Bulk MgB2 Research Articles

The discrepancies in different facets of MgB2 bulk superconductors prepared under various sintering durations by spark plasma sintering

Seven MgB2 bulk superconductors with good superconductivity and crystallinity were prepared under the pressure of 50 MPa at 950 °C and different sintering durations (15 ∼ 240 min) by spark plasma sintering (SPS), with the onset critical temperature (T c,onset) around 37.5 K. The superconducting properties and microstructure measured from the facets perpendicular (PeF) and parallel (PaF) to the compression direction of the SPSed MgB2 bulk samples were also analyzed to investigate the effect of the sintering duration on the MgB2 bulks and the discrepancy between the PeF and the PaF. The optimum performance was obtained from the sample prepared for 45 min for both facets, and the critical current density (J c) measured from the PeF and the PaF are 364 kA cm−2 and 344 kA cm−2 in self field at 20 K, respectively. The PeF exhibits better Jc performance than the PaF at low fields and the PaF exhibits better J c performance than the PeF at high fields. It can be concluded that the sintering duration affects the properties of the PeF mainly by changing their crystallite size. While for the PaF, the sintering duration mainly affects the microstructural defects, such as cracks, pores and secondary phase particles, thus further affecting their J c performances. In terms of the flux pinning mechanism of the SPSed MgB2 bulk samples, the PaF is less susceptible to sintering duration than the PeF, and the better J c performance of the PaF at high fields is due to the stronger grain boundary pinning. It can be also found that the point pinning being stronger at higher temperature is the result of the decreasing anisotropy of MgB2 bulk samples with the temperature.

Increase in the infield critical current density of MgB2 thin films by high-temperature post-annealing

We propose a novel fabrication technique based on the formation of a Nb protective layer on a MgB2 thin film and high-temperature post-annealing to increase the critical current density (J c) of MgB2 films under an external magnetic field. Analyses of the crystal structure and the composition of the processed MgB2 films confirmed the suppression of the evaporation and oxidation of Mg by high-temperature annealing above 550 °C. The MgB2 film annealed at 650 °C exhibited a J c of 1.62 MA cm−2 under 5 T, which is the highest reported value for MgB2 films, wires, and bulk samples to date.

Superconducting properties of sintered bulk MgB2 prepared from hexane-mediated high-energy-ultra-sonicated boron

Recently, novel low cost techniques have been employed to improve critical current density of MgB2. Ultra-sonication is one such technique. We report on the influence of hexane dispersant on particle size of ultra-sonicated cheap commercial boron and the superconducting properties of MgB2 bulks prepared using this new precursor. XRD showed major peaks corresponding to MgB2, with small fractions of MgO and unreacted Mg. Tc was close to 39 K, with a sharp transition. The highest Jc was found in the sample with boron ultra-sonicated for 30 min as high as 375, 328, and 270 kA/cm2 at 10, 15, and 20 K, respectively. SEM analysis revealed tiny particles and layers randomly dispersed in the microstructure, while EDX indicated that these particles were secondary phases of Mg, B, and O. Flux pinning diagrams showed the peak of normalized pinning force located close to b = 0.2, depicting dominance of grain boundary pinning mechanism.

Quick Boron Ultra-Sonication Refinement in Distilled Water for a Cheap and Mass Production of Enhanced Bulk MgB <sub>2</sub>

Quick Boron Ultra-Sonication Refinement in Distilled Water for a Cheap and Mass Production of Enhanced Bulk MgB <sub>2</sub>

Enhanced critical current density of MgB2 superconductor using a milled MgB4 precursor

The synthesis of bulk MgB2 superconductors from Mg and MgB4 precursors instead of the conventional in situ process increases the packing density, but further enhancement of the critical current density is required. Herein, to improve the critical current density of bulk MgB2, the MgB4 precursor was subjected to planetary milling in toluene. The MgB4 powder was then mixed with Mg and heat-treated at 650 °C for 1 h to synthesize bulk MgB2. The microstructure, phases, and superconductivity of bulk MgB2 were investigated to determine the effect of MgB4 milling. MgB4 milling decreased the MgB2 grain size, and carbon incorporation from the milling solvent was observed, which caused the deterioration of the MgB2 crystallinity. These changes caused a reduction of the critical temperature; however, the critical current density was improved due to the increased magnetic flux pinning sites such as grain boundary and lattice distortion.

Dehydrogenation-induced crystal defects for significant enhancement of critical current density in polycrystalline H-doped MgB2

The present study discovers the significant enhancement of critical current density by the pinning of borohydride and crystal defects in the hydrogen-treated MgB2 bulks. Based on the concept of gas doping, the nanosized borohydride Mg(BH4)2 is formed by synthesizing H-doped MgB2 bulks in an H2 atmosphere at 300 °C and 350 °C, and the critical current density was enhanced over the entire field. The H-doped MgB2 bulks are then experienced dehydrogenation at 300 °C and 350 °C, respectively, and the decomposition of Mg(BH4)2 induced nanosized pits on the surface of the MgB2 grains, leading to a further enhancement of critical current density, 1.5 × 104 A cm−2 at 20 K and 2.5 T, which is three times larger than that of the un-doped MgB2 sample, 4.8 × 103 A cm−2. The hydrogenation and dehydrogenation hardly changed the superconducting transition temperature or the pinning mechanism of the MgB2 samples. The enhancement of the critical current density is possibly attributed to the pinning effects of the crystal defects, and the reduction of MgO.

Reverse advance internal magnesium diffusion process to produce dense MgB2 bulks and high JC wires through high pressure heat treatment

Here we report a new versatile technique to manufacture MgB2 massive samples, called reverse advance internal magnesium diffusion (r-AIMI). The idea focuses on the goal of obtaining dense bulk or wire samples depending on synthesis conditions. In respect to the traditional AIMI procedure, in which a central Mg rod is covered with a B corona, here a Mg tube is filled with B powder and clad in a Ti external sheath, which is quite similar to the traditional (powder in tube) technique. After cold deformation, during which several intermediate low temperature heat treatments are necessary in order to relax the Ti sheath and Mg tube, samples are reacted at high temperature and ambient pressure to form a dense MgB2 core. The MgB2 phase results are totally disconnected from metallic sheath, and can be easily extracted and characterized. Critical current density measurements show values exceeding 106 A cm−2 below 1.5 T at 20 K.In the last part of the paper, we show the effect of final heat-treatment performed under high pressure to eliminate the present void and connect the external sheath to the internal MgB2 core and so permitting the electric transfer necessary for power applications of wires.

Superconducting and levitation force characterisation of pyrene added MgB2 bulk superconductors

This research presents the influence of pyrene (C16H10) addition (0, 2, 4, 6, 8, 10 wt%) on the superconducting properties of bulk MgB2. For C16H10 added MgB2 samples, a shrinkage in a-lattice parameters was determined, whereas c-lattice parameters remained practically unchanged. The (110) peak observed at 2θ ≈ 59.9◦ slightly shifted to higher angles, the lattice strain increased and the crystallite size reduced after C16H10 addition. By virtue of induced stronger pinning force, the in-field critical current density (Jc) increased after C16H10 addition. The Jc value at 20 K and 4 T was obtained about two times higher (8.54 × 103 A/cm2) for 4 wt% C16H10 added MgB2 sample than that of the pure one. In addition, the variation of levitation force characteristic of MgB2 with increasing C16H10 content was determined at 20, 25 and 30 K. The best vertical levitation force performance in zero-field-cooled regime was obtained as 7.09 N/g at 20 K for 4 wt% C16H10 added MgB2 sample with 13 mm in diameter.

High-field superconductivity in C-doped MgB2 bulk samples prepared by a rapid synthesis route

The upper critical field sets the thermodynamic limit to superconductivity. A big gap is present between the upper-critical-field values measured in MgB2 polycrystalline bulk superconductors and those of thin films, where values as high as ~ 50 T have been achieved at 4.2 K. Filling this gap would unlock the potential of MgB2 for magnet applications. This work presents the results of an extensive experimental campaign on MgB2 bulk samples, which has been guided by a Design of Experiment. We modeled the dependence of the upper critical field on the main synthesis parameters and established a new record (~ 35 T at 4.2 K) preparing C-doped bulk samples by a non-conventional rapid-synthesis route. This value appears to be an upper boundary for the upper critical field in bulk samples. Structural disorder in films seems to act selectively on one of the two bands where superconductivity in MgB2 takes place: this enhances the upper critical field while reducing the critical temperature only by few Kelvins. On the other hand, the critical temperature in bulk samples decreases monotonically when structural disorder increases, and this imposes a limit to the maximum achievable upper critical field.

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

Partially-oriented MgB2 bulk discs (13 and 9 %) with the starting compositions of (MgB2)0.99(B4C)0.01 and (MgB2)0.99(c-BN)0.01 were fabricated by slip casting under an H0 = 12 T magnetic field (perpendicular to the disc surface) and subsequent spark plasma sintering. The maximum critical current density and irreversibility field are for H//H0 (H=applied field). These values are higher or similar to the randomly-oriented samples with the same composition. The maximum volume pinning force (Fp) is lower in the partially-oriented ones than in the randomly-oriented samples. The pinning-force-related parameters depend on the additive and orientation. Assessment of the major pinning mechanism within the scaling and percolation models considering these parameters shows significant limitations. A method to scale Fp is proposed; for the randomly and partially-oriented samples (that show an extra peak in Fp), the single and double Gaussian functions fit well. The results suggest an anisotropic influence of carbon substituting for boron in the MgB2.

Acid Assisted Synthesis of HB Sheets through Exfoliation of MgB2 Bulk in Organic Media

Hydrogen boride sheets (HB sheets) were efficiently synthesized through wet chemical exfoliation of bulk MgB2. High production yield of HB sheets over 50% was achieved in 2 h reaction time by the a...

Size reduction of boron particles by high-power ultrasound for optimization of bulk MgB2

Critical current density, J c, in superconductors is strongly connected with size of defects in the material. Frequently, the smaller defects, the higher J c. In this work, we tried to reduce the size of cheap commercial boron precursor powder using high energy ultra-sonication in ethanol media. The resulting powder was then utilized in synthesizing bulk MgB2 via sintering at 775 °C. Effect of boron powder ultra-sonication on superconducting properties of the bulk MgB2 was studied and discussed. SEM of ultra-sonicated boron showed fine particles with sharp edges (high-energy surfaces), irregular shapes and clustering of fine particles occurred for longer ultra-sonication durations. XRD proved a high quality of MgB2 with only small traces of MgO. Around 36% improvement in Jc at 20 K and Tc close to 39 K were observed in MgB2 bulk prepared with boron ultra-sonicated for 15 min. Microstructure studies showed numerous nanometre sized MgB2 grains in the bulk. Other bulks (made of boron ultra-sonicated longer, for 30, 45, and 60 min) have larger grains. It resulted in slightly lower J c, anyway, still by 22% higher than in reference bulk. The present results demonstrate that the high performance bulk MgB2 can be achieved without reduction in T c via employing a cheap boron, reduced in size by high-energy ultra-sonication.

Enhancement of Bc2 and Birr in bulk MgB2 superconductors with SnO2 Additions

Three (MgB2)1-x(SnO2)x samples with x ranging from 0 to 5 wt% were prepared by the in situ route to study the effect of tin dioxide additions on the superconducting properties of MgB2 bulk materials. All of the reacted samples were slightly Mg deficient although the starting Mg:B precursor powder ratio was 1:2. A heat treatment (HT) temperature of 700 °C with a dwell time of 30 min was used. XRD results showed evidence of peak shifts for MgB2 phases with SnO2 addition. The magnitude of the a-axis lattice constant change (0.361 ± 0.075 %) calculated for the 3 wt% doped samples is comparable in magnitude to that seen previously for the C-doped MgB2 bulks which exhibited enhanced BC2. The upper critical fields (BC2) and the irreversibility fields (Birr) were measured resistively in fields up to 14 T at 5 K to Tc. The best BC2 value at 20 K (15.2 T based on extrapolation) was seen for sample IS3 (x =3 wt%), and was comparable to the best BC2 values (≈ 15 T at 20 K) seen for C-doped MgB2 bulks. IS3 had a corresponding Birr = 10.8 T (20 K). The superconducting transition temperature (Tc) appeared to increase slightly with doping, although within the range of error bars (37.4 K to 37.6 K for 1.6 T BC2 increase at 20 K), in contrast to C doping which is accompanied by a significant decrease in Tc (39 K to 36 K for 3.8 % C doped MgB2 bulk). We attribute the observed increase in both BC2 and Birr for SnO2-additions to lattice strain caused by the introduction of precipitates within the grains.

Improvement of critical current density of MgB2 bulk superconductor processed by Spark Plasma Sintering

AbstractSpark Plasma Sintering (SPS) is a promising rapid consolidation technique that allows a better understanding and optimization of the sintering kinetics and therefore makes it possible to obtain MgB2 bulk superconductor with tailored microstructures consisting of grains with either spherical or elongated morphology. In this contribution, the role of the precursor powders on the superconducting properties of MgB2 is investigated. Three sets of bulk MgB2 material were processed from: (i) a commercially available MgB2 powder; (ii) a mixture of Mg metal and amorphous B using a single‐step solid‐state reaction process and (iii) a mixture of amorphous boron coated with carbon and Mg metal. The samples were prepared in the same SPS processing conditions. The microstructure of the samples was investigated by X‐ray diffraction, SEM and TEM and correlated to their superconducting properties. The critical current density of the best sample at 20K was Jc = 500 kA/cm2 in self‐field, which is one of the highest critical current density reported for MgB2 bulk superconductors.

Structure and pinning centres in MgB2 bulk, wires and thin films and in MT-YBCO

Structure and pinning centres in MgB2 bulk, wires and thin films and in MT-YBCO

Flux pinning and microstructure of a bulk MgB2 doped with diverse additives

In bulk high-temperature superconductors, Ag is usually used as an additive thus improving mechanical performance. In MgB2 doped with Ag, the Ag reacts with Mg, forming Mg–Ag phases acting as a vortex pinning medium. In this work, we analyze the electromagnetic and pinning properties of bulk MgB2 doped with 1 wt% MgB4, 4 wt% Ag, and 1 wt% Dy2O3, prepared at the Shibaura Institute of Technology (SIT), Tokyo. In three compounds of MgxB2 + 4 wt% Ag with x = 1, 1.075, and 1.1, the effect of Mg excess was studied. The magnetic moment was measured by a vibrating sample magnetometer (VSM). Pinning was studied in terms of a pinning diagram, i.e. the field dependence of the normalized pinning force density, F n = F/F max. In all studied samples, the peak of the F n (b) dependence (b= B/B irr, B irr being the irreversibility field) was observed at around b= 0.2, indicating a prevailing flux pinning at grain boundaries. A slight shift of the peak with decreasing temperature indicated a defect size distribution in the pinning landscape. Transmission electron microscopy (TEM) showed a granular structure of all samples composed of MgB2 grains of about 230 nm (average size), with ensembles of small grains (22 nm in average) of Ag3Mg, AgMg, Ag, Dy2O3, and MgB4. While the large MgB2 grains control the main pinning mechanism, the small precipitates seem to determine details of the current flow through the grain boundaries.

Optimization of Carbon Encapsulated Boron Doping for High‐Performance Bulk Sintered MgB2

Carbon has been a standard doping agent in MgB2 for long time. It, however, has also participated in a non‐uniform distribution of the constituents throughout the bulk MgB2. To address this issue, carbon encapsulated boron (CEB) was used instead of the manually added mixture of boron and carbon. The previous studies confirmed that only low concentrations of carbon in CEB were effective for synthesis of a high‐performance bulk MgB2. Here, a further step in optimization carbon content in CEB is reported. Carbon content in CEB varied as 1, 1.1, 1.35, 1.5, and 1.9 wt%. X‐ray diffraction (XRD) results depict a slight shift in peaks corresponding to a–b plane, indicating carbon substitution into the lattice. High superconducting critical current density in self‐field, such as 660, 550, and 435 kA cm−2, was observed in the samples with 1.5 wt% CEB at 10, 15, and 20 K, respectively. In addition, Jc of 75 kA cm−2 at 2 T and 20 K was observed in the 1.5 wt% CEB sample, which is thrice the value observed in the pure sample, with a minute tradeoff in Tc (around 37.5 K). Scanning electron microscope (SEM) images reveal that small particles of size ranging from 50 to 200 nm contribute to Jc improvement. Energy‐dispersive X‐ray (EDX) results show carbon uniformly distributed throughout the bulk.

Magnetic Flux Trapping and Flux Jumps in Pulsed Field Magnetizing Processes in REBCO and Mg-B Bulk Magnets

Pulsed-field magnetization technique (PFM) is expected as a cheap and an easy way for HTS bulk materials for utilizing as intense magnets. As the generation of heat due to magnetic flux motion in bulk magnets causes serious degradation of captured fields, it is important to investigate the flux motions during PFM in various field applications. The authors precisely measured the magnetic flux motion in the cryocooled MgB2 bulk magnets containing various amount of Ti. We classified the motions to “no flux flow (NFF)”, “fast flux flow (FFF)”, and “flux jump (FJ)” regions. The results showed that addition of Ti shifts the field invasion area to high field areas, and expands the NFF regions. The highest field-trapping appears at the upper end of the NFF region. Since the heat generation and its propagation should attribute to the dissipation of magnetic flux, FFF leads to FJ. Compared with MgB2, we referred to GdBCO as for the flux motion. A flux jump was observed at 30 K when the pulse field of 7 T was applied to the preactivated sample, showing its stability against FJ.

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 5\xa0T

Bulk discs (20 mm diameter and 4.3 mm thickness) of MgB2 added with Ge2C6H10O7 were obtained by Spark Plasma Sintering. Six samples with composition MgB2(Ge2C6H10O7)0.0014 and one undoped sample were fabricated under similar conditions and were magnetically characterized in order to determine the scattering of properties and reproducibility. The main source of the scattering of the properties is the decomposition of the additive due to elimination of the organic part in gas form, which occurs stepwise with intensive vacuum drops at around ~ 560 and ~ 740 °C. A third drop, which is sometimes not well resolved being part of the second peak at 740 °C, occurs at ~ 820 °C. The critical temperature at the midpoint of the transition, Tc, shows only a relatively small variation between 37.4 and 38 K, and the irreversibility field at a low temperature of 5 K takes values between 8 and 10 T. The pinning force and pinning force related parameters do not correlate with the carbon substituting for boron in MgB2 and suggest a synergetic influence of the microstructural details and carbon. Overall, despite the superconducting properties scattering, the samples are of high quality. Stacked into a column of six samples, they can trap at the center and on the surface of the column a magnetic field of 6.78 and 5.19 T at 12 K, 5.20 and 3.98 T at 20 K and 2.39, and 1.96 T at 30 K. These promising values, combined with facile fabrication of the samples with relatively high quality and reproducibility, show the feasibility of their use in building complex and large compound arrangements for bulk magnets and other applications.

A record-high trapped field of 1.61 T in MgB2 bulk comprised of copper plates and soft iron yoke cylinder using pulsed-field magnetization

A trapped field of BT = 1.61 T was experimentally achieved at the central surface of an MgB2 bulk composite (60 mm in diameter and 20 mm in height) at 20 K by double pulsed-field magnetization (PFM) using a split-type coil. The composite bulks consisted of two MgB2 ring bulks sandwiched by thin copper ring plates, which were then stacked, and a soft iron yoke cylinder was inserted in the central bore of the rings. The copper ring plates delayed the rise time and duration of the magnetic pulse due to eddy currents. The inserted soft iron yoke attracted the magnetic flux and enhanced the trapped field strength mainly due to its large permeability. As a result, the trapped field was enhanced from BT = 0.34 T for the single MgB2 ring bulk without the copper plates and soft iron yoke to BT = 1.00 T for the composite with both copper plates and the soft iron yoke. The inserted soft iron yoke can be exploited to enhance the trapped field because the intrinsic BT of the single MgB2 ring bulk was smaller than the saturation field of the yoke (∼2 T). Using an optimized second pulse application after suitable flux trapping from the first pulse application, the trapped field was enhanced considerably to BT(2nd) = 1.61 T, which is a record-high trapped field for an MgB2 bulk by PFM to date. The combination of the longer magnetic pulse application by the copper plates, the enhancement of the effective applied field by the inserted soft iron yoke, and the double pulse application using split-type coil is an effective technique to enhance the trapped field in the MgB2 bulk using PFM.