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Dr. Mihai BURDUSEL

Scientific Researcher III

1

Trapped Magnetic Field of MgB2 Machinable Disks with Different Additives

Burdusel, M; Aldica, GV; Pasuk, I; Grigoroscuta, MA; Kuncser, A; Badica, P

JUL 10 2025, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 38, 179

DOI: 10.1007/s10948-025-07002-w

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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.

2

Ex-situ spark plasma sintered MgB2 with Ge-based organometallic additions: Key ingredients for superconductivity enhancement

Batalu, D; Nakamura, T; Burdusel, M; Pasuk, I; Bezergheanu, A; Badica, P

FEB 2024, SOLID STATE SCIENCES, 148, 107429

DOI: 10.1016/j.solidstatesciences.2023.107429

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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.

3 Open Access

Microstructure and coupling mechanisms in MnBi-FeSiB nanocomposites obtained by spark plasma sintering

Alexandru-Dinu, A; Locovei, C; Bartha, C; Grigoroscuta, MA; Burdusel, M; Kuncser, A; Palade, P; Schinteie, G; Iacob, N; Lu, W; Batalu, D; Badica, P; Kuncser, V

JUL 24 2024, SCIENTIFIC REPORTS, 14, 17029

DOI: 10.1038/s41598-024-67353-7

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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.

4

Screening of magnetic fields by superconducting and hybrid shields with a circular cross-section

Gozzelino, L; Fracasso, M; Solovyov, M; Gömöry, F; Napolitano, A; Gerbaldo, R; Ghigo, G; Laviano, F; Torsello, D; Grigoroscuta, MA; Aldica, G; Burdusel, M; Badica, P

APR 1 2022, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 35, 044002

DOI: 10.1088/1361-6668/ac4ad0

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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.

5

New superdielectric materials: (1-x) SrFe12O19 - x BNT-BT nanocomposites

Greculeasa, SG; Comanescu, C; Iacob, N; Kuncser, A; Smaranda, I; Amarande, L; Cioangher, M; Burdusel, M; Teodorescu, V

OCT 1 2022, PHYSICA B-CONDENSED MATTER, 642, 414139

DOI: 10.1016/j.physb.2022.414139

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Novel (1-x) SrFe12O19 - x BNT-BT0.08 (x = 0; 0.5; 0.8; 1) nanocomposites were explored in this study. The samples were produced by sol-gel method and compacted by conventional sintering. The composition, morphology, local structure, dielectric and magnetic properties were investigated by X-ray diffraction, Transmission Electron Microscopy, Impedance Analysis, Mossbauer spectroscopy, and SQUID magnetometry. The desired composition and the presence of the magnetoplumbite SrFe12O19 and perovskite BNT-BT structures were verified by X-ray diffraction. Irregular morphology and large size distributions are evidenced in the electron microscopy micrographs. The reported room temperature dielectric constants in this study are the highest values obtained in multiferroic composites at room temperature: giant dielectric constants (similar to 1.3 x 10(6)) were obtained, relative to 0.13 x 10(4) in BNT-BT. The hyperfine parameters allowed the identification of the Wyckoff positions of the Fe ions corresponding closely to the theoretical case. The hard magnetic character of the SrFe12O19 phase is evidenced from the magnetic measurements. For the first time in multifermic composites, superdielectric characteristics are evidenced at room temperature.

6

ZnS stacking order influence on the formation of Zn-poor and Zn-rich Cu2ZnSnS4 phase

Zaki, MY; El Khouja, O; Nouneh, K; Touhami, ME; Matei, E; Azmi, S; Rusu, MI; Grigorescu, CEA; Briche, S; Boutamart, M; Badica, P; Burdusel, M; Secu, M; Pintilie, L; Galca, AC

MAY 2022, JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS, 33

DOI: 10.1007/s10854-022-08160-6

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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.

7 Open Access

Mud and burnt Roman bricks from Romula

Badica, P; Alexandru-Dinu, A; Grigoroscuta, MA; Burdusel, M; Aldica, GV; Sandu, V; Bartha, C; Polosan, S; Galatanu, A; Kuncser, V; Enculescu, M; Locovei, C; Porosnicu, I; Tiseanu, I; Ferbinteanu, M; Savulescu, I; Negru, M; Batalu, ND

SEP 23 2022, SCIENTIFIC REPORTS, 12, 15864

DOI: 10.1038/s41598-022-19427-7

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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.

8

MgB2 with Addition of Cubic BN and Ge2C6H10O7 Obtained by Spark Plasma Sintering Technique

Ionescu, AM; Aldica, G; Popa, S; Enculescu, M; Sandu, V; Pasuk, I; Burdusel, M; Grigoroscuta, MA; Miu, L; Badica, P

DEC 2022, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 35

DOI: 10.1007/s10948-022-06350-1

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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.

9

Intrinsic losses in microwave dielectrics investigated by THz-TDS: A comparison between conventional and spark plasma sintered Zr0.8Sn0.2TiO4 ceramics

Nedelcu, L; Banciu, MG; Geambasu, CD; Burdusel, M; Grigoroscuta, MA; Enculescu, M; Badica, P

2022, 2022 47TH INTERNATIONAL CONFERENCE ON INFRARED, MILLIMETER AND TERAHERTZ WAVES (IRMMW-THZ 2022)

DOI: 10.1109/IRMMW-THz50927.2022.9895934

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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.

10

Effect of polysilane addition on spark plasma sintering and superconducting properties of MgB2 bulks

Sandu, V; Aldica, G; Grigoroscuta, MA; Burdusel, M; Pasuk, ; Ching, YC; Ionescu, AM; Badica, P

NOV 1 2022, CERAMICS INTERNATIONAL, 48

DOI: 10.1016/j.ceramint.2022.07.127

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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.

11 Open Access

Microwave and Terahertz Properties of Spark-Plasma-Sintered Zr0.8Sn0.2TiO4 Ceramics

Nedelcu, L; Burdusel, M; Grigoroscuta, MA; Geambasu, CD; Enculescu, M; Badica, P; Banciu, MG

FEB 2022, MATERIALS, 15, 1258

DOI: 10.3390/ma15031258

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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).

12 Open Access

MgB2-based biodegradable materials for orthopedic implants br

Badica, P; Batalu, ND; Balint, E; Tudor, N; Barbuceanu, F; Peteoaca, A; Micsa, C; Eremia, AD; Trancau, OI; Burdusel, M; Grigoroscuta, MA; Aldica, GV; Radu, D; Porosnicu, I; Tiseanu, I

SEP-OCT 2022, JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY-JMR&T, 20

DOI: 10.1016/j.jmrt.2022.07.164

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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/).

13 Open Access

New Chalcogenide Glass-Ceramics Based on Ge-Zn-Se for IR Applications

Velea, A; Sava, F; Badica, P; Burdusel, M; Mihai, C; Galca, AC; Matei, E; Buruiana, AT; El Khouja, O; Calvez, L

JUL 2022, MATERIALS, 15, 5002

DOI: 10.3390/ma15145002

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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.

14 Open Access

Towards high degree of c-axis orientation in MgB2 bulks

Grigoroscuta, MA; Aldica, G; Burdusel, M; Sandu, ; Kuncser, A; Pasuk, ; Ionescu, AM; Suzuki, TS; Vasylkiv, O; Badica, P

AUG 2022, JOURNAL OF MAGNESIUM AND ALLOYS, 10

DOI: 10.1016/j.jma.2021.10.013

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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

15 Open Access

Antimicrobial Activity of MgB2 Powders Produced via Reactive Liquid Infiltration Method

Padhi, SK; Baglieri, N; Bonino, V; Agostino, A; Operti, L; Batalu, ND; Chifiriuc, MC; Popa, M; Burdusel, M; Grigoroscuta, MA; Aldica, GV; Radu, D; Badica, P; Truccato, M

AUG 2021, MOLECULES, 26, 4966

DOI: 10.3390/molecules26164966

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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.

16 Open Access

MgB2 powders and bioevaluation of their interaction with planktonic microbes, biofilms, and tumor cells

Badica, P; Batalu, ND; Chifiriuc, MC; Burdusel, M; Grigoroscuta, MA; Aldica, G; Pasuk, I; Kuncser, A; Enculescu, M; Popa, M; Marutescu, LG; Gheorghe, I; Thamer, O; Bleotu, C; Pircalabioru, GG; Operti, L; Bonino, V; Agostino, A; Truccato, M

MAY-JUN 2021, JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY-JMR&T, 12

DOI: 10.1016/j.jmrt.2021.04.003

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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.

17 Open Access

In Vitro Evaluation of MgB2 Powders as Novel Tools to Fight Fungal Biodeterioration of Heritage Buildings and Objects

Gheorghe, I; Avram, I; Corbu, VM; Marutescu, L; Popa, M; Balotescu, I; Blajan, I; Mateescu, V; Zaharia, D; Dumbrava, AS; Zetu, OE; Pecete, I; Cristea, VC; Batalu, D; Grigoroscuta, MA; Burdusel, M; Aldica, GV; Badica, P; Datcu, AD; Ianovici, N; Bleotu, C; Lazar, V; Ditu, LM; Chifiriuc, MC

JAN 13 2021, FRONTIERS IN MATERIALS, 7, 601059

DOI: 10.3389/fmats.2020.601059

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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.

18 Open Access

On the pinning force in high density MgB2 samples

Sandu, V; Ionescu, AM; Aldica, G; Grigoroscuta, MA; Burdusel, M; Badica, P

MAR 15 2021, SCIENTIFIC REPORTS, 11, 5951

DOI: 10.1038/s41598-021-85209-2

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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.

19

New superconductor/ferromagnet heterostructure formed by YBa2Cu3O7-x and CaRuO3

Ivan, I; Pasuk, I; Crisan, A; Sandu, V; Onea, M; Leca, A; Cosar, C; Burdusel, M

NOV 2021, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 34, 115009

DOI: 10.1088/1361-6668/ac2622

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Almost all proposed configurations and practical achievements based on superconductor/ferromagnet (S/F) heterostrucutres focus on s-wave superconductors. However, several attempts targeted also high temperature superconductors, most of them using manganite ferromagnets LaXMnO3 (X: Ca or Sr) and Y1Ba2Cu3O7-x (YBCO). Here we propose a new ferromagnetic material that can be used with YBCO for the fabrication of S/F hybrid structures. We show that a ferromagnetic order can be induced in a thin layer (similar to 130 nm thickness) of CaRuO3 grown by pulsed laser deposition on epitaxial YBCO film. Detailed magnetic and structural investigations show that the observations of the weak ferromagnetism are consistent with the magnetic order induced by in-plane tensile strain of about 1.7% and the easy-magnetization axis forms an angle of similar to 180o with the layer plane. The value of the Curie temperature T (Curie) estimated using the Curie-Weiss law was 340 K. An unusual temperature dependence of the magnetic moment around the superconducting transition was observed in both field-cooled and zero-field-cooled configurations which is attributed to the paramagnetic Meissner effect.

20 Open Access

Antibacterial composite coatings of MgB2 powders embedded in PVP matrix

Badica, P; Batalu, ND; Burdusel, M; Grigoroscuta, MA; Aldica, G; Enculescu, M; Pircalabioru, GG; Popa, M; Marutescu, LG; Dumitriu, BG; Olariu, L; Bicu, A; Purcareanu, B; Operti, L; Bonino, V; Agostino, A; Truccato, M; Chifiriuc, MC

MAY 5 2021, SCIENTIFIC REPORTS, 11, 9591

DOI: 10.1038/s41598-021-88885-2

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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.

21 Open Access

Sintered and 3D-Printed Bulks of MgB2-Based Materials with Antimicrobial Properties

Badica, P; Batalu, ND; Chifiriuc, MC; Burdusel, M; Grigoroscuta, MA; Aldica, GV; Pasuk, I; Kuncser, A; Popa, M; Agostino, A; Operti, L; Padhi, SK; Bonino, V; Truccato, M

OCT 2021, MOLECULES, 26, 6045

DOI: 10.3390/molecules26196045

Show abstract

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.

22

Partially-oriented MgB2 superconducting bulks with addition of B4C and cubic BN obtained by slip casting under high magnetic field and spark plasma sintering

Grigoroscuta, MA; Aldica, G; Pasuk, I; Burdusel, M; Sandu, V; Kuncser, A; Suzuki, TS; Vasylkiv, O; Badica, P

FEB 2021, MATERIALS RESEARCH BULLETIN, 134, 111103

DOI: 10.1016/j.materresbull.2020.111103

Show abstract

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.

23 Open Access

Enhanced critical current density at high magnetic fields in MgB2 with Ga/In acetylacetonate processed by spark plasma sintering

Batalu, D; Aldica, G; Burdusel, M; Grigoroscuta, M; Pasuk, I; Kuncser, A; Ionescu, AM; Badica, P

MAY-JUN 2020, JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY-JMR&T, 9

DOI: 10.1016/j.jmrt.2020.01.109

Show abstract

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.

24 Open Access

Second magnetization peak, rhombic-to-square Bragg vortex glass transition, and intersecting magnetic hysteresis curves in overdoped BaFe2(As1-xPx)2 single crystals

Miu, L; Ionescu, AM; Miu, D; Burdusel, M; Badica, P; Batalu, D; Crisan, A

OCT 14 2020, SCIENTIFIC REPORTS, 10, 17274

DOI: 10.1038/s41598-020-74156-z

Show abstract

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.

25

Simple and clean method for obtaining Sn nanoparticles for hydrophobic coatings

Buruiana, AT; Sava, F; Matei, E; Zgura, I; Burdusel, M; Mihai, C; Velea, A

NOV 1 2020, MATERIALS LETTERS, 278, 128419

DOI: 10.1016/j.matlet.2020.128419

Show abstract

Sn nanoparticles (NPs) are usually obtained by difficult chemical routes in several steps followed by thermal treatments. Here, a simple and clean method, to obtain Sn NPs directly on the substrate, is developed based on a vapor transport technique. The method is versatile, thus can be easily adjusted to obtain Sn NPs of different size, areal density and morphology, by controlling the deposition conditions. NPs are grown on Si/SiO2 substrate and characterized. Water contact angle measurements show that Sn nanoparticles increase the surface hydrophobicity by 20%. Thus, NPs cleanly obtained from a low-cost, earth-abundant, and environmentally friendly material, can be used to modulate the wettability of surfaces. (C) 2020 Elsevier B.V. All rights reserved.

26 Open Access

Secondary Crystalline Phases Influence on Optical Properties in Off-Stoichiometric Cu2S-ZnS-SnS2 Thin Films

Sava, F; Diagne, O; Galca, AC; Simandan, ID; Matei, E; Burdusel, M; Becherescu, N; Becherescu, V; Mihai, C; Velea, A

OCT 2020, MATERIALS, 13, 4624

DOI: 10.3390/ma13204624

Show abstract

Cu2ZnSnS4 (CZTS) is an economically and environmentally friendly alternative to other toxic and expensive materials used for photovoltaics, however, the variation in the composition during synthesis is often followed by the occurrence of the secondary binary and ternary crystalline phases. These phases produce changes in the optical absorption edge important in cell efficiency. We explore here the secondary phases that emerge in a combinatorial Cu2S-ZnS-SnS2 thin films library. Thin films with a composition gradient were prepared by simultaneous magnetron sputtering from three binary chalcogenide targets (Cu2S, SnS2 and ZnS). Then, the samples were crystallized by sulfurization annealing at 450 degrees C under argon flow. Their composition was measured by energy dispersive X-ray spectroscopy (EDX), whereas the structural and optical properties were investigated by grazing incidence X-ray diffraction (GIXRD), Raman spectroscopy and optical transmission measurements. As already known, we found that annealing in a sulfur environment is beneficial, increasing the crystallinity of the samples. Raman spectroscopy revealed the presence of CZTS in all the samples from the library. Secondary crystalline phases such as SnS2, ZnS and Cu-S are also formed in the samples depending on their proximity to the binary chalcogenide targets. The formation of ZnS or Cu-S strongly correlates with the Zn/Sn and Cu/Zn ratio of the total sample composition. The presence of these phases produces a variation in the bandgap between 1.41 eV and 1.68 eV. This study reveals that as we go further away from CZTS in the composition space, in the quasi-ternary Cu2S-ZnS-SnS2 diagram, secondary crystalline phases arise and increase in number, whereas the bandgap takes values outside the optimum range for photovoltaic applications.

27 Open Access

Investigation of flux jumps during pulsed field magnetization in graphene-added MgB2 bulks

Yokoyama, K; Oka, T; Berger, K; Dorget, R; Koblischka, M; Grigoroscuta, M; Burdusel, M; Batalu, D; Aldica, G; Badica, P; Sakai, N; Muralidhar, M; Murakami, M

2020, 14TH EUROPEAN CONFERENCE ON APPLIED SUPERCONDUCTIVITY (EUCAS2019), 1559, 012080

DOI: 10.1088/1742-6596/1559/1/012080

Show abstract

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.

28 Open Access

Reproducibility of small Ge2C6H10O7-added MgB2 bulks fabricated by ex situ Spark Plasma Sintering used in compound bulk magnets with a trapped magnetic field above 5T

Badica, P; Aldica, G; Grigoroscuta, MA; Burdusel, M; Pasuk, ; Batalu, D; Berger, K; Koblischka-Veneva, A; Koblischka, MR

JUN 29 2020, SCIENTIFIC REPORTS, 10, 10538

DOI: 10.1038/s41598-020-67463-y

Show abstract

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.

29

Influence of boric acid concentration on the properties of electrodeposited CZTS absorber layers

Zaki, MY; Nouneh, K; Touhami, ME; Matei, E; Badica, P; Burdusel, M; Negrila, CC; Baibarac, M; Pintilie, L; Galca, AC

MAY 2020, PHYSICA SCRIPTA, 95, 054001

DOI: 10.1088/1402-4896/ab6afd

Show abstract

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.

30

High magnetic shielding properties of an MgB2 cup obtained by machining a spark-plasma-sintered bulk cylinder

Gozzelino, L; Gerbaldo, R; Ghigo, G; Torsello, D; Bonino, V; Truccato, M; Grigoroscuta, MA; Burdusel, M; Aldica, GV; Sandu, V; Pasuk, I; Badica, P

APR 2020, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 33, 044018

DOI: 10.1088/1361-6668/ab7846

Show abstract

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.

31

Extrinsic absorption in spark plasma sintered Zr0.8Sn0.2TiO4 ceramics investigated by terahertz time-domain spectroscopy

Nedelcu, L; Burdusel, M; Grigoroscuta, MA; Geambasu, CD; Banciu, MG; Badica, P

2019, 2019 44TH INTERNATIONAL CONFERENCE ON INFRARED, MILLIMETER, AND TERAHERTZ WAVES (IRMMW-THZ)

Show abstract

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.

32

Passive magnetic shielding by machinable MgB2 bulks: measurements and numerical simulations

Gozzelino, L; Gerbaldo, R; Ghigo, G; Laviano, F; Torsello, D; Bonino, V; Truccato, M; Batalu, D; Grigoroscuta, MA; Burdusel, M; Aldica, GV; Badica, P

MAR 2019, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 32

DOI: 10.1088/1361-6668/aaf99e

Show abstract

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.

33

Ex Situ Spark Plasma Sintering of Short Powder-in-Tube MgB2 Tapes with Open and Closed Ends

Aldica, G; Burdusel, M; Popa, S; Pasuk, I; Ionescu, AM; Kuncser, A; Badica, P

NOV 2018, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 31, 3432

DOI: 10.1007/s10948-018-4616-9

Show abstract

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.

34

Compressive properties of pristine and SiC-Te-added MgB2 powders, green compacts and spark-plasma-sintered bulks

Badica, P; Batalu, D; Burdusel, M; Grigoroscuta, MA; Aldica, GV; Enculescu, M; Gabor, RA; Wang, ZY; Huang, RX; Li, PF

JUN 15 2018, CERAMICS INTERNATIONAL, 44, 10191

DOI: 10.1016/j.ceramint.2018.03.008

Show abstract

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.

35

Addition of Sb2O5 into MgB2 Superconductor Obtained by Spark Plasma Sintering

Badica, P; Burdusel, M; Popa, S; Hayasaka, Y; Ionescu, MA; Aldica, G

AUG 2017, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 30, 2080

DOI: 10.1007/s10948-017-4016-6

Show abstract

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.

36

POWDER-IN-TUBE TAPES OF MgB2 IN Fe-SHEATH PROCESSED BY EX-SITU SPARK PLASMA SINTERING

Burdusel, M; Ionescu, AM; Grigoroscuta, M; Batalu, D; Enculescu, M; Popa, S; Mihalache, V; Aldica, G; Badica, P

2017, UNIVERSITY POLITEHNICA OF BUCHAREST SCIENTIFIC BULLETIN SERIES B-CHEMISTRY AND MATERIALS SCIENCE, 79, 172

Show abstract

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.

37

Graphene addition to MgB2 superconductor obtained by ex-situ spark plasma sintering technique

Aldica, G; Burdusel, M; Popa, S; Hayasaka, Y; Badica, P

MAY 2016, MATERIALS RESEARCH BULLETIN, 77, 211

DOI: 10.1016/j.materresbull.2016.01.041

Show abstract

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.

38

Reactive spark plasma sintering of MgB2 in nitrogen atmosphere for the enhancement of the high-field critical current density

Badica, P; Burdusel, M; Popa, S; Pasuk, I; Ivan, I; Borodianska, H; Vasylkiv, O; Kuncser, A; Ionescu, AM; Miu, L; Aldica, G

OCT 2016, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 29

DOI: 10.1088/0953-2048/29/10/105020

Show abstract

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.

39

Thin films of amorphous Ga2S3 and rare-earth sulphides

Popescu, M; Lorinczi, A; Sava, F; Velea, A; Simandan, ID; Badica, P; Burdusel, M; Galca, AC; Socol, G; Jipa, F; Zamfirescu, M

MAR 1 2015, MATERIALS LETTERS, 142, 231

DOI: 10.1016/j.matlet.2014.12.028

Show abstract

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.

40

B4C in ex-situ spark plasma sintered MgB2

Burdusel, M; Aldica, G; Popa, S; Enculescu, M; Mihalache, V; Kuncser, A; Pasuk, I; Badica, P

OCT 2015, CURRENT APPLIED PHYSICS, 15, 1270

DOI: 10.1016/j.cap.2015.07.017

Show abstract

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.

41

The influence of heating rate on superconducting characteristics of MgB2 obtained by spark plasma sintering technique

Aldica, G; Burdusel, M; Popa, S; Enculescu, M; Pasuk, I; Badica, P

DEC 15 2015, PHYSICA C-SUPERCONDUCTIVITY AND ITS APPLICATIONS, 519, 189

DOI: 10.1016/j.physc.2015.10.004

Show abstract

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.

42

Ge-Added MgB2 Superconductor Obtained by Ex Situ Spark Plasma Sintering

Batalu, D; Aldica, G; Burdusel, M; Popa, S; Enculescu, M; Pasuk, I; Miu, D; Badica, P

FEB 2015, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 28, 534

DOI: 10.1007/s10948-014-2705-y

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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.

43

Ceramics and amorphous thin films based on gallium sulphide doped by rare-earth sulphides

Popescu, M; Sava, F; Lorinczi, A; Velea, A; Simandan, ID; Badica, P; Burdusel, M; Galca, AC; Matei, E; Preda, N; Secu, M; Socol, G; Jipa, F; Zamfirescu, M; Balan, A

APR 2015, SEMICONDUCTOR SCIENCE AND TECHNOLOGY, 30

DOI: 10.1088/0268-1242/30/4/044001

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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.

44

Growth and characterization by STM of BiCo222 crystal objects: whiskers and bows

Burdusel, M; Miu, L; Zhao, PH; Yan, W; Han, YL; Nie, JC; Badica, P

MAR-APR 2015, JOURNAL OF OPTOELECTRONICS AND ADVANCED MATERIALS, 17, 430

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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.

45

Trapped magnetic field in a (NdFeB)-(MgB2) pair-type bulk magnet

Aldica, G; Burdusel, M; Badica, P

OCT 15 2014, PHYSICA C-SUPERCONDUCTIVITY AND ITS APPLICATIONS, 505, 23

DOI: 10.1016/j.physc.2014.07.001

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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.

46

Significant enhancement of the critical current density for cubic BN addition into ex situ spark plasma sintered MgB2

Badica, P; Aldica, G; Burdusel, M; Popa, S; Negrea, RF; Enculescu, M; Pasuk, I; Miu, L

SEP 2014, SUPERCONDUCTOR SCIENCE & TECHNOLOGY, 27

DOI: 10.1088/0953-2048/27/9/095013

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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.

47

Challenges of nanostructuring and functional properties for selected bulk materials obtained by reactive spark plasma sintering

Badica, P; Aldica, GV; Burdusel, M; Borodianska, H; Sakka, Y; Vasylkiv, O

MAY 2014, JAPANESE JOURNAL OF APPLIED PHYSICS, 53

DOI: 10.7567/JJAP.53.05FB22

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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

48

Influence of the Carbo-Chromization Process on the Microstructural, Hardness, and Corrosion Properties of 316L Sintered Stainless Steel

Iorga, S; Cojocaru, M; Chivu, A; Ciuca, S; Burdusel, M; Badica, P; Leuvrey, C; Schmerber, G; Ulhaq-Bouillet, C; Colis, S

JUN 2014, METALLURGICAL AND MATERIALS TRANSACTIONS A-PHYSICAL METALLURGY AND MATERIALS SCIENCE, 45A, 3096

DOI: 10.1007/s11661-014-2247-8

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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.

49

MgB2 with Addition of Bi2O3 Obtained by Spark Plasma Sintering Technique

Burdusel, M; Aldica, G; Popa, S; Enculescu, M; Pasuk, I; Badica, P

MAY 2013, JOURNAL OF SUPERCONDUCTIVITY AND NOVEL MAGNETISM, 26, 1556

DOI: 10.1007/s10948-012-2015-1

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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.

50

CoNb2O6 Ceramic with Geometric Frustration

Sandu, V; Nicolescu, MS; Banciu, MG; Popa, S; Burdusel, M

2012, AUTOMATION EQUIPMENT AND SYSTEMS, PTS 1-4, 468-471, 545

DOI: 10.4028/www.scientific.net/AMR.468-471.542

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We present the preparation, structure and physical properties of CoNb2O6 ceramics using spark plasma sintering technique. Magnetic data reveal the two antiferromagnetic transitions at 2.9 and 2 K. Microwave measurements gives epsilon(r) = 23.5 and a loss tangent of 29x10(-3).

51

MgB2 with addition of Sb2O3 obtained by spark plasma sintering technique

Burdusel, M; Aldica, G; Popa, S; Enculescu, M; Badica, P

APR 2012, JOURNAL OF MATERIALS SCIENCE, 47, 3836

DOI: 10.1007/s10853-011-6238-5

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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.

52

Composites of MgB2 with Bi2O3, Bi, Sb2O3, or Sb Obtained by Ex-situ Spark Plasma Sintering

Badica, P; Aldica, G; Burdusel, M; Endo, K

NOV 2012, JAPANESE JOURNAL OF APPLIED PHYSICS, 51

DOI: 10.1143/JJAP.51.11PG13

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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