Dr. Eng. Mihai-Alexandru GRIGOROSCUTA

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.

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.

In this study, thermal analysis (including differential thermal analysis and thermogravimetric analysis coupled with mass spectrometry) was used to design the sintering process of alumina as well as Al2O3-Mo and Al2O3-Ni green bodies obtained by digital light processing (DLP) 3D printing. The measurements were performed for selected organic additives, which are commonly used in the DLP technique, such as photoinitiators, dispersing agents, and organic monomers. Additionally, metallic powders (Ni, Mo), as well as ceramic and composite green bodies, have been subjected to thermal analysis. The obtained results allowed us to determine proper sintering conditions for a two-step sintering program. Firstly, the organic phase was burnt out at 400 degrees C in the air. At this temperature, metallic powders have not yet started to oxidize, and most of the organic additives have already been eliminated from the sample. The second step was performed using spark plasma sintering at 1150 degrees C with a pressure equaling 60 MPa in an argon atmosphere to prevent the oxidation of metals. The samples were gradually cooled down to 800 degrees C at a cooling rate of 35 degrees C min-1 and then furnace-cooled to room temperature, preventing the formation of intrinsic defects (microcracks) in a multicomponent ceramic-metal composite. The XRD and SEM-EDS analysis allowed us to conclude that the obtained composites are well densified, no other phases apart from alumina and metals are present in the samples, and that the alumina grain growth is smaller than for conventional sintering. An increase in fracture toughness for the composite samples was observed compared to pure alumina.

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.

Iron oxide nanoparticles were synthesized using a vortex microfluidic system and subsequently functionalized with a primary shell of salicylic acid, recognized for its ability to increase the stability and biocompatibility of coated materials. In the second stage, the vortex platform was placed in a magnetic field to facilitate the growth and development of a porous silica shell. The selected drug for this study was micafungin, an antifungal agent well regarded for its effectiveness in combating fungal infections and identified as a priority compound by the World Health Organization (WHO). The resulting nanocomposite system was characterized using various techniques, including Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), dynamic light scattering (DLS), Brunauer-Emmett-Teller (BET) analysis, UV-Vis spectroscopy, and Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS). The synthesis method produced nanoparticles with dimensions of 5-7 nm, highlighting the advantages of the chosen approach. A desorption profile was established using a continuous-flow, UV-Vis analysis system, indicating that the bioactive compound was released slowly; after two hours, approximately 50% of the loaded micafungin was detected in the release medium. Furthermore, the results obtained from the FT-ICR MS analysis provided molecular-level confirmation, thereby supporting the release mechanism of micafungin from the nanosystem.

The paper describes the chemical modification of the graphene oxide (GO) surface with glucosamine, which was conjugated to GO via a carbodiimide-mediated amidation-type reaction. The efficiency of the reaction was confirmed by FT-IR and Raman spectroscopy and elemental analysis. The elaborated functionalization significantly reduces the agglomeration of graphene oxide platelets. The interactions at the interface of GO and two types of ceramic nanoparticles (ZrO2 and Al2O3 with particle sizes of 58 nm and 158 nm, respectively) were examined by zeta potential measurements at different pH values. The viscosity of ZrO2 suspensions (35 vol% of solid loading) at 1.5 s- 1 increases from 24.8 Pas to 170.7 Pas and 142.7 Pas with the addition of GO and f-GO, respectively. The interfaces at ceramic-graphene heterostructures obtained by slip casting method have been analyzed by SEM. The investigations revealed the presence of multilayer graphene oxide and flexible single-layer f-GO within the ceramic matrix.

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.

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.

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.

This work was devoted to the first multi-parametric unitary comparative analysis of a selection of sintered piezoceramic materials synthesised by solid-state reactions, aiming to delineate the most promising biocompatible piezoelectric material, to be further implemented into macro-porous ceramic scaffolds fabricated by 3D printing technologies. The piezoceramics under scrutiny were: KNbO3, LiNbO3, LiTaO3, BaTiO3, Zr-doped BaTiO3, and the (Ba0.85Ca0.15)(Ti0.9Zr0.1)O-3 solid solution (BCTZ). The XRD analysis revealed the high crystallinity of all sintered ceramics, while the best densification was achieved for the BaTiO3-based materials via conventional sintering. Conjunctively, BCTZ yielded the best combination of functional properties-piezoelectric response (in terms of longitudinal piezoelectric constant and planar electromechanical coupling factor) and mechanical and in vitro osteoblast cell compatibility. The selected piezoceramic was further used as a base material for the robocasting fabrication of 3D macro-porous scaffolds (porosity of similar to 50%), which yielded a promising compressive strength of similar to 20 MPa (higher than that of trabecular bone), excellent cell colonization capability, and noteworthy cytocompatibility in osteoblast cell cultures, analogous to the biological control. Thereby, good prospects for the possible development of a new generation of synthetic bone graft substitutes endowed with the piezoelectric effect as a stimulus for the enhancement of osteogenic capacity were settled.

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.

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.

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.

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 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.

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.

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.

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.

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.

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.

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)).

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.

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.