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).     

Magnetic Characterization of SiC Doped Bulk MgB2 Superconductor

Flux pinning is a very significant mechanism to improve critical current density in MgB₂ for many applications, such as developing the performance of wires and tapes. In this study, we have done a systematic study of SiC inclusions in the main matrix of MgB₂. Sample production in the form of MgB_2?x (SiC) _x was carried out by using solid state reaction method (x=0,0.01,0.02,0.04,0.06,0.10) in the argon atmosphere. The structural and magnetic properties of the prepared samples were investigated. Structural characterization of samples was performed by the X-ray powder diffraction (XRD) technique and the Scanning Electron Microscopy (SEM) measurements. Magnetic properties were determined by M?CH loops, magnetization-temperature (M?CT), and AC susceptibility measurements. The T _c of the samples was determined by the M?CT measurements while the J _c is determined through the M?CH measurements. SiC inclusions up to some ratios (x=0.06) increase the critical current density by up to about 50%, while the critical temperature T _c remains unchanged in compatible with the literature.     

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.     

Surface Barrier and Bulk Pinning in MgB2 Superconductor

We present a modified method of preparation of the new superconductor MgB₂. The polycrystalline samples were characterized using X-ray and magnetic measurements. The surface barriers control the isothermal magnetization loops in powder samples. In bulk as prepared samples we always observed symmetric magnetization loops indicative of the presence of a bulk pinning mechanism. Magnetic relaxation measurements in the bulk sample reveal a crossover of surface barrier to bulk pinning.     

Superconductivity in High-Pressure Synthesized Pure and Doped MgB2 Compounds

Dense pure and doped (Mg_{1 ? x} A _x )B₂ samples with A = Na, Ca, Cu, Ag, Zn, and Al were synthesized at high pressure–high temperature in a multi-anvils press (3.5–6 GPa, 900–1000°C) for 0 < x ≤ 0.20. They were studied by X-ray diffraction, scanning electron microscopy and their superconducting properties were investigated by AC susceptibility, magnetization, and transport measurements. Only Al is really substituted on the Mg site. The other elements form secondary phases with B or Mg. No large effect is observed on the superconducting properties T _c, j _c critical current, H _irr, and H _c2.     

Magnetic Characterization of MgB2 Bulk Superconductor for Magnetic Field Mitigation Solutions

Magnetic shielding properties of MgB₂ bulk samples synthesized by the SPS (Spark?CPlasma?CSintering) technique were characterized in low applied magnetic fields at temperatures ranging from 20 to 37 K. The used growth technique allows one to produce this compound in different shapes and sizes required for shielding applications. In this framework, shielding magnetic-induction field profiles generated by MgB₂-based shield components, shaped as planar thick disks, were measured by means of a suitable Hall probe in-plane array. The magnetic field distribution at different vertical distances above the sample was also obtained by a micrometric motion of the probe ensemble. Magnetic field profiles were then analyzed in the framework of the critical state model and the critical current density, J _c , was evaluated. The J _c magnitude indicates that the material under test is a good candidate for passive magnetic shield manufacturing up to temperatures close to the transition one.     

Superconducting Performance of Ex-situ SiC Doped MgB2 Monofilamentary Tapes

The superconducting performance of the ex-situ SiC doped MgB₂ monofilamentary tapes are reported. Polycrystalline powders of MgB₂ doped with 5 and 10 wt% SiC were synthesized by a conventional solid-state reaction route and characterized for their superconducting performances. It was found that the superconducting parameters viz., upper critical field (H _c2), irreversibility field (H _irr) and critical current density (J _c) were improved significantly with SiC addition. It was also found that relatively lower synthesis temperature resulted in further improved superconducting parameters in comparison to higher synthesis temperature. Thus, synthesized powders are used for the fabrication of ex-situ powder-in-tube (PIT) monofilamentary tapes. The superconducting performance in terms of critical current density (J _c), being determined from both magnetization (J _cm) and transport (J _ct) measurements, was improved significantly. In particular, the SiC doped MgB₂ tapes (fabricated using 700 °C heat treated bulk powder) exhibited the transport J _ct of nearly 10⁴ A/cm² under applied fields of as high as 7 Tesla. Further, it was found that the J _ct anisotropy decreases significantly for SiC doped tapes. Disorder due to substitution of C at B site being created from broken SiC and the presence of nano SiC respectively in SiC added ex-situ MgB₂ tapes was responsible for decreased anisotropy and improved J _c(H) performance.     

Evaluation of Microstructural and Mechanical Properties of Ag-Diffused Bulk MgB2 Superconductors

Electrical, microstructural, and mechanical properties of undiffused and Ag-diffused bulk MgB₂ superconductors are systematically studied using dc resistivity, scanning electron microscopy (SEM), and Vickers microhardness (H _V ) measurements. The resistivity (at room temperature), critical (onset and offset) temperature, variation of transition temperature, hole-carrier concentration, surface morphology, Vickers microhardness, elastic modulus, and yield strength values of the samples are obtained and compared with each other. One can see that all superconducting parameters given above depend on the Ag diffusion on MgB₂ system. The obtained results illustrate that the room temperature resistivity reduces with the increment of diffusion annealing temperature because of the hole filling when the onset ( $T_{c}^{\mathrm{onset}}$ ) and offset ( $T_{c}^{\mathrm{offset}}$ ) critical temperatures determined from the resistivity curves are obtained to enhance from 38.4 to 39.7 K and from 36.9 to 38.8 K, respectively. Further, SEM studies carried out for the microstructural characterization demonstrate that the surface morphology and grain connectivity also improve with the increase of the diffusion annealing temperature. In fact, the best surface morphology is observed for the Ag-diffused bulk MgB₂ superconductor exposed to 850 °C annealing temperature. Besides, it is obtained that the load-dependent microhardness values reduce nonlinearly as the applied load increases until 2 N, beyond which the curves shift to the saturation region, presenting that all the samples exhibit the indentation size effect (ISE) behavior. Further, the elastic modulus and yield strength values observed decrease with the enhancement of the applied load.     

Fabrication of Bulk Targets of MgB2 with Stoichiometric and Nonstoichiometric Contents

Powder of magnesium diboride was obtained by solid phase reaction of mixture of magnesium （〉 99% pure） and amorphous boron （〉 99% pure） powders at 650-900 ℃ temperatures in inert atmosphere. During synthesis process main attention was paid. to removing oxide layer of surfaces of powder particles by organic solvents in Glovebox, where concentration of oxygen and water steam is less than 5 ppm. Homogenization and activation of powders were conducted in a planetary nano-mill by WC balls in an inert area. Pressing of the obtained powders was conducted in an argon atmosphere. MgB2 nonstoichiometric powders contained excess boron and magnesium, Magnesium hydride was used as source of excess boron, which is fragile compound and easy to grind in nano-mill. It decomposites with metallic magnesium and hydrogen up to 280 ℃ temperature. Commercial magnesium diboride powder （Aldrich, 〉 99%） was used for fabrication of MgB2 bulk targets. Powders systems of MgB2-Mg, MgB2-MgH2, MgB2-B homogenized by nano-mill in Glove box was used for fabrication of composites with nonstoichiometric contents. The targets were cylinders with diameters of 27-52 mm and height of 5-15 mm. Consolidation of pressed powdery composites was conducted in argon atmosphere. Synthesis of MgB2 from mixture of magnesium and amorphous boron powders and simultaneous consolidation were conducted by hot pressing （HP） method. Phase content of the obtained targets were established by XRD method after dry polishing. Superconducting characteristic of the obtained samples were measured by vibrational magnetometer. The superconducting transition with an onset at 39 K was observed in a good agreement with the results of the other groups obtained on samples prepared by conventional techniques. The phase exists near the nominal composition without a significant homogeneity range.     

多元耦合场CVI法制备C/C的工艺与结构研究

以丙烯气作为炭源气体,普通炭毡作为增强体,采用多元耦合场CVI方法快速制备了炭/炭复合材料.为了在炭/炭复合材料制备的实验条件和材料质量之间建立相应的关系,设计了一组实验.通过使用偏光显微分析、XRD测定、Raman微区分析等手段对结果进行了表征.结果表明:在650℃,12kPa实验条件下可以得到密度较高、均匀性较好,并具有较好结构的炭/炭复合材料,这说明较低的温度和较高的压力适合实验需要.对样品中出现的巨大再生锥结构进行了简要的分析.实验中出现了一种新形貌的热解炭,其具有最高的可石墨化性能.这种雨点状偏光结构热解炭被命名为点状热解炭,其形成机理可以认为是电磁场吸附和不完全固化粘液层的脱氢炭化.     

硫化锌掺杂二氧化硅靶材致密化研究

硫化锌掺杂二氧化硅(以下简用ZnS+SiO2表示)靶材主要用于CD-RW,DVD-RAM光盘,它通过溅射方法在光盘上形成一层保护膜,以保证光盘的记录性能不受外界条件的影响.靶材的密度越高,溅射形成的膜的质量越好.ZnS+SiO2靶材可通过热等静压工艺或热压工艺获得,本实验采用真空热压工艺对ZnS+SiO2靶材致密化进行了研究,分析了主要热压工艺参数对ZnS+SiO2靶材密度的影响.最适宜的热压温度为1 250℃,压力为36 MPa,时间为3 h,采用此工艺参数制备的靶材相对密度达99.2%.     

用扩散法制备MgB2块材的研究进展

MgB₂超导体具有优良的超导电性能,受到了极大的关注。用不同方法制备的MgB₂超导体,其超导电性能也不尽相同。常压扩散法使用的设备简单且操作方便,制备出的MgB₂超导电性能也较为优越。本文系统地介绍了属于扩散法的渗透生长法、渗透胶囊法、液相Mg扩散法和气相扩散法并对其优缺点进行了比较,重点介绍了液相Mg扩散法在超导电缆、电磁屏蔽和磁悬浮等方面的应用。根据对各种合成方法的比较及其相关的应用,展望了扩散合成法的发展趋势。     

A New Method for the Estimation of H c2 Anisotropy in Polycrystalline MgB2 Samples

By using isothermal magnetization measurements in polycrystalline MgB₂ samples, we estimate the H ^c _c2 in the interval [0, T _c]. By combining these measurements to the estimated H ^ab _c2 from the onset of the diamagnetic transition in isofield and isothermal magnetic measurements, an estimation of the anisotropy parameter can be achieved. The H ^c _c2 values coming from high quality polycrystalline samples agrees nicely to those obtained on single crystals. Our results show a temperature variation of the γ(T ) = H ^ab _c2/H^c2 with γ(T _c) ≈ 3.     

起始粉末对MgB2超导线材成相及微结构的影响

采用原位法粉末装管工艺制备了不同起始粉末MgB2/Nb/Cu单芯线材。通过X射线衍射(XRD)、扫描电镜(EMS)研究了不同起始粉末对线材微观结构及相成分的影响。结果显示,从线材的微观结构和相成分角度来看,B粉影响不大,起主要作用的是Mg粉。     

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 ₀ H = 160 kOe. A small but distinct anisotropy of the upper critical field 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 (₀ 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).     

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.     

MgB2 Superconducting Tips for Scanning Tunneling Microscopy Study

We report a simple method for the fabrication of reproducible, clean, and stable MgB₂ superconducting tips. The quality of these tips has been verified by imaging the surface of a thin Au(111) film sample, using a low temperature scanning tunneling microscopy (STM). Using the MgB₂ superconducting tip, high-quality semiatomically resolved STM surface images of the thin Au(111) film sample have been observed, which unambiguously indicates that the fabrication of relatively superconducting MgB₂, suitable for use as STM tips, is feasible.     

Densification and Grain-Growth Behavior of Various Amounts of SiO2 Doped 8YSCZ/SiO2 Composites

The effect of SiO₂ addition on densification and grain-growth behavior of 8YSCZ/SiO₂ composites was investigated using high purity 8 mol% yttria-stabilized cubic zirconia powders (8YSCZ) doped with 0, 1, 5, 10 wt% SiO₂. The specimens were sintered at 1400°C for 1 hour. It was seen that the sintered density increased with SiO₂ content up to 1 wt% and further increase in SiO₂ content led to a decrease in density. The enhanced density with increasing SiO₂ content up to 1 wt% could be mainly attributable to liquid phase sintering. For grain growth measurements, the specimens sintered at 1400°C were annealed at 1400, 1500, and 1600°C for 10, 50, and 100 hours. The experimental results showed that the grain growth in 8YSCZ/SiO₂ composites occurred more slowly than that in undoped 8YSCZ. Also, the grain growth rate decreased with increasing SiO₂ content. The grain growth exponent value and the activation energy for undoped 8YSCZ were found to be 2 and 289 kJ/mol, respectively. The addition of SiO₂ raised the grain growth exponent value to 3, and activation energy for the grain growth process was increased from 289 to 420 kJ/mol for the addition of SiO₂ from 0 to 10 wt%.