we have found superconductivity in a cubic antiperovskite-like compound Li2BPd3. A new pseudo-binary complete solid solution Li2B(Pd1-xPtx)(3), x = 0-1 with similar structure has been synthesized and observation of superconductivity in the entire x-range is reported. Our results strongly suggest that superconductivity is of bulk type. Critical temperature T, is decreasing approximately linearly with amount (x) of Pt from 7.2-8 K for Li2BPd3 to 2.2-2.8 K for Li2BPt3. From isothermal magnetization (M-H) measurements, lower critical fields H-cl (138Oe/(x=0), 38Oe/(x=1)), upper critical fields H-c2(WHH) (3.4 T/(x=0), 1 T/(x=1)), coherence length xi(0) (9.8 nm/(x=0), 17.9 nm/(x=1)) and penetration depth lambda(0) (190nm/(x=0), 364nm(x=1)) were estimated and shown to follow approximately linear dependencies with.x, either. Structure and superconducting similarities with MgCNi3, viewed as a bridge between low and high T-C superconductors are increasing the expectations that Li2B(Pd1-xPtx)(3), x = 0-1 superconductor can be included in the same class of `intermediate' superconductors. For x = 0-1 a weak fishtail effect was observed at low and intermediate fields. Apart from this effect, some samples for x = 1 have shown magnetization jumps at fields close to H-c2.

Growth of such non-superconducting whiskers [Sr2.24Ca0.4Al2Ox, (Ca0.8-0.85Sr0.15-0.1)(2)CuO3, CuO, or Bi2.44Sr2Ca1.3-2Cu6.9-9.95Al0.35-0.46Ox (Cu-rich whiskers)] formed during the growth of Bi-2212 superconducting whiskers from powder or glassy substrates, is discussed. These whiskers are likely to grow from the bottom end, and there is a tight relationship with the growth of the Bi-2212 whiskers. A general reaction-path model for the whisker growth in the BSCCO system, independent of the type of the catalytic impurity and substrate, is proposed. When whiskers are grown under magnetic fields, up to 10 T, changes in the whisker size, aspect ratio, and morphology are observed.

Magnetization in dc magnetic fields and at different temperatures has been measured on the antiperovskite Li2Pd3B with a cubic structure composed of distorted Pd6B octahedrons. This material was recently found to exhibit superconductivity at 7-8 K. The critical fields H-c1(0) and H-c2(0) are determined to be 135 Oe and 4 T, respectively. Critical current density, scaling of the pinning force within the Kramer model, and irreversibility field data are presented. Several superconductivity parameters were deduced: Coherence length xi=9.1 nm, penetration depth lambda=194 nm, and Ginzburg-Landau parameter kappa=21. The material resembles other boride superconductors from the investigated points of view. (C) 2004 American Institute of Physics.

AC susceptibility measurements have been performed on Bi1.7Pb0.4Sr1.5Ca2.5Cu3.6Ox (Bi-2223) samples doped with different Li-based compounds and prepared by the solid-state method. As-prepared samples and/or samples annealed in oxygen or argon, ground or unground, have been investigated in detail in order to understand the occurrence, nature and evolution of the anomalous peaks observed in chi " (T) curves versus the measuring parameters; we have detected up to four peaks instead of the usual two peaks observed in the non-doped samples. It was found that intrinsic physical-chemical properties, such as the melting temperature of the doping compound, are no less important for the final properties of the superconductor than their insertion properties into the crystal lattice of Bi-2223. Doping compounds with melting temperatures below or close to the phase formation temperature of the Bi-2223 phase can act as flux, changing the growth conditions. Intensification of some processes against others (e.g. decomposition-recovery of the BI-2223 phase, solubilization-precipitation of the secondary phases, changes in the properties of the liquid phase, etc) can lead to the formation of the Bi-2223 phase with different properties than for the non-doped superconductor. Generally, when using flux-type doping compounds, anomalous AC losses peaks are detected and the intra-granular critical current density is enhanced.

Superconductivity at about 8 K was observed in the metal-rich Li-Pd-B ternary system. Structural, microstructural, electrical, and magnetic investigations for various compositions proved that the Li2Pd3B compound, which has an antiperovskite cubic structure composed of distorted Pd6B octahedrons, is responsible for the superconductivity. This is the first observation of superconductivity in metal-rich ternary borides containing alkaline metal and Pd as a late transition metal. The compound prepared by arc melting has a high density and is relatively stable in the air. The upper critical fields H-c2(0) estimated by linear extrapolation and the Werthamer-Helfand-Hohenberg theory are 6.2 and 4.8 T, respectively.

Critical current density J(c) of Na0.35CoO2.1.3H(2)O superconductor (T-c=4.4 K) has been estimated from magnetization measurements: J(c)(1.9 K,0 T)=5x10(4) A/cm(2), J(c) (1.9 K,0.4 T)=4x10(2) A/cm(2) and J(c) (3.4 K,0 T)=10(3) A/cm(2). J(c) versus applied magnetic field H cannot be fitted, as for high-T-c superconductors (HTS), by a power law for any temperature. The temperature dependence for a given H is not of the linear type as for MgB2, but is close to quasiexponential (associated with the thermally activated flux creep) as for HTS. Irreversibility field data points H-irr versus (1-T/T-c) obey a power law with power exponent n=3.4. The irreversibility line is located below, but in vicinity of, the line for Bi-2223. Details of morphology are also presented. (C) 2004 American Institute of Physics.

Precursor powders of Ba/Zr = 1:1 chloride have been prepared by freeze drying (FD) and conventional mixing. A simple, laboratory-made apparatus for sublimation of the frozen water from the cryo-particles is presented. Both powders have the same phase formation behavior. Up to 500-600 degreesC, Zr chloride transforms into ZrO2. At high temperatures, BaCl2 starts melting and decomposing and two subsequent processes take place: (a) chlorination of the Zr atoms from the oxide and (b) formation of BaZrO3 phase, These processes depend on treatment atmosphere and reactivity of the starting powders. Freeze-dried powders with higher reactivity and/or O-2 atmosphere are suitable to obtain high content of BaZrO3 phase. In the freeze-dried powder, decomposed in O-2 atmosphere at 1190 degreesC for 20 h, 90% of BaZrO3 phase content was attained. No new phases were observed during decomposition of the freeze-dried powder. In the as-synthesized freeze-dried powder, some XRD lines remained unidentified. (C) 2003 Elsevier B.V. All rights reserved.

Superconducting whiskers of Bi-2212 have been grown by an airtight crucible method in elevated magnetic fields, up to 10 T. Growth behavior with and without application of a magnetic field, as well as the SEM detailed study of the growth defects of the whiskers allow to emphasize some aspects of the growth mechanism. The conclusion is that whiskers are growing mainly through continuous crystallization at the base-end and from the so-called 'micro-crucible' formed by the glassy or powdered substrates. The supply of cations by a vapor transfer is very probable, but is taking place to the micro-crucible reaction site rather than to the droplet, as in the classic vapor-liquid-solid (VLS) growth mechanism. Therefore, whiskers grow by a modified VLS-microcrucible mechanism (MVLS-MC). Application of magnetic fields during growth has proven to be a powerful tool to investigate and influence some processes. Observation of stoichiometric Bi(Pb)-2212, CuO and Ca2CuO3 whiskers is also reported. (C) 2004 Elsevier B.V. All rights reserved.

Bi2Sr2CaCu2Ox, whiskers have been grown by a modified airtight two-crucible method, employing radial and vertical thermal gradients resulting from the relative position of the crucibles. A heating profile with a constant heating rate applied from 842 to 846degreesC allows formation of whiskers up to 2 cm in length for a certain level of Al impurity in the glass. A cation-rich atmosphere is found to be a key intrinsic parameter. Our data confirm the importance of the thermal gradients, but this parameter is a somewhat extrinsic one and from a practical point of view should be correlated to other intrinsic parameters that influence growth atmosphere (i.e. to total and partial pressures). As-grown whiskers have composition Bi:Sr:Ca:Cu = (2.9-3.5):2:(1.7-2.05):(2.4-3.0) (normalized to SrA zero-resistance critical temperature T-c(R=0) = 76-98 K and maximum transport critical current density above J(c) = 10(4) A cm(-2) at 77 K in self-field.

(Cu, C)Ba2Ca3Cu4Ox superconductor with addition of y mol LiF has been synthesized by a high-pressure method. For the same synthesis conditions it was found that (almost) single-phase Cu, C-1234 samples can be synthesized for y(LiF) = 0-0.1 if the amount of z mol AgO oxidizer is increased linearly from Z(AgO) = 0.45 to 0.73 and for y(LiF) = 0 - 1-0.2 if ZAgO = 0.73 = constant. Transport measurements (rho(T) and room-temperature Seebeck coefficient) have shown that these samples are overdoped: LiF is an effective addition for synthesis of overdoped Cu, C-1234 with a controlled level of carriers. LiF addition continuously decreases T-c. The critical point at y(LiF) = 0.1 is discussed as the solubility limit of LiF and/or the point where the doping mechanism changes. It is proposed that the reason is the reaction of extra Li with C and O to form Li2CO3, inducing a lower concentration of C in Cu, C-1234/LiF crystals, and at the same time a possible substitution of Li not only for the Cu site but also for the Ca site, resulting in formation of a higher amount of residual Ca0.828CuO2 (for y(LiF) > 0.1). LiF induces the formation of a liquid phase and acts as a flux promoting the formation of Cu, C-12(n - 1)n with n greater than or equal to 4. LiF modifies to some degree the grain growth from a 3D to a 2D type (thinner platelike grains have been observed in the LiF added samples).

Precipitate-free thin films of multicomponent materials (e.g. superconductors) have been successfully grown (see Figure) on substrates onto whose surfaces artificial steps have been generated. The steps had widths that were equal to twice the migration length of the atomic species being deposited on the films. The resulting clean, high-quality films were due to the gathering of precipitates at the step edges, where the free energy is lowest.

Thin films of the infinite-layer compound Sr0.6Ca0.4CuO2-delta have been prepared by off-axis rf magnetron sputtering on SrTiO3 (001). For an opt mum level of oxygen vacancy superconductivity was observed (T-c onset = 42 K and T-c(rho=0) = 11 K). Structural and transport data suggesting n-type superconductivity are presented and discussed. Infinite-layer thin films of Sr0.5Ca0.4CuO2-delta, without trivalent cation doping and showing n-type superconductivity, are reported for the first time.

From DC magnetization studies in fields up to 14 T and temperatures between 20 and 100 K, we estimated the intra-and inter-grain critical current density J(c) of (Cu,C): 1234 high-T-c superconductors, in the frame of critical state models. The inter-grain J(c) was determined by comparing the magnetization loops of as-grown sample and of the ground sample. Finally, short comments on J(c) resulted from AC susceptibility measurements and of the impressive increase of intra-grain J(c) due to heavy-ion and neutron irradiation are presented. (C) 2003 Elsevier Science B.V. All rights reserved.

Thin films of (Ca1-xBax)CuO2 (x = 0-1) have been grown on (0 0 1) SrTiO3 by metal organic chemical vapor deposition. These films are potential candidates as barrier layer for SIS and/or SNS Josephson junctions. For this purpose, the films should be flat and smooth. In this regard we have investigated the possibility of decreasing the films roughness by the control of the Ba/Ca ratio, the substrate temperature and oxygen partial pressure during the growth of the film. The minimum mean square root roughness and regular morphology are obtained for the x = 0.3-0.5. In the samples with x = 0.5 the highest intensity of the X-ray diffraction peaks for the (Ca0.5Ba0.5)CuO2 phase and the lowest for the impurity phases were attained at a substrate temperature of 750-780 degreesC and oxygen partial pressure of 15 Torr. (C) 2002 Published by Elsevier Science B.V.

TlBa(2)Ca(2)Cu(3)O(y) (Tl-1223) superconducting films were prepared under identical conditions, on MgO substrates with different morphologies resulting from heat treatments at temperatures between 600 and 1350 degreesC. The superconducting films have almost the same morphology, in-plane alignment and composition, but different critical current densities J(c). Critical current density J(c) determined at 77.3 K differs for films with various annealed MgO substrates, by a factor of 5 in zero field and 10 in 1 T. The behavior of J(c) is discussed in relation with the flatness of the MgO surface, and with pinning effects induced by the Ca-segregates. For the present work, the best films were obtained for the un-annealed (as-received) substrates and for substrates treated at 1350 degreesC. In these samples, the substrate's flatness and morphology with regular steps are essential for high quality of the superconducting films. In the films grown on MgO annealed between 800 and 1200 degreesC and showing rough surface and Ca-segregates, J(c) was lower. However, J(c) was increasing with heat treatment temperature of the substrate, possibly due to the Ca-segregates inducing or acting as pinning centers. The effects of Ca-segregates are of interest for maximization of the quality of the high-temperature superconducting films. In the literature, up to now, these effects have not been considered and therefore Ca-segregates removal has been recommended. (C) 2002 Elsevier Science B.V. All rights reserved.

Superconducting (0 0 1) thin films of SmBa2Cu3Oy have been grown by MOCVD on (0 0 1) SrTiO3 and (0 0 1) LaAlO3 substrates. The films on both substrates are smooth with RMS of 1.428 and 1.037 nm respectively, but have different morphology (revealed by atomic force microscopy) for the same synthesis conditions. The films grown on SrTiO3 have shown rectangular- or square-type terraces. The height between the neighboring terraces was corresponding to the c-axis length of one unit dell. This type of morphology is due to the two-dimensional nucleation and growth mechanism. In the case of the films on the LaAlO3 the surface morphology consisted of irregular grains (close to spherical). For both situations we have not found any evidence for a spiral growth mechanism. Therefore, our films are suitable for electronics applications of integrate type and not only. The as-grown films were oxygen deficient and due to this exhibited rather poor superconducting properties. Oxygen annealing at temperatures of 500-600 degreesC increased T-c(R=0) up to 87.8 K. (C) 2002 Published by Elsevier Science B.V.

Superconducting YBCO c-axis oriented thin films have been grown by MOMBE (metalorganic molecular-beam-epitaxy). Growth of the films on different substrates (100) (Y, Nd)AlO3, (100) SrTiO3 and (100) MgO has been investigated by, in situ monitoring the reflection high energy electron diffraction (RHEED). The paper discusses our results suggesting significant differences in films growth on the three presented substrates. The highest quality (high uniformity, epitaxy and low roughness) has been attained for the films prepared on SrTiO3. All films, regardless substrates, have shown values between 81 and 84 K for zero resistance critical temperature T-c0.

Thin films of infinite-layer compound Sr1-xCaxCuO2-delta have been prepared by rf magnetron sputtering. For an optimum level of oxygen vacancy superconductivities were observed (T-c (onset) = 42 and 50 K, T-c(rho=0) = 11 and 20 K). Structural and transport data suggest that the doping mechanism is electron-type. The superconducting transitions were also confirmed by ac susceptibility. Further increase of doping showed to destroy superconductivity. (C) 2003 Elsevier Science B.V. All rights reserved.

Films of (119) Bi-2223 high-T-c superconductor, potentially useful for future sandwich-stacked structures exhibiting Josephson effect have been prepared by MOCVD on (100) NdGaO3 and (110) SrTiO3 flat and vicinal substrates with different off-angles. It is shown that off-angle is a key parameter in growth control mechanism of the films. In-plane aligned films, with regular morphology and low roughness as well as having maximum zero-resistivity critical temperature: of T-c0=67.2K and T-c0=74K when "single" and "two"-temperature growth routes are used, respectively, have been obtained for high of-angles (20 degrees). Growth mechanism is changing from a two-dimensional type for the flat substrate to a step-flow one for vicinal substrates.

Orientation control of high T-c superconductors is essential for superior device performance, because the coherence length is longer along the non c-axis directions than along c-axis direction. In this study, we report on the first successful preparation of (119) oriented Bi-2223 films by MOCVD using (100) NdGaO3 Substrates. Atomic force microscopy observations of the (119) Bi-2223 films are also reported. Our films have an in-plane aligned mountain-range-shaped surface morphology. This morphology is resulting from the epitaxial relationship between the (119) Bi-2223 film and (100) NdGaO3 substrate. Films exhibited a large in-plane anisotropy as revealed by, resistivity measurements and surface morphology observations.

TlBa2Ca2Cu3Oy (Tl-1223) superconducting films were prepared under identical conditions, on MgO substrates with different morphologies resulting from heat treatments at temperatures between 600 and 1350 degreesC. The superconducting films have almost the same morphology, in-plane alignment and composition, but different critical current densities J(c). Critical current density J(c) determined at 77.3 K differs for films with various annealed MgO substrates, by a factor of 5 in zero field and 10 in 1 T. The behavior of J(c) is discussed in relation with the flatness of the MgO surface, and with pinning effects induced by the Ca-segregates. For the present work, the best films were obtained for the un-annealed (as-received) substrates and for substrates treated at 1350 degreesC. In these samples, the substrate's flatness and morphology with regular steps are essential for high quality of the superconducting films. In the films grown on MgO annealed between 800 and 1200 degreesC and showing rough surface and Ca-segregates, J(c) was lower. However, J(c) was increasing with heat treatment temperature of the substrate, possibly due to the Ca-segregates inducing or acting as pinning centers. The effects of Ca-segregates are of interest for maximization of the quality of the high-temperature superconducting films. In the literature, up to now, these effects have not been considered and therefore Ca-segregates removal has been recommended. (C) 2002 Elsevier Science B.V. All rights reserved.

By very short time rf sputtering in certain deposition conditions we have grown three-dimensional Ag nanodots on the substrate prior to the growth of TI-based superconducting films. These nanodots create pinning centers, leading to an increase in the critical current density about 10 times. From the frequency dependence of the critical current density we estimated also the, actiation energy for the flux jumps, which resulted to. be several times higher. The rate of the thermally-activated flux jumps decreases several orders of magnitude. We suggest that our method can be used for the reduction of thermal noise in high-T-c dc SQUID's.

Application of active technology factors (for example, the introduction of Bi2Sr2Ca2CU3Oy, (2223) phase additive) and corresponding optimization of synthesis parameters of Bi(Pb)-Sr-Ca-Cu-O (BSCCO) ceramics have allowed reducing the time of oxide precursor sintering from 250 to 25 h. Conditions of positive influence of 2223 phase additives have been investigated. Intensification of BSCCO ceramics synthesis was the basic purpose, but the authors have deliberately conducted broader examinations of the influence of technological parameters on the properties and structure of this material. The complex of the obtained effects (similarly to the solution of an equation set with several unknowns) helps increasing the probability of exact comprehension of the system: technology-processes occurring under ceramics synthesis-phase composition and structure-properties of BSCCO. (C) 2002 Elsevier Science B.V. All rights reserved.

Ag2O-doped (1.2% wt.) nitrate freeze-dried powders (Bi : Pb : Sr : Ca : Cu = 1.7 : 0.3 : 2 : 2.5 : 3.5) were processed under an external electrical field and 17.5 MPa pressure at 800 degreesC, for 4 min in vacuum. Final heat treatments (HT) were applied at 835 - 850 degreesC for 70 h. in air (Bi, Pb)(2)Sr2CaCu2Ox (2212-phase) was formed by electrical field processing in just 4 min. Electrical field application enhanced (Bi, Pb)(2)Sr2Ca2Cu3Oy (2223-phase) formation during final HT. Ag2O additions to field sintered BSCCO ceramics increased the amount of 2223-phase and the zero resistance critical temperature (T-e(R=0)) by similar to 4 k.

In high temperature superconductors (HTS) the coherence length along non-c-axis directions is longer. This feature can be useful when designing electronics devices based on HTS. Therefore, growth and characterization of non-c-axis oriented thin HTS films is of great interest. In this paper we present our comparative results on preparation by MOCVD and characterization by atomic force microscopy, X-ray diffraction and transport measurements of as-grown (119) Bi-2223 and (103) Y-123 thin films on (110) SrTiO3. The films have shown the same type of surface morphology (grains with mountain-range shape, aligned in parallel chains to the [001] substrate's azimuth). This morphology is the result of the orientation relationship between the (119) Bi-2223 or (10 3) Y-123 and (110) SrTiO3. The transport measurements with temperature revealed strong anisotropy of the films in the normal state region when the measuring current has been applied in-plane, parallel and perpendicular to the edges (from the basal plane) of the mountain-range grains. Higher values for T-c0 have been obtained for the Y-123 films (42 K) than for the Bi-2223 ones (31 K). The both films are as-grown and non-oxygenated ones. (C) 2002 Published by Elsevier Science B.V.

Samples of (Cu0.6C0.4)Ba2Ca3Cu4Oy ((Cu,C)-1234) with addition of 0.1 mol LiF have been synthesized by high pressure technique. It was found that LiF promotes' the formation of superconducting phases with n higher than 4 of the (Cu,C)Ba2Can-1CunOy series. In order to obtain single-phase samples, for the same synthesis conditions, the oxygen content in the starting mixture (supplied by AgO) should be increased from 0.45 to 0.73 mol AgO, when using LiF. Samples with LiF have shown a certain morphology suggesting an enhanced 2D and suppressed 3D type of growth assisted by a liquid phase. T-c decreased from 116.5 to 113 K for the sample with LiF, but at the same time the transition width also decreased and J(c) has shown a fish-tail effect. (C) 2003 Elsevier Science B.V. All rights reserved.

The paper presents a review of our data and the current status on synthesis and processing of Bi-2223 superconducting ceramic, by spray frozen, freeze drying method (SF-FD). By this method powders of 200-300 nm were obtained and processed by several different routes to the final superconducting product. Optimization process and comparative analysis with the literature data revealed intrinsic problems associated to the specific nature (i.e high degree of mixing and large surface area relative to the volume) of the SF-FD material. The paper focuses on the effects induced by the specific features of the SF-FD material, sometimes opposite to those observed in the conventional materials produced by solid-state method. It resulted that in order to take full advantage of the specific features for a nano SF-FD material, it is necessary to consider a special, non-conventional, processing approach and some examples in this regard will be presented.

From ac susceptibility measurements of the [Bi(Pb)](2)Ca2Sr2Cu3Oz (Bi-2223) samples doped with LiCl, we have found and report for the first time anomalously suppressed superconductivity (T, is anomalously decreasing) in the slightly under-doped region. For our BPSCCO/(LiCl)(y) samples this region is situated around y = 0.07. Hole concentration (p) per number of Cu-O planes of the Bi-2223 unit cell, determined from room temperature thermopower (S-300 K) measurements, is approximately 0.15 when y is within anomalous region. Literature data shows that for the La-based cuprates, similar suppression of superconductivity was observed at p similar to 0.12 (so-called "1/8 problem"). This discrepancy would appear because charge ordering phenomenon (probably induced by Li known as a pair breaker as e.g. Zn) may be accompanied by changes in oxygen content or oxygen ordering effects. (C) 2003 Elsevier B.V. All rights reserved.

In high temperature superconductors (HTS) the coherence length along non-c axis directions is longer. This feature can be useful when designing electronics devices based on HTS. Therefore growth and characterization of non-c axis oriented thin HTS films is of great interest. In this paper we present a short review of our data regarding (119) Bi-2223 thin films grown by MOCVD on (100) NdGaO3 and (110) SrTiO3. The emphasis is made on improvement and control of the quality of the films by the "two-temperature" technological approach and/or use of the vicinal substrates. Phase and morphology evolution for different processing conditions, substrate's type and off-angle are presented. The highest critical temperatures of T-c0=67.2 K and T-c0=74 K for the "single-" and "two-" temperature routes were obtained on vicinal SrTiO3 with the off-angle of 20degrees. A higher off-angle promoted the formation of a specific step-like morphology with lower roughness. For the films grown on flat substrates the morphology was of mountain-range shape. Surface morphology as a result of two types of growth mechanisms (two-dimensional (2D), assisted by a so-called "twin"-growth and step-flow growth) for the (119) Bi-2223 films are discussed.

We report the growth of TlBa2Ca2Cu3Oy superconducting thin film on CeO2 buffered r-cut sapphire substrate by amorphous phase epitaxy method, wherein an amorphous phase of a composition, TlBa2Ca3Cu4Oy was deposited by rf magnetron sputtering and subsequently crystallized by annealing at high temperatures in a closed system. There exists an optimum thickness of about 200 Angstrom of CeO2 buffer layer that gives a smooth buffer layer surface. At the temperature around 840 degreesC we get only Tl-2212 phase and for a longer annealing time it results in Tl-1212 phase. At higher temperatures Ba reacts with Ce to form BaCeO3. To avoid this reaction process we introduced another amorphous buffer layer, TlSr2CaCu2Oy onto CeO2 layer. By this method we could prepare a good quality TI-1223 thin film which showed a T-c of 104 K and a J(c) = 0.3 MA/cm(2) at 77 K and 0.1 T field. (C) 2002 Elsevier Science B.V. All rights reserved.

Superconducting samples with a starting composition Cu0.5TlxBa2Ca3Cu4O12 (x = 1-0.35) were prepared in Au tubes from oxides by using different heating rates. The optimum heating rate was 0.11 degreesC min(-1) applied between 860 and 880 degreesC. These samples show the highest content of 1234 phase and the lowest of Ba-Cu-O phases as well as the highest critical temperatures. The highest values were T-c = 119.2 K and T-c0 = 115.1 K. All samples show J(c) values around 6 x 10(5) A cm(-2), at 60 K and 0.5 T. In the rest of the samples, heated by using lower or higher heating rates, a high concentration of 1223 and/or 1245 phases is detected. The content of the 1234 phase and of Ba(Ca.Tl)-Cu-O residual liquid phase, in the samples synthesized for the optimum heating rate, depends on the Tl content in the starting mixture. The influence of the oxygen content in the starting mixture on phase composition is not as strong as of Tl, but it has a major role in establishing the superconducting behaviour of the 1234 grains. Some arguments that suggest the dependence of the transport properties of the non-superconducting matrix on oxygen content will be discussed. In our technological arrangement the determined optimum heating rate can be applied to the synthesis of other single-layered superconducting phases, e.g. 1212 phase from a Cu0.25Tl0.75Ba2CaCu2O8.115 starting composition.

The reactive-field-assisted-sintering technique (RFAST) has been applied to freeze-dried decomposed precursor powders with a starting cation composition of Bi:Pb:Sr:Ca:Cu = 1.7:0.3:2.0:2.5:3.5. A short time (< 15 min) RFAST treatment at 800-900degreesC did not lead to the formation of Bi2Sr2Ca2Cu3O10+x, (2223-phase). But RFAST was favourable to Bi2Sr2CaCu2O8+y, (2212-phase) formation particularly in samples with a low content of the 2212-phase in the precursor powder. Heat treatment (HT) after RFAST showed that the 2223 phase could form more rapidly than in freeze-dried pressed and sintered pellets produced by the traditional technique. The resultant ceramics after 70 h of annealing contain 75% 2223-phase and have T-c(R=0) = 100.7 K, T-c = 109.5 K and DeltaT(c) = 22.4 K.

Thermal decomposition processes in mixtures of Ca : Cu = 1 : 1 nitrate powders produced by a conventional technique and by freeze drying method have been investigated by thermal analysis and X-ray diffraction. Results have been compared with literature values and data obtained by our investigations of individual calcium and copper nitrates. Temperatures at which decomposition processes occur change with by +/-30degreesC and depend also on the level of mixing of the nitrates. An exemption is the temperature for CuO phase formation, which was determined for the Cu-nitrate and for both 1 : 1-nitrate powders to be at 266degreesC. The domains of stability for different phases are shown to be variable. Also, for 1 : 1-powders, alpha-type and beta-type Ca(NO3)(2) . 2H(2)O phases coexist, while in Ca-nitrate only the alpha-type phase was observed. (C) 2002 Kluwer Academic Publishers.

Superconducting samples have been synthesized from starting compositions CU0.5TlxBa2Ca3Cu4O12+y, x(Tl) = 0.35-1 in the sealed Au-tubes. Starting oxygen content was y = 0 and/or y = +/-0.225. Samples contain non-superconducting phases and only one main superconducting phase, 1234. The energy dispersive spectroscopy grain composition was Tl0.87-1.3Ba1.9-2.05Ca2.55-3.1Cu4Ox (normalized to Cu = 4). The starting Tl and oxygen content do not influence the occurrence of the phases, grain size, morphology and composition. On the other hand the phase content strongly depends on Tl content and almost does not depend on oxygen content. Both Tl and oxygen content are important for the transport properties of the superconducting grains and it seems that also of the non-superconducting matrix. T-c of the samples was in the range 119.1-111.3 K. (C) 2002 Elsevier Science B.V. All rights reserved.

Temperature and time dependence of the phase formation in the (Cu-0.5,Tl-0.5)-1234 composition have been studied. The liquid-vapour deposition mechanism for the formation of 12(n - 1)n superconducting phases is presented. XRD, SEM, EDS and weight loss data are discussed. Samples were superconducting with maximum T-c and J(c) (at 60 K and 0.5 T), determined from M(H) loops of 118 K and 4 x 10(5) A cm(-2), respectively.

From frequency-dependent ac susceptibility studies of (Cu,T1)BaSrCa2Cu3Oy superconducting thin films, with and without nanodot-induced artificial pinning centers, we estimated the activation energy of flux jumps. The result was that, in the film with nanodots, the pinning potential is several times higher, leading to a probability of thermally activated flux jumps several orders of magnitude lower than in the film without artificial pinning centers. We suggest that our no cost straightforward method for creating extended defects can be successfully employed for the reduction of thermal noise in superconducting electronic devices. (C) 2002 American Institute of Physics.

Thin films of Cum-1Bam(Sr,Ca)(n)Cun+1O2m+2n+1, i.e., [BaCuO2](m)/[(Sr,Ca)CuO2](n) superlattices have been grown by layer-by-layer growth method with rf magnetron sputtering on NdGaO3(1 1 0) substrate. Two targets with the compositions BaCuO2 and (Sr,Ca)CuO2, which form the charge reservoir and superconducting layers, respectively, were used. [BaCuO2](m)/[(Sr,Ca)CuO2](n) superlattice was grown at 460-520 degreesC in a gas mixture of Ar and N2O by alternatively depositing the charge reservoir layer and superconducting layer. The superlattice modulation is close to that of high pressure synthesized bulk materials. By means of the layer-by-layer growth method, a system of Cu-based artificial lattice structures is formed. Electrical transport properties of these superlattices were also investigated. (C) 2002 Elsevier Science B.V. All rights reserved.

A slice of the (Cu,C)Ba2Ca3Cu4O12-y bulk superconductor grown by high-pressure synthesis was polished down to a thickness of 50 mum, and then irradiated with high-energy (240 MeV) Au15+, ions (10 11 cm(-2)). Since the length of the ion tracks was estimated to be 12.2 mum, our sample consists of two different types of grain, with and without columnar defects, having very different critical current densities. Using the third-harmonic response of the sample, we were able to separate the small dissipation in the irradiated grains from the much larger dissipation in the non-irradiated grains, in a certain experimental range of temperature, field and current density. The critical current density was estimated from critical state models. For temperatures in the range of 85-105 K, we observed a peak effect at high dc magnetic fields, suggesting the possibility of a record irreversibility field at 77.3 K.

Spray frozen, freeze dried nitrate powder with composition Bi:Pb:Sr:Ca:Cu 1.7:0.3:2.0:2.5:3.5 has been thermally decomposed (up to 870 degreesC). In situ neutron diffraction investigations during heating and cooling of the powder have been performed at DN2 instrument from the IBR2 reactor at JINR, Dubna, Russia. Phase formation and reformation and domains of stability for different phases were observed and discussed.

The Ca0.45CU0.55O phase was successfully produced from a mixture of Ca and Cu nitrate powders with cation ratio Ca:Cu = 1:1. The heat treatment for decomposition and the synthesis of the indicated phase were pet-formed at 710 degrees C in air and flowing oxygen, respectively. The Ca0.45Cu0.55O phase concentration increases with synthesis time. After 209 h of heat treatment, the concentration of the Ca0.45Cu0.55O phase determined by X-ray diffraction (XRD) analysis has reached 87% and the kinetic data have indicated that the material enters the saturation stage of the reaction, The secondary phases are CaO and CuO. (C) 2000 Elsevier Science B.V. All rights reserved.

Nitrate powder with cation composition Bi:Pb:Sr:Ba:Ca:Cu= 1.8:0,4:1.8:0.2:2.2:3.0, the precursor powder for synthesis of Bi-2223 superconducting phase, was obtained by spray-frozen, freeze drying technique. Samples of the nitrate precursor powder were placed in a heated furnace and extracted in air when temperature of the powder has attained values of 640, 660, 710, 750, 760, 778, 790, 815 and 850 degrees C. Samples have been investigated by X-ray diffraction analysis. The obtained data allow us to propose and discuss phase formation and decomposition processes and reactions that occur in non-isothermal conditions at different temperatures during thermal decomposition of the nitrate powder.

In a freeze-dried nitrate precursor powder with cation composition Bi:Pb:Sr:Ca:Cu = 1.7:0.3:2.0:2.5:3.5, Sc2O3 was added. The stoichiometry for the mixed precursor powder was Bi:Pb:Sr:Sc:Ca:Cu = 1.7:0.3:2.0:0.25:2.5:3.5. The two nitrate precursor powders with and without Sc were thermally decomposed, pressed, and sintered in the same conditions. They show different behavior, as revealed by thermal analysis. X-ray diffraction (XRD), Scanning electron microscopy (SEM), and chi'(T) measurements. Addition of Sc slows down synthesis processes, including 2223-phase during reactive sintering. After 70 h of sintering, 43% of 2223-phase formed in the pellet with Sc, whereas in the Sc-free pellet, 51% of the 2223-phase was attained. Moreover, addition of Sc leads to a certain morphology, resulting in lower superconducting characteristics.

One step synthesis of the superconducting Bi(Pb)-2223 phase during heat treatment for non-equilibrium decomposition of the freeze dried Bi:Pb:Sr:Ba:Ca:Cu = 1.8.0.4: 1.8:0.2:2.2:3.0 nitrate powder has been studied. The heating rate was similar to 100 degrees C min(-1) and samples were maintained in air at 848 degrees C for 0, 5, 10, 20, 30, 60, 90, 240 and 1080 min. Each batch was investigated by x-ray diffraction analysis and ac magnetic susceptibility chi'(T). Evolution of phases and kinetics of phase formarion-decomposition processes were discussed. similar to 80% of Bi(Pb)-2223 has formed indicating the possibility of lowering the processing time of the freeze dried precursor powders by one order of magnitude comparative to the multistep synthesis route (from hundreds to tens of hours). A 30 min heat treatment step at 840 degrees C performed on the way up to the synthesis temperature is a forthcoming operation in order to block the formation of secondary undesired phases (e.g. (Ca1-xSrx)(14)Cu24O41).

Nitrate powder with cation composition Bi:Pb:Sr:Ba:Ca:Cu = 1.8: 0.4:1.8:0.2:1.2:2.0 was obtained by spray-frozen, freeze-drying technique. Samples of the nitrate precursor powder were placed in a heated furnace (heating rate similar to 100 degrees C/min) and extracted in air when temperature of the powdered samples attained values of 439, 495, 550, 600, 640, 647, 717, 766, 814, and 850 degrees C. Samples have been investigated by X-ray diffraction analysis. The obtained data allow us to propose and discuss phase formation and decomposition processes and reactions that occur in non-isothermal conditions at different temperatures during thermal decomposition of the nitrate powder.

Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) have been used to evidence the occurrence, morphology and microcomposition of the superconducting phases (Bi,Pb)(2)Sr2Ca2Cu3O10+delta (2223) and (Bi,Pb)(2)Sr2CaCu2O8+delta (2212), and of other non-superconducting phases, in the sintered pellets obtained from nitrate solution by spray frozen, freeze drying technique. For decomposition of the nitrate powder four different heat treatments were used. Superconducting and structure properties of the pellets have been tested by AC susceptibility measurements (610 Hz, 0.5 Oe) and X-ray diffraction analysis, respectively. A correlation between the SEM and EDS observations and the superconducting properties has been established. (C) 1997 Elsevier Science B.V.

Superconducting samples of the Bi(Pb)-Sr-Ca-Cu-O system have been irradiated in transmission electron microscopy (TEM) to investigate the effect of a relative high fluence of electrons with 75 and 100 keV energy on the microstructure of the material. The diffraction pattern images show a dramatic change from very uniform lattice spots at ab crystalline planes to a circular pattern corresponding to damage and breaking of the materials in very small crystallites.

The effect of intermediate grounding and sintering environment (air or sintered powder) on the superconducting characteristics of Bi(Pb)-Sr-Ca-Cu-O hulk ceramics obtained by spray-frozen freeze drying technique was investigated by X-ray diffraction, electric and magnetic measurements. Intermediate grounding leads to higher scattering coefficients of the superconducting characteristics. This result does not depend on sintering environment. Improved results are obtained when sintering is performed by immersing pellets "in powder" rather than placing them "on powder". The powder used as sintering environment was pyrolized precursor powder calcinated in air for 100 h. (C) 1998 Elsevier Science Ltd. All rights reserved.

Bi-Pb-Sr-Ca-Cu-O samples were produced by the spray-frozen, vacuum-freeze drying method from nitrate solutions. Structural modifications of crystallites during sintering were investigated in agreement with bulk density, phase structure of the samples, critical temperature T-c and critical current density j(c). A model for morphology changes of (2223) crystallites during sintering was proposed. Maximum j(c) in a zero magnetic field is reached on samples sintered for 200-250 h.

The effect of annealing duration in oxygen flow on the superconducting characteristics of YBa2Cu3Osimilar to 7 bulk ceramics was investigated by structural, electrical, magnetic, and electronic microscopy investigations. The long-time annealing is deleterious for the superconductivity in YBa2Cu3Osimilar to 7 ceramics. The optimum time interval for annealing is from 20 to 70 h at 950 degrees C, and within this range the maximum value of T-c is obtained.

The chemical precipitation was used to obtain carbon fibers (CF) with surface modified by magnetite particles (Fe3O4). Processing was carried out by employing up to three subsequent coating stages of ultrasonic treatments. After each sonication stage, the coating was 17, 33, and 47 wt. % of the total weight of the modified fibers. Raman spectroscopy indicates the presence in the coating of a mixture of iron II and III states. As-decorated fibers were used to fabricate composites with an epoxy resin (ED-20) matrix cured with PEPA. The quantity of the carbon fiber filler was of 1, 3, and 6 wt %. At room temperature, the saturation magnetization of the soft magnetic samples was 0.37, 0.83, and 1.72 emu/g for the indicated compositions. Carbon fiber reinforced polymer materials with extra functions such as magnetic in this case, are expected to be useful in applications from the power and energy industries.

The chemical precipitation was used to obtain carbon fibers (CF) with surface modified by magnetite particles (Fe3O4). Processing was carried out by employing up to three subsequent coating stages of ultrasonic treatments. After each sonication stage, the coating was 17, 33, and 47 wt. % of the total weight of the modified fibers. Raman spectroscopy indicates the presence in the coating of a mixture of iron II and III states. As-decorated fibers were used to fabricate composites with an epoxy resin (ED-20) matrix cured with PEPA. The quantity of the carbon fiber filler was of 1, 3, and 6 wt %. At room temperature, the saturation magnetization of the soft magnetic samples was 0.37, 0.83, and 1.72 emu/g for the indicated compositions. Carbon fiber reinforced polymer materials with extra functions such as magnetic in this case, are expected to be useful in applications from the power and energy industries.

Almost six decades ago, in Romania a small group of physicists begun to study chalcogenide compositions, motivated primarily by the desire to understand the phase-change phenomenon in these materials, discovered recently, at that time, by Stanford R. Ovshinsky. It took not too long for them to realize the challenges these materials set to the research. With newcomers to the field, the research was broadened. In some cases just for basic research, to model, and to understand the chalcogenide materials, whereas in other cases, the applicative potential was revealed and used. Herein, the evolution of the field of these somewhat exotic materials is followed, listing the main contributions done in Romania, both in basic and applied research.