Development of Σ3<Superscript><Emphasis Type="Italic">n</Emphasis></Superscript> CSL boundaries in austenitic stainless steels subjected to large strain deformation and annealing

The development of annealing twins was studied in chromium–nickel austenitic stainless steels subjected to cold or warm working. The annealing behavior can be characterized by an austenite reversal, recrystallization, and grain growth, depending on the deformation microstructures. The grain coarsening during recrystallization followed by a grain growth was accompanied by the development of twin-related Σ3 ⁿ CSL boundaries. The fraction of Σ3 ⁿ CSL boundaries and their density are defined by a unique parameter that is a relative change in the grain size, i.e., a ratio of the annealed grain size to that one evolved by preceding plastic working (D/D ₀). The fraction of Σ3 ⁿ CSL boundaries rapidly increased at early stage of recrystallization and grain growth while the ratio of D/D ₀ attained 5. Then, the rate of increase in the fraction of Σ3 ⁿ CSL boundaries slowed down significantly during further grain coarsening. On the other hand, the density of Σ3 ⁿ CSL boundaries increased to its maximum at a ratio of D/D ₀ about 2.5 followed by a gradual decrease during subsequent grain growth.     

Sintering behavior,phase structure and electric properties of KNNTS-BKNZ ceramics with excessive alkali metals

We investigated the effect of excessive alkali metals on sintering character, phase structure, dielectric, piezoelectric and ferroelectric properties in KNN-based ceramics thoroughly. The 0.96(K_0.48Na_0.52)_1+xNb_0.93Sb_0.02Ta_0.05O₃–0.04Bi_0.5(K_0.12Na_0.88)_0.5ZrO₃ [(KN) _x NTS-BKNZ] lead-free piezoelectric ceramics were prepared by conventional solid-state reaction method. The sintering temperature of (KN) _x NTS-BKNZ ceramics increases gradually while the sintering temperature zone becomes narrow with the increasing x value. For the composition of x?>?0.03, the grains could not grow in all sintering temperature. The coexistence system of rhombohedral and tetragonal phases has been found in (KN) _x NTS-BKNZ ceramics and the T_R?T, T_C, d₃₃, and ε_r show a upward tendency with the increasing x when 0?≤?x?≤?0.03. The maximal piezoelectric coefficient d₃₃ of 415 pC/N was obtained at x?=?0.03. In addition, these ceramics presented good temperature stability. This study exhibits that excessive alkali metals influence sintering character and electrical properties on KNN ceramics deeply. It was believed that this work would be helpful for further understanding the effect of excessive alkali metals on sintering behavior and electric properties in KNN-based ceramics.     

Effects of Ge<Superscript>4+</Superscript> acceptor dopant on sintering and electrical properties of (K<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)NbO<Subscript>3</Subscript> lead-free piezoceramics

Lead-free (K_0.5Na_0.5)(Nb_1-xGe _x )O₃ (KNN-xGe, where x = 0-0.01) piezoelectric ceramics were prepared by conventional ceramic processing. The effects of Ge⁴⁺ cation doping on the phase compositions, microstructure and electrical properties of KNN ceramics were studied. SEM images show that Ge⁴⁺ cation doping improved the sintering and promoted the grain growth of the KNN ceramics. Dielectric and ferroelectric measurements proved that Ge⁴⁺ cations substituted Nb⁵⁺ ions as acceptors, and the Curie temperature (T_C) shows an almost linear decrease with increasing the Ge⁴⁺ content. Combining this result with microstructure observations and electrical measurements, it is concluded that the optimal sintering temperature for KNN-xGe ceramics was 1020°C. Ge⁴⁺ doping less than 0.4 mol.%can improve the compositional homogeneity and piezoelectric properties of KNN ceramics. The KNN-xGe ceramics with x = 0.2% exhibited the best piezoelectric properties: piezoelectric constant d₃₃ = 120 pC/N, planar electromechanical coupling coefficient k_p = 34.7%, mechanical quality factor Q_m = 130, and tanδ = 3.6%.     

Addition of Sb<Subscript>2</Subscript>O<Subscript>5</Subscript> into MgB<Subscript>2</Subscript> Superconductor Obtained by Spark Plasma Sintering

High-density (92–98 % of the theoretical density) MgB ₂ samples added with Sb ₂ O ₅ ((MgB ₂)+ (Sb ₂ O ₅) _x ,x= 0, 0.0025, 0.005, 0.015) were obtained by Spark Plasma Sintering. A higher amount of additive decreases density. In added samples, grains of secondary phases are located at MgB ₂ grain boundaries and they are of large size. Hence, Sb ₂ O ₅ does not promote effective flux pinning, connectivity is lower, and this suppresses the critical current density and the irreversibility field. Pinning force-related parameters indicate that added samples are close to the point pinning region and they show a higher grain boundary pinning contribution when compared with pristine MgB ₂ sample and when temperature is lower. It is speculated that for fixed processing conditions and Sb-oxide phases, a lower stability of the additive, reflected by a lower melting temperature, may promote reactive processes to start earlier leading to coarsening of the grains belonging to secondary phases.     

Performance enhancement in high-<Emphasis Type="Italic">T</Emphasis><Subscript><Emphasis Type="Italic">c</Emphasis></Subscript> ceramics through melting by Joule heating,infrared lamps,and laser radiation

We have analyzed experimental data on the effect of short-term melting followed by recrystallization on the microstructure and critical current density of YBa₂Cu₃O_{7 ? x} , Bi₂Sr₂CaCu₂O_{8 ? x} , and Bi₂Sr₂Ca₂Cu₃O_{10 ? x} high-T _c ceramics. The ceramics were melted using different heat sources: infrared lamps, laser radiation, and electric current. A significant increase in the critical current density of Bi₂Sr₂Ca₂Cu₃O_{10 ? x} ceramics (by a factor of 40 at 20 K and by a factor of 8 at 77 K) was achieved using cw CO₂ laser irradiation. Melting TiC-doped (0.1%) Bi₂Sr₂Ca₂Cu₃O_{10 ? x} ceramics with a CO₂ laser, followed by annealing, insured an even larger increase in critical current density: by a factor of 35 at 77 K. We have calculated the thickness of the molten layer produced by laser heating of high-T _c ceramics.     

Very high thermal stability with excellent dielectric,and non-ohmics properties of Mg-doped CaCu<Subscript>3</Subscript>Ti<Subscript>4.2</Subscript>O<Subscript>12</Subscript> ceramics

In this work, the nominal CaCu_3?xMg_xTi_4.2O₁₂ (0.00, 0.05 and 0.10) ceramics were prepared by sintering pellets of their precursor powders obtained by a polymer pyrolysis solution method at 1100 °C for different sintering time of 8 and 12 h. Very low loss tangent (tanδ)?<?0.009–0.014 and giant dielectric constant (ε′) ～?1.1?×?10⁴–1.8?×?10⁴ with excellent temperature coefficient (Δε′) less than ±?15% in a temperature range of ??60 to 210 °C were achieved. These excellent performances suggested a potent application of the ceramics for high temperature X8R and X9R capacitors. It was found that tanδ values decreased with increasing Mg²⁺ dopants due to the increase of grain boundary resistance (R_gb) caused by the very high density of grain, resulting from the substitution of small ionic radius Mg²⁺ dopants in the structure. In addition, CaCu_3?xMg_xTi_4.2O₁₂ ceramics displayed non-linear characteristics with the significant enhancements of a non-linear coefficient (α) and a breakdown field (E_b) due to Mg²⁺doping. The high values of ε′ (14012), α (13.64) and E_b (5977.02 V/cm) with very low tanδ value (0.009) were obtained in a CaCu_2.90Mg_0.10Ti_4.2O₁₂ ceramic sintered at 1100 °C for 8 h.     

Improved electrical properties of Co-doped 0.92NBT–0.04KBT–0.04BT lead-free ceramics

The (1???2x)NBT–xKBT–xBT ternary piezoelectric system has been extensively studied in recent years. However, its electrical performance is far inferior to lead-based counterparts, and could not meet the requirements for practical applications. In this contribution, the 0.92NBT–0.04KBT–0.04BT (abbreviated as NKBT4) ceramics were prepared by traditional solid-state method. The effects of doped cobalt content on the structure and electrical performance of NKBT4 ceramics were studied systematically. The content of Co₂O₃ affects the average grain size, maximum dielectric constant, piezoelectric properties and the ferroelectric responses of the ceramics. It was found that the introduction of cobalt did not affect the phase structure of the ceramics, but is beneficial for the improvement of the dielectric and piezoelectric properties. When x?=?0.2, the piezoelectric coefficient (d₃₃) is around 130 pC/N, which is greatly improved compared to pure NKBT4 ceramics. Besides, a relatively high dielectric constant (ε_r?=?1150) was obtained at the same composition. This work paves a new way for the further development of high performance lead-free piezoelectric ceramics.     

Effects of Nb doping on the microstructure,ferroelectric and piezoelectric properties of 0.7BiFeO<Subscript>3</Subscript>–0.3BaTiO<Subscript>3</Subscript> lead-free ceramics

Donor-doped lead-free Bi_0.7Ba_0.3(Fe_0.7Ti_0.3)_1?x Nb_0.66x O₃ + 1 mol% MnO₂ ceramics were prepared by a conventional oxide-mixed method and the effects of Nb-doping on microstructure, piezoelectric and ferroelectric properties of the ceramics were investigated. All the ceramics exhibit a pure perovskite structure with rhombohedral symmetry. The grain growth of the ceramics is inhibited after the addition of Nb doping. High electric insulation (R = 10⁹–10¹⁰ Ω?cm) and the poor piezoelectric performance and weak ferroelectricity are observed after the addition of Nb₂O₅ in the ceramics. Different from the donor effect of Pb-based perovskite ceramics, the introduction of Nb into 0.7BiFeO₃–0.3BaTiO₃ degrades the piezoelectricity and ferroelectricity of the ceramics. The Bi_0.7Ba_0.3(Fe_0.7Ti_0.3)_1?x Nb_0.66x O₃ + 1 mol% MnO₂ ceramic with x = 0 exhibits the optimum piezoelectric properties with d ₃₃ = 133 pN C^?1 and k _p = 0.29 and high Curie temperature (T_C = 603^°C).     

Effect of sintering temperature on microstructures and microwave dielectric properties of Ba<Subscript>2</Subscript>MgWO<Subscript>6</Subscript> ceramics

The microwave dielectric properties of Ba₂MgWO₆ ceramics were investigated with a view to the use of such ceramics in mobile communication. Ba₂MgWO₆ ceramics were prepared using the conventional solid-state method with various sintering temperatures. Dielectric constants (? _r ) of 16.8–18.2 and unloaded quality factor (Q _u  × f) of 7000–118,200 GHz were obtained at sintering temperatures in the range 1450–1650 °C for 2 h. A maximum apparent density of 6.76 g/cm³ was obtained for Ba₂MgWO₆ ceramic, sintered at 1650 °C for 2 h. A dielectric constant (? _r ) of 18.4, an unloaded quality factor (Q _u  × f) of 118,200 GHz, and a temperature coefficient of resonant frequency (τ _f ) of ?34 ppm/°C were obtained when Ba₂MgWO₆ ceramics were sintered at 1650 °C for 2 h.     

Effect of MoO<Subscript>3</Subscript> Addition on the Magnetic Properties and Complex Impedance of Mn–Zn Ferrites with High <Emphasis Type="Italic">B</Emphasis><Subscript><Emphasis Type="Bold">s</Emphasis></Subscript> and High Initial Permeability

Mn–Zn ferrites with high initial permeability (μ _i) and high saturation magnetic flux density (B _s) were successfully synthesized by using a conventional ceramic processing route with addition of MoO₃. The structure, morphology, magnetic properties, and complex impedance of all samples were investigated by X-ray diffraction, scanning electron microscopy, DC magnetic instrument, and precision LCR meter. The addition of MoO₃ promotes the growth of larger and more uniform grains and therefore enhances the μ _i. Meanwhile, it improves the density and hence the B _s. Through the analysis of complex impedance spectra by an equivalent circuit model, it is demonstrated that MoO₃ mainly exists at grain boundaries and improves the impedance in a wide frequency range.     

The Effect of <Emphasis Type="Italic">Ar</Emphasis> Ambient Pressure and Annealing Duration on the Microstructure,Superconducting Properties and Activation Energies of MgB<Subscript>2</Subscript> Superconductors

MgB₂ samples are produced by ex situ reaction method under vacuum, and various (0, 10, 20 Bar) Ar pressure for 0.5 and 1 h. The effect of ambient pressure and annealing duration on the microstructure and electrical properties of bulk samples are investigated. XRD, SEM, and magnetoresistance measurements are made. The a and c lattice parameters and the grain size values are the highest for the samples produced under vacuum and their values decrease with increasing Ar pressure. Moreover, these values increase when the annealing duration increases from 0.5 to 1 h. The increasing pressure reduces the bond lengths between the atoms thus the grain sizes decrease. Smaller grain size promotes the connection between grains which results in an increase of the critical current density (J _c ). SEM micrographs reveal that the produced samples have granular structure which is a characteristic feature of MgB₂. The decrease of grain sizes and thus enhancement in grain connectivity with increasing pressure is also confirmed by SEM images. Magneto resistivity measurements show that T _c values of the samples produced under vacuum are the highest. T _c values decrease with increasing ambient pressure and applied magnetic field. The activation energies (U ₀) of the samples are calculated using Arrhenius plots due to thermally activated flux flow theory. Existence and increase of Ar pressure causes increase of activation energies. The samples produced with 0.5-h annealing have higher activation energies than the ones produced with 1-h annealing.     

Influence of Nd doping on microwave dielectric properties of SrTiO<Subscript>3</Subscript> ceramics

Sr_1?x Nd _x TiO₃ (x?=?0.08–0.14) ceramics were prepared by conventional solid-state methods. The analysis of crystal structure suggested Sr_1?x Nd _x TiO₃ ceramics appeared to form tetragonal perovskite structure. The relationship between charge compensation mechanism, microstructure feature and microwave dielectric properties were investigated. Trivalent Nd³⁺ substituting Sr²⁺ could effectively decrease oxygen vacancies. This reduction and relative density were critical to improve Q?×?f values of Sr_1?x Nd _x TiO₃ ceramics. For ε _r values, incorporation of Nd could restrain the rattling of Ti⁴⁺ cations and led to the reduction of dielectric constant. The τ _f values were strongly influenced by tilting of oxygen octahedral. The τ _f values decreased from 883 to 650 ppm/°C with x increasing from 0.08 to 0.14. A better microwave dielectric property was achieved for composition Sr_0.92Nd_0.08TiO₃ at 1460 °C: ε _r ?=?160, Q?×?f?=?6602 GHz, τ _f ?=?883 ppm/°C.     

Effects of <Emphasis Type="Italic">β</Emphasis>-Sn grain <Emphasis Type="Italic">c</Emphasis>-axis on electromigration behavior in BGA Sn3.0Ag0.5Cu solder interconnects

The anisotropy of β-Sn grain can significantly affect the electromigration (EM) behavior in Sn3.0Ag0.5Cu (SAC305) solder interconnects. A real ball grid array (BGA) specimen with a cross sectioned edge row suffered electromigration for 600 h to investigate the effects of β-Sn c-axis on the behavior of electromigration in SAC305 solder interconnects. Scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD) were used to obtain the microstructure and orientation of β-Sn grains in as-reflowed and low current density conditions. Besides, the orientation of c-axis had a great effect on the growth direction of IMCs in solder matrix. The solder interconnect with the Sn grain c-axis pointing the positive direction of ND would emerge serious electromigration phenomena. The density of Cu₆Sn₅ IMCs distributing at the surface of solder matrix increased obviously. However, when Sn grain c-axis was in the same direction with the opposite direction of ND, the original Cu₆Sn₅ IMCs in as-reflowed solder interconnect disappeared. Therefore, the results show that the solder interconnects will performance a different electromigration behavior due to the direction of c-axis in Sn grain: the growth direction of Cu₆Sn₅ IMCs in solder matrix will along the c-axis accompanied growing into solder matrix or gathering at the surface of the cross section.     

Effect of strong gravitational field on oriented crystalline perovskite-type manganese oxide La<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Sr<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>MnO<Subscript>3</Subscript>

We report the effect of a strong gravitational field on oriented crystalline perovskite-type manganese oxide La_1?x Sr _x MnO₃ (LSMO). The perovskite-type manganese oxides La_1?x Sr _x MnO₃ (LSMO) have been investigated for giant magnetoresistance (GMR) by controlling the hole-doping level (x). A strong gravitational field can change in crystalline state and the enhancement of usual diffusion. We subjected oriented crystalline La_1?x Sr _x MnO₃ with different grain and grain-boundary (GBs) Sr concentrations to a strong gravitational field and investigated the resulting changes in the A-site cation diffusion and physical properties of the material. Electron probe micro-analysis (EPMA) results showed appearance of the GBs where the Sr concentration was quite high compared with in other GBs. The quantitative analysis at the grain and GBs indicated that cation diffusion was more enhanced than the annealed one. The temperature dependence of the magnetic susceptibility of the gravity samples changed with the Sr concentration in the grains. The temperature dependence of the resistivity curves of the gravity sample showed several abrupt changes, which corresponded to phase transitions at the grains and GBs, which may be caused by composition changes.     

Thermoelastic martensitic transformations in ternary Ni<Subscript>50</Subscript>Mn<Subscript>50–<Emphasis Type="Italic">z</Emphasis></Subscript>Ga<Subscript><Emphasis Type="Italic">z</Emphasis></Subscript> alloys

We have studied the effect of gallium alloying on the structure, phase composition, and physical properties of ternary alloys of the Ni₅₀Mn_50–z Ga _z (0 ≤ z ≤ 25 at %) quasi-binary section in a broad temperature range. Dependences of the type of crystalline structure of the high-temperature austenite phase and martensite, as well as the critical temperatures of martensitic transformations on the alloy composition, are determined. A phase diagram of the structural and magnetic transformations is constructed. Concentration boundaries of the existence of tetragonal L1₀ (2M) martensite and martensitic phases (10M and 14M) with complex multilayer crystalline lattices are found. It is established that the predominant martensite morphology is determined by the hierarchy of packets of thin coherent nano- and submicrocrystalline plates with habit planes close to {011} _B2, pairwise twinned along one of 24 equivalent {011}<011> _B2 twinning shear systems.     

Preparation,structure and microwave dielectric properties of 3MgO–Al<Subscript>2</Subscript>O<Subscript>3</Subscript>–3TiO<Subscript>2</Subscript> ceramics

3MgO–Al₂O₃–3TiO₂ (MAT) ceramics were prepared by a conventional solid-state reaction method. The crystal structure, sintering behavior and microwave dielectric properties of ceramics were investigated using X-ray diffraction, scanning electron microscopy and network analyzer. MAT ceramics contained the coexistence of three phases, including MgAl₂O₄, MgTiO₃ and MgTi₂O₅. The ceramics sintered at 1350 °C for 4 h presented excellent comprehensive performances with relative permittivity (ε _r ) of 15.4, quality factor (Q × f) of 91,000 GHz and temperature coefficient of resonant frequency (τ _f ) about ?55.1 ppm/°C.     

Effect of Oxygen Pressure on the Surface Roughness and Intergranular Behavior of YBCO Thin Films

YBa₂Cu₃ O _7?δ (YBCO) thin films were deposited by pulsed laser deposition on single-crystal LaAlO₃ (100) substrates in O₂ partial pressure (P _O2) from 400 to 500 mTorr. The XRD data shows the presence of a-axis-oriented grains in the YBCO films deposited at P _O2 = 500 mTorr. The a-axis grains lead to increase of strain. Atomic force microscopy images show as oxygen pressure has increased, average surface roughness of the films and size of droplets were increased. The grain misorientaion could be the reason for high average roughness. However, surface analysis by statistical methods reveals that three surfaces have multi-affine structure irrespective of oxygen pressure. Analysis of the temperature dependence of the AC susceptibility near the transition temperature indicates that with increasing oxygen pressure, intergranular critical current density has decreased. It is also suggested that the nature of weak links in the samples is of superconductor-normal-superconductor (SNS) type irrespective of the oxygen pressure.     

Structure,dielectric and ferroelectric properties of lead free (K,Na)(Nb)O<Subscript>3</Subscript>-xBiErO<Subscript>3</Subscript> piezoelectric ceramics

The effect of BiErO₃ (BE) as a doping material on the structural, dielectric and ferroelectric properties of (KNa)NbO₃ ceramics was explored in this research. Co-existence of two phase regions was confirmed in the composition range at x?=?0.5% and x?=?1.0%. The addition of BE content led to a decrease of the grain size and the ceramics became denser. Bulk P–E hysteresis loops were obtained with a maximum polarization of P _max = 30.56 µC/cm² and a remnant polarization of P _r = 25.10 µC/cm², along with a coercive field of E _c  ~ 11.26 kV/cm. The results revealed that a field strain value of ~?0.26 for x?=?0.5% of BE substitution was attained. This presents outstanding piezoelectric and dielectric properties.     

Influence of the Preparation Conditions and Percolation Threshold on the Properties of Lead Zirconate Titanate/Cobalt Nickel Ferrite Magnetoelectric Composites

We have prepared magnetoelectric (ME) composite ceramics, free of foreign phases, in the lead zirconate titanate–cobalt nickel ferrite two-phase system: xPZT-36 + (100–x)Ni_0.9Co_0.1Fe₂O₄. The sol–gel derived ferrite powder used in our preparations seems to be doped with titanium cations from the PZT-36. The ceramics have a percolation threshold at x = 50–70 wt %, which is due to the increased electrical conductivity of Ni_0.9Co_0.1Fe₂O₄. As a consequence, the piezoelectric parameters of the ME ceramics drop sharply at x < 50–70 wt %: the piezoelectric moduli |d_ij| and piezoelectric voltage coefficients |g_ij| decrease by a factor of 3–5 in this composite range. The piezoelectric parameters |d_ij| and |g_ij| of the composites produced using the fine ferrite powder exceed those of the materials prepared using macrocrystalline Ni_0.9Co_0.1Fe₂O₄ powder by more than a factor of 2. The piezoelectric voltage coefficient g33 correlates with the ME coefficient ΔE/ΔH. The highest ME conversion efficiency (up to 45 mV/(cm Oe)) is offered by the 80 wt % PZT-36 + 20 wt % Ni_0.9Co_0.1Fe₂O₄ composites, whose composition lies in a subpercolation region. Even though the composites produced using the fine ferrite powder possess improved piezoelectric properties, they have smaller ΔE/ΔH coefficients (no greater than 25 mV/(cm Oe)), which can be tentatively attributed to the degradation of the properties of the ferrite as a consequence of doping with Ti⁴⁺ cations during the sintering of the composite ceramics.     

Low temperature sintering and microwave dielectric properties of Li<Subscript>6</Subscript>Mg<Subscript>7</Subscript>Ti<Subscript>3</Subscript>O<Subscript>16</Subscript> ceramics with LiF additive for LTCC applications

Li₆Mg₇Ti₃O₁₆ ceramics were prepared by the conventional solid-state method with 1–5 wt% LiF as the sintering aid. Effects of LiF additions on the phase compositions, sintering characteristics, micro-structures and microwave dielectric properties of Li₆Mg₇Ti₃O₁₆ ceramics were investigated. The LiF addition could effectively lower the sintering temperature of Li₆Mg₇Ti₃O₁₆ ceramics from 1550 to 900 °C. For different LiF-doped compositions, the optimum dielectric permittivity (ε _r ) and quality factor (Q·f) values first increased and then decreased with the increase of LiF contents, whereas the temperature coefficient of resonant frequency (τ _f ) fluctuated between ??14.39 and ??8.21 ppm/°C. Typically, Li₆Mg₇Ti₃O₁₆ ceramics with 4 wt% LiF sintered at 900 °C exhibited excellent microwave dielectric properties of ε _r ?=?16.17, Q·f?=?80,921 GHz and τ _f ?=???8.21 ppm/°C, which are promising materials for the low temperature co-fired ceramics applications.