Excellent Jc in the low-temperature sintered MgB2 superconductors consisted of uncompleted MgB2 phase and residual Mg

Though low-temperature sintering of MgB₂ superconductors below Mg melting point can effectively depress volatility of Mg and increase sintering density, its development was limited in recent years for the reason that it usually took very long time to form complete MgB₂ phase with excellent J_c at low temperature. In present work, significantly improved J_c was surprisingly obtained in the MgB₂ samples sintered at 575 °C for only 5 h after short-time ball milling, even though formation of MgB₂ phase is not completed and lots of residual Mg is still present in these samples. The grain connectivity in prepared samples is obviously improved compared to referred MgB₂ sample sintered at high temperature, which is responsible for the improvement of J_c. The method developed in present work seems bring a new opportunity for the development of low-cost practical MgB₂ superconductors with improved J_c without using expensive nanometer-size dopants or high-temperature sintering.     

Analysis of the precipitation process of secondary phase MgNi2.5B2 and superconducting properties in Ni-doped MgB2 bulk

A polycrystalline MgB₂ sample with 4 at.% Ni powder addition has been synthesized by a solid-state reaction at 750 °C. Two different Ni powders, raw (40 μm) and ball-milled (10 μm) particles were selected to clarify the influence of the Ni particle size on the secondary phase MgNi_2.5B₂ formation and the critical current density J_c of MgB₂ bulks. According to the investigation of the sintering, it was found that the smaller Ni particles may significantly decrease the formation temperature of the MgNi_2.5B₂ ternary compound to 550 °C. Combined with scanning electron microscopy (SEM) analysis and magnetic measurements, it was suggested that the addition of fine Ni particles led to MgNi_2.5B₂ inclusion precipitating along the spiral terraces of MgB₂ grains and with small particles sizes. The unique microstructure is responsible for the smaller reduction in J_c, which partly eliminates the effect of weak links compared with the coarse Ni particles. Besides, the formation mechanism of the microstructures and the relative location of MgNi_2.5B₂ varying from cluster at the MgB₂ grain boundaries to a screw arrangement around the MgB₂ grains with the decrease of the Ni grain sizes were also discussed in detail.     

Effect of Na2W2O7 addition on low-temperature sintering and microwave dielectric properties of CaWO4

Effects of Na₂W₂O₇ addition on low-temperature sintering, microstructure and microwave dielectric properties of CaWO₄ were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and microwave dielectric resonator methods in this paper. The CaWO₄ material could be sintered into a dense ceramic (~ 96% theoretical density) at 850 °C/2 h without affecting its microwave dielectric properties greatly by adding appropriate amount of Na₂W₂O₇. The XRD results showed that CaWO₄ main phase with trace amount of Na₂W₂O₇ second phase was observed in (1 − x) CaWO4-xNa₂W₂O₇ (0 < x ≤ 0.04) ceramics. The chemical compatibility of 0.96CaWO₄-0.04Na₂W₂O₇ ceramic with silver (Ag) powders was also investigated. The Ag showed inert behavior with 0.96CaWO₄-0.04Na₂W₂O₇ ceramic when co-fired at 875 °C for 2 h.     

Synthesis and structural characterization of (Bi2O3)1?x (Y2O3)x and (Bi2O3)1?x (Gd2O3)x solid solutions

Solid solution series, (Bi₂O₃)_1−x (Y₂O₃)_x and (Bi₂O₃)_1−x (Gd₂O₃)_x, forx = 0.10, 0.20, 0.30 and 0.40 were synthesized by standard ceramic technique. The structural phase characterization was carried out using X-ray powder diffraction technique. It was found that the solid solution containing 20–40 mole% of Y₂O₃ had face-centred cubic structure. All samples of the solid solution series, (Bi₂O₃)_1−x (Gd₂O₃)_x, had rhombohedral single phase in the concentration range 0.10 ≤x ≤ 0.40. Lattice parameters offcc phase of Y₂O₃ doped samples were calculated from the X-ray diffraction data. The lattice constant ‘a’ gradually decreases with increasing content of dopant concentration (x) for the Y₂O₃ doped system and obeys Vegard’s rule. The unit cell parameters for the (Bi₂O₃)_1−x (Gd₂O₃)_x doped samples showing rhombohedral phase were obtained on hexagonal setting.     

Synthesis,structural and optical characterization of Ni-doped ZnO nanoparticles

Nanocrystalline Zn_1−x Ni _x O (x = 0.00, 0.02, 0.04, 0.06, 0.08) powders were synthesized by a simple sol–gel autocombustion method using metal nitrates of zinc, nickel and glycine. Structural and optical properties of the Ni-doped ZnO samples annealed at 800 °C are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive analysis using X-rays (EDAX), UV–visible spectroscopy and photoluminescence (PL). X-ray diffraction analysis reveals that the Ni-doped ZnO crystallizes in a hexagonal wurtzite structure and secondary phase (NiO) was observed with the sensitivity of XRD measurement with the increasing nickel concentration (x ≥ 0.04). The lattice constants of Ni-doped ZnO nanoparticles increase slightly when Ni²⁺ is doped into ZnO lattice. The optical absorption band edge of the nickel doped samples was observed above 387 nm (3.20 eV) along with well-defined absorbance peaks at around 439 (2.82 eV), 615(2.01 eV) and 655 nm (1.89 eV). PL measurements of Ni-doped samples illustrated the strong UV emission band at ~3.02 eV, weak blue emission bands at 2.82 and 2.75 eV, and a strong green emission band at 2.26 eV. The observed red shift in the band gap from UV–visible analysis and near band edge UV emission with Ni doping may be considered to be related to the incorporation of Ni ions into the Zn site of the ZnO lattice.     

Preparation and characterization of NiO, Fe2O3, Ni0.04Zn0.96O and Fe0.03Zn0.97O nanoparticles

Nickel oxide (NiO), iron (III) oxide (Fe₂O₃), and mixed oxide (Ni_0.04Zn_0.96O and Fe_0.03Zn_0.97O) nanoparticles were synthesized by modified sol–gel method. The nanoparticle structural and morphological properties were investigated by infrared spectroscopy (FTIR), X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), and Mössbauer spectroscopy. The mixed oxides were characterized by energy-dispersive X-ray spectroscopy (EDX). The oxide precursor powders were analyzed by thermogravimetry (TG) and differential scanning calorimetry (DSC). The average sizes of the obtained NiO and Ni_0.04Zn_0.96O nanocrystallites were evaluated by X-ray line broadening using Scherrer's equation and were found to be 36 and 23 nm, respectively. Fe₂O₃ and Fe_0.03Zn_0.97O nanoparticles presented similar sizes, around 19 nm. EDX spectroscopy indicated that the calculated compositions of the mixed oxides were nearly consistent with their estimated molar ratios.     

Dielectric properties of Pb[(1?x)(Zr1/2Ti1/2)?x(Zn1/3Ta2/3)]O3 ceramics prepared by columbite and wolframite methods

Polycrystalline samples of Pb[(1 − x)(Zr_1/2Ti_1/2) − x(Zn_1/3Ta_2/3)]O ₃ , where x = 0.1–0.5 were prepared by the columbite and wolframite methods. The crystal structure, microstructure, and dielectric properties of the sintered ceramics were investigated as a function of composition via X-ray diffraction (XRD), scanning electron microscopy (SEM), and dielectric spectroscopy. The results indicated that the presence of Pb(Zn_1/3Ta_2/3)O₃ (PZnTa) in the solid solution decreased the structural stability of overall perovskite phase. A transition from tetragonal to pseudo-cubic symmetry was observed as the PZnTa content increased and a co-existence of tetragonal and pseudo-cubic phases was observed at a composition close to x = 0.1. Examination of the dielectric spectra indicated that PZT–PZnTa exhibited an extremely high relative permittivity at the MPB composition. The permittivity showed a ferroelectric to paraelectric phase transition at 330 °C with a maximum value of 19,600 at 100 Hz at the MPB composition.     

Effects of Fe2O3 doping on the microstructure and piezoelectric properties of 0.55Pb(Ni1/3Nb2/3)O3-0.45Pb(Zr0.3Ti0.7)O3 ceramics

0.55Pb(Ni_1/3Nb_2/3)O₃-0.45Pb(Zr_0.3Ti_0.7)O₃(PNN-PZT) ceramics with different concentration of xFe₂O₃ doping (where x = 0.0, 0.8, 1.2, 1.6 mol%) were synthesized by the conventional solid state sintering technique. X-ray diffraction analysis reveals that all specimens are a pure perovskite phase without pyrochlore phase. The density and grain size of Fe-doped ceramics tend to increase slightly with increasing concentration of Fe₂O₃. Comparing with the undoped ceramics, the piezoelectric, ferroelectric and dielectric properties of the Fe-doped PNN-PZT specimens are significantly improved. Properties of the piezoelectric constant as high as d₃₃ ~ 956 pC/N, the electromechanical coupling factor k_p ~ 0.74, and the dielectric constant ε_r ~ 6095 are achieved for the specimen with 1.2 mol% Fe₂O₃ doping sintered at 1200 °C for 2 h.     

Influence of doping Nb5+ and Mn2+ on the PTCR effects of Ba0.92Ca0.05(Bi0.5Na0.5)0.03TiO3 ceramics

As a positive temperature coefficient of resistivity (PTCR) material, Ba_0.92Ca_0.05(Bi_0.5Na_0.5)_0.03TiO₃ ceramics with donor doping of Nb⁵⁺ and acceptor doping of Mn²⁺ were prepared by a conventional mixed oxide method. The influence of contents of Nb⁵⁺ and Mn²⁺ on the microstructure and PTCR characteristics of Ba_0.92Ca_0.05(Bi_0.5Na_0.5)_0.03TiO₃ ceramics sintered at 1,360°C for 2 h was investigated. The result showed that the Curie temperature (T _c) was shifted to a lower temperature with increasing of the content of Nb⁵⁺ and the resistance jump (ρ_max/ρ_min) was enhanced with doping of Mn²⁺. The grain size of ceramic sample decreased with increasing of contents of donor Nb⁵⁺ and acceptor Mn²⁺. The Ba_0.92Ca_0.05(Bi_0.5Na_0.5)_0.03TiO₃ ceramic with 0.4 mol%Nb⁵⁺ and 0.04 mol%Mn²⁺ exhibited a low ρ_RT of 5.0 × 102 Ω cm, a typical PTCR effect of ρ_max/ρ_min > 10³, and a T _c of 158°C.     

Ferroelectric, dielectric and piezoelectric properties of Pb1?xCex(Zr0.60Ti0.40)O3, 0?≤?x?≤?0.08

The ferroelectric, dielectric and piezoelectric properties of compositions Pb_1−x Ce _x (Zr_0.60Ti_0.40)O₃, (x = 0.0, 0.01, 0.02, 0.04, 0.06 and 0.08) are studied. The above compositions are prepared from their constituent oxides, calcined at 900 °C for 4 h and various phases present are characterized by X-ray diffraction (XRD) technique. The above powders are uniaxially pressed into circular compacts, sintered at 1,250 °C for 2 h, electroded, poled at 2 kV/mm D.C. voltage and their electrical properties are measured. The XRD analysis shows the presence of rhombohedral phase up to 2 mol% ceria while tetragonal phase found at higher concentrations. It is observed that the ferroelectric, dielectric and piezoelectric properties increase with the addition of ceria with a maximum at 2 mol% and then decreases. The higher piezo properties associated with low ceria concentration are attributed to rhombohedral phase.     

Crystallite structure,microstructure, dielectric,and piezoelectric properties of (Pb1.06−xBax)(Nb0.94Ti0.06)2O6 piezoelectric ceramics prepared using calcined powders with different phases

In an attempt to obtain dense lead metaniobate-based ceramics with improved dielectric and piezoelectric properties, the (Pb_1.06−xBa_x)(Nb_0.94Ti_0.06)₂O₆ (x = 0, 0.04, 0.08, 0.12) piezoelectric ceramics were prepared separately from the two kinds of calcined powders, i.e., the powders with the rhombohedral phase and orthorhombic phase. For obtaining the calcined powders with the different phases, two different calcination temperatures of 900 °C and 1250 °C were chosen. The calcined powders were characterized using X-ray diffraction, scanning electron microscope, laser particle size analyzer and differential scanning calorimetry. Effects of the phase structures of the calcined powders on crystallite structure, microstructure, dielectric and piezoelectric properties of the ceramics were studied in detail. The lattice parameters and grain size of the ceramics are related to the phase structures of the calcined powders. The doping of Ba²⁺ has an influence on the dielectric and piezoelectric properties of the ceramics. The ceramics with x = 0.08 fabricated from the calcined powders with the orthorhombic phase demonstrate the optimum dielectric and piezoelectric properties.     

11B NMR Study of Pure and Lightly Carbon-Doped MgB2 Superconductors

We report a ¹¹B NMR line shape and spin-lattice relaxation rate (1/(T₁T))(1/(T_1T)) study of pure and lightly carbon-doped MgB_2-xC_x_{2-x}{\rm C}_x for x = 0,0.02x = 0,0.02, and 0.04, in the vortex state and in magnetic field of 23.5 kOe. We show that while pure MgB₂_2 exhibits the magnetic field distribution from superposition of the normal and the Abrikosov state, slight replacement of boron with carbon unveils the magnetic field distribution of the pure Abrikosov state. This indicates a considerable increase of H^c_c2H^c_{c2} with carbon doping with respect to pure MgB₂_2. The spin-lattice relaxation rate 1/(T₁T)1/(T_1T) demonstrates clearly the presence of a coherence peak right below T_cT_{\rm c} in pure MgB₂_2, followed by a typical BCS decrease on cooling. However, at temperatures lower than ?\approx 10 K strong deviation from the BCS behavior is observed, probably from residual contribution of the vortex dynamics. In the carbon-doped systems both the coherence peak and the BCS temperature dependence of 1/(T₁T)1/(T_1T) weaken, an effect attributed to the gradual shrinking of the σ hole cylinders of the Fermi surface with electron doping.     

Synthesis and Optical Studies of Superconducting MgB2 Thin Films

Synthesis and optical transmission of MgB₂ thin films on optically transparent glass are reported. In the 400–1000 nm regime as deposited films show high metallic reflectivity and very little transmission. After deposition, the films were annealed ex situ and rendered superconducting with T _c of 38 K, approaching that of the bulk material. The reaction conditions where quite soft ∼10 min at 550°C. The optical absorption coefficient, α and photon energy, E followed a Tauc-type behavior, = _T (E - E_g )(\alpha E)^{1/2} = \beta _T (E - E_{\rm g} ). The band gap (E _g) was observed to peak at 2.5 eV; but, the slope parameter β _T behaved monotonically with reaction temperature. Our results indicate that an intermediate semiconducting phase is produced before the formation of the superconducting phase; also optical measurements provide valuable information in monitoring the synthesis of MgB₂ from its metallic constituents. In addition these films have interesting optical properties that may be integrated into optoelectronics.     

Influence of sintering temperature on piezoelectric properties of (K0.4425Na0.52Li0.0375)(Nb0.8925Sb0.07Ta0.0375)O3 lead-free piezoelectric ceramics

Microstructure characteristics, phase transition, and electrical properties of (K_0.4425Na_0.52Li_0.0375) (Nb_0.8925Sb_0.07Ta_0.0375)O₃ (KNLNST) lead-free piezoelectric ceramics prepared by normal sintering were investigated with an emphasis on the influence of sintering temperature. The microstructure and piezoelectric, ferroelectric, and dielectric properties were investigated, with a special emphasis on the influence of sintering temperature from 1,100 to 1,140 °C. Orthorhombic phases mainly exist in the ceramics sintered at 1,100–1,130 °C, whereas the tetragonal phase becomes dominant when sintering temperature is above 1,130 °C. Because of the existence of MPB-like transitional behavior, the piezoelectric coefficient (d ₃₃), electromechanical coupling coefficient (kp), and dielectric constant (ε) show peak values of 304pC/N, 0.48, and 1,909, respectively, which are obtained in the sample sintered at 1,120 °C, and its Curie temperature (T _C) is about 271 °C.     

Studies on electrical properties of ( x ) BaTiO3?+?(1? x ) Ni0.92Co0.03Mn0.05Fe2O4 ME composites

The (1−x) Ni_0.92Co_0.03Mn_0.05Fe₂O₄ + (x) BaTiO₃ magnetoelectric (ME) composite have been prepared using conventional double sintering ceramic process where x varies as 1.00, 0.85, 0.70, 0.55 and 0.00. The presence of both phases has been confirmed by X-ray diffraction and the microstructure study will be carried out by SEM technique. The dc resistivity and thermo-emf of the samples have been studied with variation in temperature. The variation of dielectric constant (έ) and loss tangent (tan δ) will be measured in the frequency range 100 Hz–1 MHz. The ac conductivity has been derived from dielectric constant (έ) and loss tangent (tan δ). The static value of magnetoelectric conversion factor dc (ME)_H has been studied as a function of intensity of magnetic field.     

Characterization and corrosion behavior of NiTi-Ti2Ni-Ni3Ti multiphase intermetallics produced by vacuum sintering

An in-situ synthesis method was employed to produce NiTi-Ti₂Ni-Ni₃Ti multiphase intermetallics. In this regard, the amorphous/nanocrystalline Ni-Ti powders were sintered at 1300 °C for 2 hrs to obtain Ni-Ti alloys with dense structure. Tafel polarization tests were employed to study corrosion behavior of multiphase materials in 3.5% NaCl and 0.1 M H₂SO₄ corrosive media. The results indicated that the microstructure of sintered samples consists of NiTi(Fe) and Ti₂Ni/Ti₄Ni₂O_x phases embedded in a Ni₃Ti matrix. The synthesized multiphase materials had microhardness up to 873 HV1 kg.Further investigations showed the corrosion performance of multiphase samples in 3.5% NaCl solution was inferior to that of wrought NiTi alloy. In contrast, the corrosion resistance of multiphase samples in 0.1 M H₂SO₄ solution was comparable to that of wrought NiTi alloy.     

Structure and superconducting properties of pure and variously doped bulk MgB2 obtained by uniaxial and isostatic hot pressing

The preparation of dense MgB₂ bodies, undoped and doped with different atomic species (Na, Ag, Y), was performed via reactive sintering by uniaxial and isostatic hot pressing, starting from the pure elements, and compared with undoped samples obtained by commercial MgB₂ powder. The superconducting characteristics of the obtained materials, namely critical temperature (T_c) and current (J_c), were obtained through ac susceptibility measurements and compared to their structural features, like phase purity and secondary phases formation and distribution in the MgB₂ matrix. Both the adopted hot pressing techniques gave rise to undoped MgB₂ pieces exhibiting phase purity in the range 85–95% and relative density above 80%; although in most cases the doped samples underwent higher extents of phase decomposition and lesser densification, they all exhibited higher critical temperature and current compared to the corresponding undoped material, indicating a net influence of the doping on the superconducting behaviour of MgB₂, particularly Ag and Y. An opportune quality factor was adopted, to obtain a more reliable comparison between the different MgB₂ samples and evaluation of the samples goodness, in relation to their superconducting characteristics. It was put in evidence that low amounts of doping can improve the superconducting behaviour of MgB₂ and that this influence can be addressed in terms of pinning centres, as there was no experimental evidence of an actual atomic substitutions in the MgB₂ crystal.     

Electrical properties of sintered EuTiO3  EuNbO3

Two-phase sintered products [yEuTiO₃ + (1?y)EuNbO₃] were investigated as electrical-resistor materials. Electrical resistivities of the products did not depend on y in the range 0 < y < 0.96, and rapidly increased with increasing y over y = 0.96. The sintered products were metallic conductors from y = 0 to y = 0.96, and were semiconductors at y > 0.96. Thermal coefficients of resistivity for sintered products varied continuously with y, and became a maximum of 2.8 × 10^?3 K^?1 at y = 0.75 and a minimum around y = 1.00. The coefficient was positive at y < 0.96 and negative at y > 0.96. The absolute value of the thermal coefficient of resistivity minimized, namely ($\text{1}\text{?}$) ($\text{d}\text{?}\text{dT}\text{) = 0}$, at y = 0.96.     

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.     

Structural evolution of the Ti70Ni15Al15 powders prepared by mechanical alloying

Amorphization and crystallization behaviors of Ti₇₀Ni₁₅Al₁₅ powders during mechanical alloying (MA) and subsequent heat treatments are studied. Amorphous phase that cannot be obtained in the rapidly quenched ribbon is formed in the powders after MA for 60 h. Upon continuous heating of the amorphous powders in DSC, two exothermic events are observed. The first exothermic event corresponds to the crystallization of the amorphous matrix into a supersaturated α-Ti phase of hexagonal close-packed structure. The growth kinetic of the α-Ti phase is sluggish, resulting in the formation of nanostructured α-Ti matrix. The second exothermic event corresponds to the solid state transformation of the meta-stable α-Ti into the equilibrium phases, Ti₂Ni and Ti₃Al. Using the amorphous powders, Ti-based bulk materials with novel microstructures can be developed for structural applications.