Degradation of Superconducting Properties in MgB2 by Formation of the MgB4 Phase

Superconducting MgB₂ polycrystalline samples have been fabricated under two different conditions in order to determine the effect of MgB₄ phase. A series of samples was placed in an -alumina container closed with a cup and fired under high purity argon gas. The other series of samples was placed in an -alumina boot without any lid and fired under similar conditions. For the first series of samples, we have found pure MgB₂ phase formation and a narrow transition width at 0.4 K. For the second series of samples, significant amount of MgB₄ phase were formed and the T _zero was decreased to 27 K. For both the group of samples magnetization hysteresis loops obtained at various temperature range and applied field up to 2 T. The best J _cmag for the first series of samples was 1.9 × 10⁵ A/cm² at 10 K and 0 T, and for the second series of samples was 0.7 × 10⁴ A/cm² at 10 K and 0 T.     

Improved Transport J c in MgB2 Tapes by Graphene Doping

Graphene is a special form of carbon which can effectively enhance the critical current density J _c of MgB₂. In this work, a systematic investigation on the impact of sintering conditions and doping level was carried out for graphene-doped MgB₂ tapes. It is found that an appropriate addition level, i.e., 8 at% in this work, is very critical to obtain a high J _c in graphene-doped samples. The critical field and pinning force are improved obviously due to the graphene doping. The magnetic J _c of samples sintered at 800 °C with 8 at% graphene doping reached 1.78 × 10⁴ A/cm², at 5 T, 20 K. At the same time, the transport J _c was up to 2.38 × 10⁴ A/cm² at 10 T, 4.2 K. The lattice distortion caused by C substitution and residual C at the grain boundaries were thought to be the major factors affecting the J _c of graphene-doped MgB₂ samples.     

Superconducting Properties and Microstructure of Nanocrystalline MgB2 Bulk Prepared by Sintering of Ball-Milled Powders

Ultrafine nanostructured MgB₂ bulks with an average grain size less than 10 nm have been fabricated by high-energy ball milling and subsequent high pressure sintering. Microstructural evolution in MgB₂ subjected to high-energy ball milling has been investigated by means of X-ray diffraction (XRD). The finer grain size of MgB₂ powders of about 7 nm has been estimated from Rietveld refinement analysis of XRD data, which is confirmed by a transmission electron microscope (TEM) observation. There is almost no grain growth in the subsequent sintering at low temperature of 600?°C under pressure of 3?C5 GPa for 10?C30 min. The nanocrystalline MgB₂ bulks exhibit the lower onset critical transition temperatures (T _{c onset}) of 32?C33?K. The relative wider width of the magnetic hysteresis loops at high external magnetic field and the higher critical current density (J _c ) are obtained in nanocrystalline bulks. J _c is as high as 10⁵?A/cm² in 8?T at 10?K and 2.7×10³?A/cm² in 4?T at 20?K.     

Improving the Characteristics of Powder-In-Tube MgB2 Superconductor Fabricated Using the Extrusion Technique

High-density cylindrical MgB₂ superconductors were manufactured using an ex situ powder in tube extrusion technique. The superconducting properties of the steel-sheathed MgB₂ samples were examined with respect to their magnetisation responses, critical temperature and current density. The critical current density of the superconductor was determined by means of magnetisation measurements using Bean’s critical state model. J _c reached a maximum of 4×10⁵ A/cm² at 5 K.     

The Magnetic and Structural Properties of SiC-Doped MgB2 Bulks Prepared by the Standard Ceramic Processing

According to general formula MgB_2?x SiC _x (x=0,0.05,0.1,0.2), MgB₂ and SiC-doped bulk superconductors were prepared by the standard ceramic processing. The mixtures of the corresponding powders were sintered at 750?°C for 0.5 h under pressure of 8 bar Argon. X-ray diffraction patterns show that all the samples have MgB₂ as the main phase with a very small amount of MgO; further, with SiC-doped, the presence of Mg₂Si is also noted. The magnetization-temperature measurements showed a transition temperature of 37.5 K for the undoped sample which indicates the typical transition temperature of MgB₂. When the content of SiC increased in the sample, the transition temperatures decreased to the lower temperatures systematically. The M?CH loops measured using a VSM showed very large magnetization value at low temperature for SiC doped samples. The largest M?CH loops were taken from the sample contains 5% SiC. The critical current density of samples calculated from M?CH loops indicated a value of around 4×10⁵ A/cm², which is in good agreement with the literature.     

Superconducting properties and growth mechanism of layered structure in MgB2 bulks with Cu/Y2O3 co-doping

Bulk MgB₂ samples containing Cu and Y₂O₃ have been prepared by conventional solid state reaction at 850 °C, and the structure and superconducting properties have been investigated. Differing from the structure in previous studies, a type of novel, layered structure was obtained in Cu/Y₂O₃-doped MgB₂ sample. Furthermore, the critical current density (J _c) at high field (>4 T) was improved compared to undoped, and Cu-doped MgB₂ samples. After analyzing the phase composition, microstructure, and sintering process, it was found that Y₂O₃ and Cu are independent in providing effective pinning centers, and YB₄ impurity should be responsible for the enhancement of J _c as well as the increased irreversible magnetic field. However, J _c at low field was slightly worsened, but still maintaining 10⁵ A cm^?2 at 0 T, since the intercrystalline connectivity was not seriously deteriorated. Finally, a possible growth model was put forward to describe the formation sequences of the layered structure. It was supposed that the formation of steps at low temperature originated from the coherent relationship between Mg and MgB₂, while the steps formed at high temperature were related to the pinning effect of secondary phase during the migration of grain boundary.     

Effects of High Pressure on the Physical Properties of MgB2

The synthesis of MgB₂-based materials under high pressure gave the possibility to suppress the evaporation of magnesium and to obtain near theoretically dense nanograined structures with high superconducting, thermal conducting, and mechanical characteristics: critical current densities of 1.8?C1.0×10⁶ A/cm² in the self-field and 10³ A/cm² in a magnetic field of 8 T at 20 K, 5?C3×10⁵ A/cm² in self-field at 30 K, the corresponding critical fields being H _c2=15 T at 22 K and irreversible fields H _irr=13 T at 20 K, and H _irr=3.5 T at 30 K, thermal conduction of 53±2 W/(m?K), the Vickers hardness H _V =10.12±0.2 GPa under a load of 148.8 N and the fracture toughness K _1C =7.6±2.0 MPa?m^0.5 under the same load, the Young modulus E=213 GPa. Estimation of quenching current and AC losses allowed the conclusion that high-pressure-prepared materials are promising for application in transformer-type fault current limiters working at 20?C30 K.     

Enhancement of Critical Current Density in MgB2 Bulk with CNT-coated Al Addition

Bulk MgB₂ sample with carbon nanotube (CNT)-coated Al addition was prepared by conventional solid-state reaction at 900 °C for 30 min. We investigated the effects of Al and C co-doping on the lattice parameter, the microstructure, and the critical current density of MgB₂. The substitution of Al and C atoms for the sites of Mg and B in the MgB₂ lattice resulted in dislocations in the MgB₂ grains, which makes great contributions, along with the nanoscale oxide particles, to the enhancement of critical current density at high field (10³ A cm^?2, 7 T, 5 K) in the co-doped sample. These results contrasted significantly with the measured values of the pure MgB₂ and Al- and C-doped samples. Co-doping introduced more electrons into MgB₂ and decreased both the parameters c and a of MgB₂ lattice, and the used coating technique delayed and shortened the oxidation process of Mg and Al, leading to the decrease in the size and the content of the oxide. These advantages should be responsible for the enhancement of the critical current density as well.     

Artificial Pinning Centers on MgB2 Superconducting Thin Films Coated by FeO Nanoparticles

MgB₂ thin films were fabricated on MgO (100) single crystal substrates. First, deposition of boron was performed by rf magnetron sputtering on MgO substrates and followed by a post deposition annealing at 850?°C in magnesium vapor. In order to investigate the effect of FeO nanoparticles on magnetic properties of MgB₂ thin films, the films were coated with different concentrations of FeO nanoparticles by spin coating process. The magnetic field dependence of the critical current density $J_{\mathrm{c}}$ was calculated from the M?CH loops and also magnetic field dependence of the pinning force density $f_{\mathrm{p}}(b)$ was determined for the films containing different concentrations of FeO nanoparticles. The values of the critical current density $J_{\mathrm{c}}$ in zero field at 5?K was found to be around 1×10⁶?A/cm² for pure MgB₂ film, 1.4×10⁶ for MgB₂ film coated with 25?%, 7.2×10⁵ for MgB₂ film coated with 33?%, 9.1×10⁵ for MgB₂ film coated with 50?% and 1.1×10⁶?A/cm² for MgB₂ film coated with 100?%. It?was?found that the film coated with 25?% FeO nanoparticles has slightly enhanced critical current density and it can be noted that especially the film coated with 25?% FeO became stronger in the magnetic field. The films coated with FeO were successfully produced and they indicated the presence of artificial pinning centers created by FeO nanoparticles. The superconducting transition temperature of the film coated with 25?% FeO nanoparticles was determined by moment?Ctemperature (M?CT) measurement to be 34?K which is 4?K higher than that of the pure film.     

The role of various boron precursor on superconducting properties of MgB2/Fe

The superconducting properties of Fe sheathed MgB₂ wire has been studied as a function of precursor B powder particle size. The in situ processed MgB₂ samples were prepared by means of conventional solid state reaction method with magnesium powder (99.8%, 325 mesh) and three different types of amorphous boron powders (purity; 98.8%, >95% and 91.9%) from two sources, Pavezyum (Turkish supplier) and Sigma Aldrich. The particle sizes of Turkish boron precursor powder were selected between 300 and 800 nm. The structural and magnetic properties of the prepared samples were investigated by means of the X-ray powder diffraction (XRD) and ac susceptibility measurements. The XRD patterns showed that the diffraction peaks for our samples belong to the main phase of the MgB₂ diffraction patterns. The highest critical temperature, T_c = 38.4 K was measured for the MgB₂ sample which was fabricated by using the 98.8% B. The critical current density of this sample was extracted from the magnetization measurements and J_c = 5.4 × 10⁵ A cm⁻² at 5 K and B = 2 T. We found that the sample made by using the 98.8% boron showed almost 2 times higher J_c than that of obtained from 91.9% B powder.     

Comparative Study of Dense Bulk MgB2 Materials Prepared by Different Methods

We report on the results of a comparative investigation of highly dense bulk MgB₂ samples prepared by three methods: (i) hot deformation; (ii) high pressure sintering; and (iii) mechanical alloying of Mg and B powders with subsequent hot compaction. All types of samples were studied by AC susceptibility, DC magnetization, and resistivity measurements in magnetic fields up to μ₀ H = 160 kOe. A small but distinct anisotropy of the upper critical field $\psi {\rm H}_{c2}^{\alpha ,b} /H_{c2}^c \sim 1.2$ connected with some texture of MgB₂ grains was found for the hot deformed samples. The samples prepared by high pressure sintering as well as by mechanical alloying show improved superconducting properties, including high upper critical fields H _c2 (μ₀ H _c2 (0) ～ 23 T), irreversibility fields H _irr which are strongly shifted towards higher values H _irr(T) ～ 0.8 H _c2(T) and high critical current J _c (J _c = 10⁵ A/cm² at 20 K and 1 T).     

Properties of MgB2 Thin Films Deposited on Different Substrates Prepared by Ex-Situ Annealing Process

MgB₂ thin films were deposited on MgO (100) substrate and r-plane Al₂O₃ $(1\bar{1}02)$ substrate by ex-situ annealing of boron film in magnesium vapor. The thickness of ex-situ annealed MgB₂ films is approximately 600 nm according to data observation by ellipsometer. The magnetic properties of samples were determined using a vibrating sample magnetometer. The magnetic field dependence of the critical current density J _c was calculated from M–H loops and also the magnetic field dependence of F _p was compared for the different temperature ranges from 5 to 25 K. The critical current density J _c was found to be around 1.0×10⁶ A/cm² and 1.7×10⁶ A/cm² in zero field at 5 K for MgB₂ films deposited on MgO and r-plane Al₂O₃ substrates, respectively. It was found that the critical current density of the film deposited on MgO became stronger than that of r-plane Al₂O₃ in the magnetic field. The superconducting transition temperature was determined by ac susceptibility measurement using physical properties measurement system. ac susceptibility measurements for MgB₂ films deposited on MgO and r-plane Al₂O₃ substrates were performed as a function of temperatures at constant frequency and ac field amplitude in the absence of dc bias field. The critical current densities as a function of temperature were estimated from the ac susceptibility data.     

High Critical Current Densities in MgB2 Films Grown on Hastelloy Tape by Hybrid Physical-Chemical Vapor Deposition

We report on the high critical current densities in MgB₂ films directly grown on Hastelloy tapes without any buffer layer by using the hybrid physical-chemical vapor deposition method. MgB₂ films were formed by reaction of Mg metal vapor with the incoming B₂H₆ gas on the heated substrates. In MgB₂ films grown for 10 min at 500 °C in total working pressure 100 Torr with gas mixing ratio H₂:B₂H₆=70:30, we observed the transport critical current density (J _c) was approximately 10⁶ A/cm² at 4 T and 20 K in magnetic fields applied parallel to the substrate plane. This value is higher than those observed in epitaxial MgB₂ films on sapphire substrates grown by using the same method. Magnetic field dependence of J _c of this sample was well explained by the grain-boundary pinning model. Our result opens up a possibility that the coated conductors made of MgB₂ films have a strong potential for high current applications.     

Microwave direct synthesis of MgB2 superconductor

Intermetallic compound superconductor MgB₂ was synthesized from spherical magnesium powder and lower purity amorphous boron powder by microwave direct heating. Powder X-ray diffraction (XRD) analysis indicates that the phases of the synthesis sample are MgB₂ (major phase) and a small amount of MgO. Scanning electron microscope (SEM) observation shows that the MgB₂ grain size is homogeneous and the particle size is about several hundreds of nanometers. The onset superconducting transition temperature of the MgB₂ sample measured by the temperature dependence of magnetization measurement is about 37.6 K. The critical current density J_c calculated according to the Bean model are about 2.0 × 10⁵ A/cm² at 20 K in self-field and 1.0 × 10⁵ A/cm² at 20 K in 1 T applied field.     

Role of diffusion-annealing temperature on the microstructural and superconducting properties of Cu-doped MgB2 superconductors

This study deals with not only investigate the effect of the copper diffusion on the microstructural and superconducting properties of MgB₂ superconducting samples employing dc resistivity as a function of temperature, scanning electron microscopy (SEM) and X-ray diffraction (XRD) measurements but also calculate the diffusion coefficient and the activation energy of copper for the first time. Electrical-resistivity measurements indicate that both the room-temperature resistivity value and zero resistivity transition temperatures (T _c ) increase with increasing the diffusion-annealing temperature from 650 to 850?°C. SEM measurements show that not only the surface morphology and grain connectivity improve but also the grain size of the samples increases with the increase in the diffusion-annealing temperature up to 850?°C. As for the XRD results, all the samples contain the MgB₂ phase only and exhibit the polycrystalline superconducting phase with more intensity of diffraction lines, leading to the increasement in the lattice parameter a and c. Additionally, the diffusion coefficient is observed to increase from 6.81?×?10^?8 to 4.69?×?10^?7?cm²?s^?1 as the diffusion-annealing temperature increases, confirming that the Cu diffusion at lower temperatures is much less significant. Temperature dependence of the Cu diffusion coefficient is described with the aid of the Arrhenius relation D?=?3.75?×?10^?3 exp (?1.15?±?0.10?eV/k _B T) and the corresponding activation energy of copper in MgB₂ system is found to be about 1.15?eV. The possible reasons for the observed improvement in microstructural and superconducting properties of the samples due to Cu diffusion are also discussed.     

Fabrication and Transport Properties of MgB2 Thin Films and Tunnel Junctions

We report on fabrication and characterization of MgB₂ thin films and tunnel junction structures. The MgB₂ films were prepared on Al₂O₃, Si, glass, and plastic foil substrates by either vacuum codeposition of boron and magnesium, or high-temperature magnesium annealing of boron films. The crystalline structure of our films depended directly on the method of preparation. The films prepared by codeposition and postannealed in Ar atmosphere were amorphous with nanocrystal inclusions and were characterized by very smooth surfaces. On the other hand, the boron-precursor films annealed in magnesium vapor were rough, polycrystalline with approximately 1-μm-diameter single-crystal blocks. Because of their surface quality, the amorphous films were used for preparation of point contact junctions and for optical characterization. The point-contact spectra of tested junctions exhibited a two-gap structure. The MgB₂ polycrystalline films was used for bulk transport studies. The best films were characterized by the critical temperature T _c of up to 39 K and the current density j _c at 4.2 K of about 10⁷ A/cm².     

One-Step Synthesis and Sintering of MgB2 by Spark Plasma Sintering

We have studied the one-step procedure for simultaneous synthesis and sintering of SiC-doped MgB₂ by the spark plasma sintering technique. Two types of composition, one in which Mg is strongly deficient, with the atomic ratio $\mathrm{B/Mg} = 3.75$ , and one in which Mg content is slightly higher than the stoichiometric value, specifically $\mathrm{B/Mg} = 1.87$ , were investigated. The amount of SiC was 12 wt.% and 9 wt.%, respectively. For comparison we also studied the way the deficit of Mg can be compensated in a second process of sintering. The sample with Mg deficit shows that SiC is left almost unreacted but the results are spectacular: the highest critical temperature, 36.5 K, the highest upper critical field and the highest self-field critical current density 6.7×10⁵ A/cm² at 10 K. In the sample with overstoichiometric Mg, SiC is decomposed, carbon diffuses within MgB₂ but the critical temperature is only of 35.8 K and the zero-field critical current density is one order of magnitude lower. The compensation of the deficit of Mg in the two-step procedure is not efficient. The critical temperature is even lower, 35.8 K, the upper critical field is also lower despite SiC decomposition and C diffusion within MgB₂ and the critical current density is slightly above 10⁵ A/cm². However, at low temperatures and fields of order 7 T the sample with overstoichiometric Mg and the sample prepared by the two-step procedure have higher critical current density.     

Role of diffusion-annealing time on the superconducting, microstructural and mechanical properties of Cu-diffused bulk MgB2 superconductor

In this study, the effect of various annealing time (0.5, 1, 1.5 and 2 h) on microstructural, mechanical and superconducting properties of the Cu-diffused bulk MgB₂ superconducting samples is investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), Vickers microhardness (H _v ) and dc resistivity measurements for the first time. The critical transition temperature, grain size, phase purity, lattice parameter, surface morphology, crystallinity and room temperature resistivity values of the bulk samples prepared are compared with each other. Electrical-resistivity measurements show that the sample (annealed at 850 °C for 1 h), exhibiting the highest room temperature resistivity, obtains the maximum zero resistivity transition temperature (T _c ). From the XRD results, all the samples contain MgB₂ as the main phase with a very small amount of Mg₂Cu phase. Moreover, SEM investigations conducted for the microstructural characterization illustrate that not only does the grain size of the samples studied enhance gradually, but the surface morphology and grain connectivity also improve with the increase in the diffusion-annealing time up to 1 h beyond which all the properties obtained start to degrade. Indeed, the worst surface morphology is observed for the Cu-diffused bulk MgB₂ superconductor exposed to 2 h annealing duration. At the same time, Vickers microhardness, elastic modulus, load independent hardness, yield strength, fracture toughness and brittleness index values are calculated separately for the pure and Cu-diffused samples. It is found that the microhardness values depend strongly on the diffusion-annealing time. Furthermore, the diffusion coefficient of the Cu ion in the bulk MgB₂ superconductor is obtained to change from 1.63 × 10^?7 to 2.58 × 10^?7 cm² s^?1. The maximum diffusion coefficient is observed for the sample prepared at 850 °C for 1 h whereas the minimum one is noted for the sample annealed at 850 °C for 2 h, confirming that the annealing-time of 1 h is the best ambient to improve the mechanical, microstructural and superconducting properties of the samples produced.     

The Effect of Cu Addition on the Phase Formation and Critical Current Density in the Sugar Doped MgB2 Superconductor

With the aim of improving the critical current density (J _c ) in the MgB₂ superconductor, minor Cu (3?at%) was doped to the MgB₂ samples in-situ sintered with Mg powder and sugar-coated amorphous B powder. Combined with thermal analysis, phase identification, microstructure observation and J _c measurement, the effect of minor Cu addition on the sintering mechanism, microstructure and critical current density of sugar-doped MgB₂ superconductors were investigated. It is found that the minor Cu addition could obviously accelerated the MgB₂ phase formation and improve the growth of MgB₂ grains during the sintering process of sugar-doped MgB₂ due to the appearance of Mg?CCu liquid at low sintering temperature. On the other hand, the Mg?CCu liquid hindered the reactive C released from sugar entering in the MgB₂ crystal lattice. Hence, the connectivity between MgB₂ grains was improved accompanying with the C substitution for B is decreased. At 20?K, the J _c of co-doped samples at low fields was further increased whereas it is decreased at high fields, compared with the only sugar-doped samples.     

Thickness Dependence of Critical Current Density in MgB2 Films Prepared by Thermal Evaporation Method

MgB₂ films with the thickness of 350 to 1150 nm have been prepared on the Al₂O₃ (001) single crystal substrates from high purity B and Mg powder by the thermal evaporation method. Films were then heat treated ex-situ under Mg vapor at 950?°C to achieve actual MgB₂ stoichiometry. Thickness of the films, so the deposition time, was varied to investigate its influence on critical current density of the films. The films fabricated were analyzed by means of microstructural, transport, and magnetic properties. The best T _c and T _zero values were obtained to be 39.5 K and 38 K, respectively, and decreased with increasing the thickness. We found that the critical current density of the films prepared is highly thickness dependent. The maximum $J_{c}^{\mathrm{mag}}$ value was calculated to be 3.18×10⁶ A?cm^?2 at 10 K and zero field for 1150 nm thick films but dropped drastically by thickness.