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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.

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.

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.

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 (Hirr) at temperatures below 25 K when compared to a pristine sample. More efficient is In-acac addition and it promotes a Hirr of ∼12.4 T (100 A/cm2 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.

International audience; 3D printing or additive manufacturing is a technology that has drastically developed in recent years for numerous industrial applications. Among the 3D printing methods the fused deposition modeling (requires filaments to generate a three dimensional objects. Currently, the polymers used in this technology are synthetic ones, derived from non renewable resources such as petroleum. Green polymers (including natural polymers) are a sustainable alternative of them as they are biodegradable/recyclable, non toxic and abundant. However the implementation in 3D printing of the major part of them remains a challenge. This chapter is focused on the most famous and promising biodegradable polymers from biomass, produced by microorganisms or derived from biotechnology for applications using fused deposition modeling. Their thermal, rheological and mechanical properties are also discussed in details.

Pure and Er-doped hematite (α-Fe2O3) nanorods were prepared by a two-step method involving hydrothermal synthesis and calcination of pure and Er-doped goethite (α-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 Mössbauer spectroscopy.

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 102 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 ⩾ 104 occurs near the close extremity of the shield to over 1 T.

Zr

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.

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 µg/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.

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 En 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.

Boron carbide added with 0–20 wt% carbon fibers was subject to Si infiltration. Samples mainly consist of B13C2, β-SiC and unreacted Si. Some amount of SiB6 and α-SiC was also detected, while formation of B12(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 μm thickness), Dextro-Levo-lactic acid (DL-PLA, 1.3 μm) or poly methyl methacrylate polymer (PMMA, 1.7 μm) 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 RZJIS 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. Keywords: NiTi alloy, Coating of TiO2, SiO2, ZrO2, DL-PLG, DL-PLA, PMMA, Roughness, In vivo test

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 ∼3 wt % and for H2 outer flow rate of ∼35 L/min. These two parameters show the strongest influence on the bubble-free growth, but other growth parameters (H2 inner flow rate, O2 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.

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.

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.

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.

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 MgB2(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 ~ 560 and ~ 740 °C. A third drop, which is sometimes not well resolved being part of the second peak at 740 °C, occurs at ~ 820 °C. The critical temperature at the midpoint of the transition, Tc, 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 T at 12 K, 5.20 and 3.98 T at 20 K and 2.39, and 1.96 T at 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.

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.

International audience; When the MgB2 bulk body is magnetized by the pulse magnetizing method, the MgB2 bulk can take the role of a pseudo permanent magnet. However, it was confirmed that the temperature at which MgB2 is expected to be used is close to the critical temperature (TC) of MgB2 and the specific heat is small, so that the heat generated by the pulse magnetizing method causes flux jump and the trapped magnetic field performance deteriorates. In this study, pulse magnetizing was performed on different samples to verify and consider changes in the trapped magnetic field performance. As the sample, the sample obtained by changing the amount of titanium added was synthesized by uniaxial hot pressing and the sample synthesized by spark plasma sintering (SPS). Figure (a) shows a comparison of the trapped magnetic fields of the samples synthesized by the uniaxial hot press. From Fig. (A), it was shown that the capture magnetic field performance may be improved or deteriorated by the composition ratio of the material, the addition of impurities, and the method of synthesizing the bulk material.

Mixtures of B4C, α-AlB12 and B powders were reactively spark plasma sintered at 1800 °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/α-AlB12 ≥ 1.3 for a constant B-amount, the major phase in the samples was the orthorhombic AlB24C4, and when R 24C4 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 B12-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.

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 δ, 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 KIC 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.

Four Ge-based organometallic (OM = C 6 H 10 Ge 2 O 7 ) polymers with similar chemical composition were used as additions for MgB 2 . MgB 2 (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, Fp max . There is no significant Ge substitution in the crystal lattice of MgB 2 , 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 MgB 2 powder shows also some drawbacks in mixing and sintering.

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.

Green compacts of B 4 C or B 4 C 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 B 4 C-based ceramic is obtained. It contains free-Si, SiC and B 4 C. 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 B 4 C 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 B 4 C raw powders are also important. It is recognized that sintering of powders larger than 10–20 µm is usually difficult: our approach is demonstrated to be suitable for processing of B 4 C powders with a very different particle size, from 10 to 250 µm. 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.

Samples of MgB2 with relative density above 95% were obtained by spark plasma sintering (SPS) at 1150 °C for a heating time of 100 °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 δ T c pinning.

High-density (92–98 % of the theoretical density) MgB 2 samples added with Sb 2 O 5 ((MgB 2)+ (Sb 2 O 5) 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 MgB 2 grain boundaries and they are of large size. Hence, Sb 2 O 5 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 MgB 2 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.

Thermal behavior of repa-germanium (C 6 H 10 Ge 2 O 7 , 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 °C, in air or argon. The first reversible transformation is below 220 °C and it was assigned to an isomerization process, based on DSC, XRD and IR measurements. The next five transformation domains (220–910 °C) are decompositions accompanied by weight loss. The main product of thermal decomposition is Ge. The next transformation domain (910–970 °C) corresponds to melting of Ge, both in argon and air. In the air, this step is followed by oxidation of Ge (970–1100 °C) and, finally, by melting of GeO 2 . Amorphous phases formed between 220 and 720 °C. Observed processes are discussed based on crystal chemistry and bonds dynamics considerations.

Dense samples with starting composition (MgB2)0.99(Tex(HoO1.5)y)0.01, x/y = 0/0, 0.73/027, 0.57/043, 0.4/0.6, 0.31/0.69, and 0.25/0.75 were processed by spark plasma sintering. Material is a bi-composite with a systematic microstructural change between “clean” and “dirty” MgB2 regions. The maximum self-field critical current density Jc0 and volume pinning force Fp, max are obtained for x/y = 0.4/0.66 = 0.67 where “clean” regions separate as isolated islands in a “dirty” matrix. The maximum value of Fp, max is high (9.2 GN/m3 at 5 K and 4.4 GN/m3 at 20 K). In the samples with x/y > 0.67 variation of the pinning-force-related parameters is small, while a decreasing x/y < 0.67 promotes a strong variation towards grain boundary pinning. In the curves of the pinning force vs. magnetic field, a shoulder occurs for a decreasing x/y (x/y < 0.67). Two pinning-behavior regimes can be defined, namely, below and above ∼25 K. When x/y decreases, variation of the midpoint critical temperature Tc, midpoint and of the irreversibility field Hirr is relatively small: Tc, midpoint decreases with less than 0.7 K and Hirr for the co-added samples is similar or slightly higher than for pristine one. Results enable material design with controlled properties.

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 2θ1 = 33.42° to a new created orientation at 2θ2 = 38.06° 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 Eg 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. Keywords: Indium sulfide thin films, Chemical bath deposition, High gamma irradiations, Structural, Morphological and optical properties

Thin films of (117) Bi2Sr2Ca2CuO8+&delta, (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&deg, Films are 3D epitaxial and X-ray diffraction &phi, &psi, 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&ndash, 600 &deg, C and continues at 700&ndash, 750 &deg, 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.

Pottery vessels made of kaolin clay from the Roman Period (2nd, 3rd centuries CE) found in Romula (Reșca 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.

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)0.01 were fabricated by slip casting under an H0 = 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//H0 (H=applied field). These values are higher or similar to the randomly-oriented samples with the same composition. The maximum volume pinning force (Fp) 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 Fp is proposed; for the randomly and partially-oriented samples (that show an extra peak in Fp), the single and double Gaussian functions fit well. The results suggest an anisotropic influence of carbon substituting for boron in the MgB2.