Investigation of Nb–B Diffusion and the Superconducting Properties of MgB2/Nb/Cu Tapes

The Nb?CB diffusion behaviors and their effects on the superconducting properties of MgB₂/Nb/Cu tapes were investigated. Two relevant samples of the Nb?CB diffusion couples and monocore MgB₂/Nb/Cu tapes were prepared with the same standard in situ PIT method, respectively. And both the samples were sintered at 650, 750, 850, and 950°C for 2 hours, respectively. It has been found that Nb?CB interface is invisible in the diffusion couples sintered at low temperatures as 650°C, correspondingly the superconducting properties of MgB₂ tapes are superior to those of the ones sintered at the other three temperatures. With the heating temperature increasing, Nb?CB interface, mainly NbB₂ with a little NbB, appears and becomes thicker gradually in the Nb?CB diffusion couples. The corresponding superconducting properties of MgB₂ tapes follow the similar patterns: within the range from 650°C to 950°C, the higher the sintering temperature, the poorer the superconducting performances, because the Nb?CB diffusion in MgB₂ tapes could cause the property degradations of MgB₂/Nb tape. As extended to the actual fabrications of Nb sheathed MgB₂ tapes or wires, suitable sintering temperature range should be from 650°C to 750°C for the desired performances.     

Frequency dependence of dielectric properties of ex situ MgB<Subscript>2</Subscript> bulks

In this study, frequency dependent electrical properties of ex situ polycrystalline MgB₂ sintered at 650–850?°C were investigated. Dielectric permittivity (ε′, ε″), dielectric loss (tan δ), alternating current (AC) conductivity (σ_ac) as a function of frequency (100 Hz–10 MHz) were measured at room temperature. The X-ray diffraction (XRD) and grain morphology were analysed and correlated to the findings in dielectric properties. Due to weakly coupled grains and presence of high fraction of oxides, positive real dielectric permittivity was measured for the ex situ samples as compared with the negative real dielectric permittivity shown by the in situ MgB₂. Nevertheless, the samples sintered at higher temperature showed improved grain connectivity as reflected by the higher AC conductivity and dielectric loss. The semicircle observed in the complex impedance plots together with the combined spectroscopy plots indicates that the electrical behavior of the ex situ samples is mainly due to the bulk and grain boundary responses as opposed to the sole bulk response of the in situ MgB₂. The modelled equivalent circuit also suggests the presence of insulating grain boundary barrier (due to the oxide phases) next to the conducting bulk in the ex situ samples.     

Sintering mechanism of Ag-doped MgB<Subscript>2</Subscript> superconductor from low temperature to high temperature

Combined with thermal analysis and phase identification, the sintering process of Ag-doped MgB₂ superconductor was investigated. It is found that the Ag doping could form Mg–Ag liquid through the eutectic reaction at low temperature (about 470 °C) and then obviously accelerated the formation of MgB₂ phase. Moreover, a sintering model is also proposed to illustrate the liquid activated sintering mechanism present in the sintering process of Ag-doped MgB₂ samples. The sintering model is supposed to provide theoretic guidance for optimizing the sintering condition in the synthesis of doped MgB₂ superconductors.     

Progress in Critical Current Density (<Emphasis Type="Italic">J</Emphasis><Subscript><Emphasis Type="Italic">c</Emphasis></Subscript>) in Sintered MgB<Subscript>2</Subscript> Bulks

The present paper focuses on methods of further improving the flux pinning and critical current density of disk-shaped MgB₂ bulk superconductors by adding excess Mg metal in combination with an optimum silver content and optimized processing conditions. Bulk MgB₂ samples were produced by in situ solid-state reaction in Ar gas ambient using high purity commercial powders of Mg metal and 1.5 wt% carbon-coated amorphous B powders mixed in a fixed ratio of Mg/B = 1.1:2. Further, 4 wt% silver was added to improve flux pinning as well as mechanical performance of the bulk MgB₂ material. The magnetization measurements confirmed a sharp superconducting transition with T_c,onset at around 37 K, which is only by 1 K lower than in bulk MgB₂ material produced without carbon-coated amorphous boron. The critical current density (J_c) values significantly improved in the MgB₂ material with 4 wt% of silver and 1.5 wt% of carbon-coated amorphous boron, sintered at 775 ^°C for 3 h. At 20 K, this sample showed J_c at around 500 and 350 kA/cm² in the self-field and 1 T, respectively, which makes it suitable for several industrial applications.     

The Effects of Structural,Thermal, and Magnetic Properties of Hexylbenzene-Doped MgB<Subscript>2</Subscript> Superconductor

The effects of the amount of hexylbenzene additive (C₁₂H₁₈) on the structural, thermal, and magnetic properties of MgB₂ superconductor are examined in this study. Pure and hexylbenzene-doped MgB₂ bulk samples were produced with in situ solid-state reaction method. X-ray diffraction patterns of MgB₂ doped with MgB₂ and hexylbenzene at different ratios were determined to have MgB₂ as the main phase and consisted of a small amount of MgO. Pure and different ratios of hexylbenzene-doped Mg and B starting powders were heat-treated by a differential scanning calorimeter between room temperature and 800 °C. It was determined from the differential scanning calorimetry curves obtained that the first exothermic peak pointed the MgB₂ phase emerging with a solid–solid (Mg–B) reaction, and this temperature shifted towards the low temperatures as the hexylbenzene addition rates increased. It was observed that there was dependency to the applied field in all samples from the ac susceptibility measurements as a function of the temperature in pure and hexylbenzene-doped MgB₂ superconductor materials, and shift towards the lower temperatures in T _c, superconducting transition temperature, with increasing content. It was observed that the changes occurred in in-phase (\(\chi ^{\prime })\) and out-off-phase (\(\chi ^{\prime \prime }\)) components of ac susceptibility both weakened the MgB₂ phase structure of hexylbenzene content and, as a result of this, led to changes in the pinning mechanism.     

Time-Dependent Diffusion Coefficient of Fe in MgB<Subscript>2</Subscript> Superconductors

The iron (Fe) diffusion in superconducting MgB₂ bulk samples has been studied for sintering time durations of 15 min, 30 min, 1 h, 2 h, and 4 h at 900^°C. Fe coating bulk polycrstalline superconducting MgB₂ samples for Fe coating were prepared by pelletizing and used in the diffusion experiments with initial sintering at 800^°C for 1 h. A thin layer of Fe was coated on MgB₂ pellets by evaporation in vacuum. Effects of Fe diffusion on the structural, electrical, and superconducting properties of MgB₂ have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (IR), energy-dispersive X-ray spectroscopy (EDS), and resistivity measurements. Fe diffused samples have slightly increased critical transition temperatures and have larger lattice parameter c values, in comparison with bare samples. Fe diffusion coefficients were calculated from depth profiles of c parameter and room temperature resistivity values. Depth profiles were obtained by successive removal of thin layers from Fe diffused surfaces of the samples. Our results have shown that the Fe diffusion coefficient decreases with increasing sintering time and resistivity measurements can be utilized for determination of diffusion coefficient.     

Phase formation sequences and mechanism of MgB<Subscript>2</Subscript> superconductor with minor Sn doping

Combined with thermal analysis and phase identification, the phase formation of Sn-doped MgB₂ superconductor during the sintering process were systematically investigated. As compared to the sintering of MgB₂, the first exothermal peak occurs at a lower temperature, which suggests the accelerated formation of MgB₂ after minor Sn doping. The sintering process of minor Sn-doped MgB₂ orderly underwent the melting of Sn, the reaction between Mg and Sn, the eutectic Mg–Sn reaction, the solid–solid Mg–B reaction, the melting of Mg, the liquid–solid Mg–B reaction and the Sn precipitation. Based on the phase formation mechanism, MgB₂ bulks was successfully synthesized by Sn-activated sintering at 600 °C for only 5 h, exhibiting a dramatic decrease in the sintering time compared to the sintering of undoped MgB₂.     

Fabrication and magnetoresistivit of ex-situ processed MgB<Subscript>2</Subscript>/Fe monofilament tapes without any intermediate annealing

We have fabricated MgB₂/Fe monofilament wires and tapes by a powder-in tube (PIT) technique, using an ex-situ process without any intermediate annealing. MgB₂/Fe monofilament tapes were annealed at 650–1,050°C for 60 min and 950°C for 30–240 min. We have investigated the effect of annealing temperatures and times on the formation of MgB₂ phase, activation energy, temperature dependence of irreversibility field H _irr(T) and upper critical field H _c2(T), transition temperature (T _c), lattice parameters (a and c), full width at half maximum, crystallinity, resistivity, residual resistivity ratio, active cross-sectional area fraction and critical current densities. We observed that the activation energies of the MgB₂/Fe monofilament samples increased with increasing annealing temperature up to 950°C and with increasing annealing time up to 60 min while it decreased with increasing magnetic field. For the MgB₂/Fe monofilament tape, the slope of the H _c2–T and H _irr–T curves decreased with increasing annealing temperature from 850 to 950°C as well as with increasing annealing time from 30 to 60 min. The transport and microstructure investigations show that T _c, J _c and microstructure properties are remarkably enhanced with increasing annealing temperature. The highest value of critical current density is obtained for the sample annealed at 950°C for 60 min. The J _c and T _c^offset values of the sample annealed at 950°C for 60 min were found to be 260.43 A/cm² at 20 and 38.1 K, respectively.     

Influence of coronene addition on some superconducting properties of bulk MgB<Subscript>2</Subscript>

This study reports the effect of coronene (C₂₄H₁₂) addition on some superconducting properties such as critical temperature (T_c), critical current density (J_c), flux pinning force density (F_p), irreversibility field (H_irr), upper critical magnetic field (H_c2), and activation energy (U₀), of bulk MgB₂ superconductor by means of magnetisation and magnetoresistivity measurements. Disk-shaped polycrystalline MgB₂ samples with varying C₂₄H₁₂ contents of 0, 2, 4, 6, 8, 10 wt%, were produced at 850 °C in Ar atmosphere. The obtained results show an increase in field-J_c values at 10 and 20 K resulting from the strengthened flux pinning, and a decrease in critical temperature (T_c) because of C substitution into MgB₂ lattice, with increasing amount of C₂₄H₁₂ powder. The H_c2(0) and H_irr(0) values are respectively found as 144, 181, 172 kOe, and 128, 161, 145 kOe for pure, 4 wt% and 10 wt% C₂₄H₁₂ added samples. The U₀ depending on the magnetic field curves were plotted using thermally activated flux flow model. The maximum U₀ values are respectively obtained as 0.20, 0.23 and 0.12 eV at 30 kOe for pure, 4 wt% and 10 wt% C₂₄H₁₂ added samples. As a result, the superconducting properties of bulk MgB₂ at high fields was improved using C₂₄H₁₂, active carbon source addition, because of the presence of uniformly dispersed C particles with nanometer order of magnitude, and acting as effective pinning centres in MgB₂ structure.     

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.     

Formation of MgO whiskers on the surface of bulk MgB<Subscript>2</Subscript> superconductors during in situ sintering

Magnesium oxide (MgO) whiskers (with diameters of about 60–80 nm) formed on the surface of bulk polycrystalline MgB₂ superconductor at a relative low temperature (720 °C) during in situ sintering process. The reaction between Mg and B powders begins at a temperature below melting point of Mg and maintains till about 750 °C. The residual Mg powders evaporate and react with trace oxygen to form MgO vapor as the temperature exceeds the melting temperature of Mg and a low supersaturation is required for the growth of MgO whiskers. The preformed MgB₂ and MgO crystals act as substrates and the melted Mg powders on the surface of them serve as catalysts during the growth process of MgO whiskers. The growth process of MgO whiskers is dominated by a self-catalytic vapor–liquid–solid (VLS) mechanism.     

Studies on the Composite System of Bi-2212 Glass Ceramic and MgB<Subscript>2</Subscript> Superconductors

The composites of glass ceramic Bi-2212 and MgB₂ superconductors were prepared at ambient conditions. The transmission electron microscopy images of the composite samples illustrate the presence of glass ceramic inclusions in bulk MgB₂. Temperature-dependent magnetization of the composite samples shows two superconducting transitions: one at 80 K corresponding to the Bi-2212 phase and a second one at 39 K corresponding to the MgB₂ phase, suggesting that the two superconducting phases are separated with clear boundaries. The critical current density (J _c) and pinning force values are increased in composite systems by an order of magnitude compared to that of individual samples. The pinning mechanism in the composite sample is the same as in the matrix phase. Reduced field maxima (h _max) are observed at 0.15 for composite samples. A low value of h _max for composite samples indicates the random orientation of grain boundaries and repulsive pinning force in the composite samples.     

Improved microstructure and flux pinning properties of Gd-substituted (Bi,Pb)-2212 superconductor sintered between 846 and 860 °C

The influence of sintering temperature on microstructural and superconducting properties of Gd-substituted (Bi,Pb)-2212 superconductor was investigated. It is found that the microstructure of the system can be tailored and refined so as to yield the best superconducting properties in terms of critical current density (J_C) and flux pinning by heat treating at a temperature in the range 846-860 °C. The samples sintered at 858 °C show the maximum self-field J_C of 31,960 kA m^{− 2} and those sintered at 846 °C show the maximum flux pinning force [F_P = 1698 kN m^{− 3}] as against 1860 kA m^{− 2} and 16 kN m^{− 3}, respectively for the undoped sample sintered at its optimum sintering temperature. The changes in microstructure followed by very high enhancement of J_C, J_C-B characteristics and F_P due to Gd-substitution within a small temperature range, is of great scientific and technological significance.     

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.     

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.     

The effects of annealing temperature on the in-field Jc and surface pinning in silicone oil doped MgB2 bulks and wires

The effects of sintering temperature on the lattice parameters, full width at half maximum (FWHM), strain, critical temperature (T_c), critical current density (J_c), irreversibility field (H_irr), upper critical field (H_c2), and resistivity (ρ) of 10 wt.% silicone oil doped MgB₂ bulk and wire samples are investigated in state of the art by this article. The a-lattice parameter of the silicone oil doped samples which were sintered at different temperatures was drastically reduced from 3.0864 Å to 3.0745 Å, compared to the un-doped samples, which indicates the substitution of the carbon (C) into the boron sites. It was found that sintered samples at the low temperature of 600 °C shows more lattice distortion by more C-substitution and higher strain, lower T_c, higher impurity scattering, and enhancement of both magnetic J_c and H_c2, compared to those sintered samples at high temperatures. The flux pinning mechanism has been analyzed based on the extended normalized pinning force density f_p = F_p/F_p,max scaled with b = B/B_max. Results show that surface pinning is the dominant pinning mechanism for the doped sample sintered at the low temperature of 600 °C, while point pinning is dominant for the un-doped sample. The powder in tube (PIT) MgB₂ wire was also fabricated by using of this liquid doping and found that both transport J_c and n-factor increased which proves this cheap and abundant silicone oil doping can be a good candidate for industrial application.     

Sintering and electrical properties of Ce<Subscript>0.8</Subscript>Sm<Subscript>0.2</Subscript>O<Subscript>1.9</Subscript> film prepared by spray pyrolysis and tape casting

Ce_0.8Sm_0.2O_1.9 (SDC) powder was synthesized by spray pyrolysis at 650 °C. XRD results showed that phase-pure SDC powder with an average crystallite size of 11 nm was synthesized. SDC electrolyte film was prepared by tape casting and sintered at different temperatures of 1,300, 1,400 and 1,500 °C for 2 h, respectively. The SDC electrolyte film was relatively denser and showed finer microstructure at relatively lower temperature of 1,400 °C, which might be due to the high sintering activity of the spray pyrolysis SDC powder. The ionic conductivity of the SDC electrolyte film sintered at 1,400 °C reached a maximum value of 9.5 × 10⁻³ S cm⁻¹ (tested at 600 °C) with an activation energy for conduction of 0.90 eV.     

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.     

Varistor properties and aging behavior of ZnO-V<Subscript>2</Subscript>O<Subscript>5</Subscript>-Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> ceramics with sintering process

The microstructure, electrical properties, and DC-accelerated aging behavior of the ZnO-V₂O₅-Mn₃O₄ ceramics were investigated at different sintering temperatures of 850–925°C. The microstructure of the ZnO-V₂O₅-Mn₃O₄ ceramics consisted of ZnO grain as a primary phase, and Zn₃(VO₄)₂ which acts as a liquid-phase sintering aid, in addition to Mn-rich phase as secondary phases. The maximum value (3,172 V/cm) and minimum value (977 V/cm) of breakdown field were obtained at sintering temperature of 850 and 900°C, respectively. The nonlinear coefficient exhibited the highest value, reaching 30 at 925°C and the lowest value, reaching 4 at 850°C. The optimum sintering temperature was 900°C, which exhibited not only high nonlinearity with 24 in nonlinear coefficient, but also the high stability, with %ΔE_1mA = −0.9% and %∆α = −12.5% for DC-accelerated aging stress of 0.85 E_1mA/85°C/24 h.     

Effect of nano-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> doping on formation and superconductivity of bulk MgB<Subscript>2</Subscript>

Bulk materials of MgB₂ have been prepared with the stoichiometry of MgB₂(Al₂O₃) _x (x = 0, 2, 5, 10 and 20% nano-Al₂O₃ powders), by using solid-state reaction route. All samples were sintered at 750 °C for 30 min in a calorimeter to monitor the sintering reaction process. It is found that the onset temperatures of reaction between Mg and B powders increase significantly with increasing the amount of Al₂O₃. However, the reaction time is shortened for the nano-Al₂O₃ powders can effectively activate the reaction as a catalyst. The critical transition temperature decreases from 38.5 to 31.6 K, and the corresponding temperature window becomes narrow (less than 2.6 K). Furthermore, the amount of MgO impurity was found to increase with the increase of Al₂O₃, which probably indicates that partial Mg was replaced by Al.