Investigation on external stimuli engendered magnetic ordering in polycrystalline CaCu3Ti4O12 quadruple perovskite

The consequences of high energy mechanical milling, microwave-assisted heating and rapid thermal cooling on magnetic ordering in polycrystalline CaCu₃Ti₄O₁₂ cubic perovskite have been investigated by means of X-ray powder diffractometry (300?K), dc magnetization in field – cooled and zero – field cooled modes (H = 100?Oe and 1000?Oe, T?=?5–300?K) (M – T curves) and M – H loop characteristics (T?=?5?K and 300?K, H_max = 70?kOe). The M – T curves of unmilled and 16?h milled samples show pure antiferromagnetic and weak ferromagnetic ordering, respectively, 1?h and 6?h milled samples demonstrate the coexistence of both the phases while microwave-assisted and quenched samples exhibit classic antiferromagnetic transition and a low temperature paramagnetic–like contribution with different weights, well supported by the M – H loop characteristics. The observed transformations in the magnetic ordering are attributed to the ball-milling induced stress which curtails hybridization of empty Ti-3d orbitals with Cu-3d and O-2p orbitals and secondary phase formation. Oxygen vacancies associated with bound magnetic polarons originate ferromagnetism in the milled samples while unpaired electrons inhabited at the empty sites are the cause of paramagnetic centers. The low-temperature Curie – tail in M – T curve for quenched and microwave assisted samples is attributed to Ti³⁺ cations.     

Growth,microstructure, energy–storage and dielectric performances of chemical–solution NBT–based thin films: Effect of sodium nonstoichimometry

Na_0.5+δBi_0.5(Ti_0.96W_0.01Ni_0.03)O₃ thin films with various Na contents (abbreviated as Na_.5+δBTWN, δ?=?? 3.0, ??1.5, 0, 1.5%) were fabricated on ITO/glass substrates using a chemical–solution process. The effects of Na nonstoichiometry on the microstructure, insulating, ferroelectric and dielectric performances are investigated. The pure perovskite phase can be obtained in Na_0.5BTWN and Na_0.515BTWN, while for Na_0.470BTWN or Na_0.485BTWN, the main composition contains secondary phase of TiO₂. The grain size increases from 30?nm at δ?=?? 3.0% to 55?nm at δ?=?0%, then decreases to 52?nm with δ?=?1.5%. The leakage current of Na_0.485BTWN sample is reduced dramatically in comparison with Na_0.5+δBTWN (δ?=?? 3.0, 0, 1.5%). The big recoverable energy–storage density of 63.1?J/cm² and high energy–storage efficiency of 55.0% can be obtained for Na_0.485BTWN due to the improved electric break–down strength and large difference value between the remanent polarization and maximum polarization. Enhanced dielectricity is achieved in Na_0.485BTWN with a high tunability of 36.0% and a figure of merit of 4.0 at 450?kV/cm and 500?kHz. These results demonstrated that the crystallization, micrographs and energy storage and dielectric properties of Na_0.5Bi_0.5TiO₃ are highly sensitive to low levels of Na–site nonstoichiometry.     

Characterization of biogenic hydroxyapatite derived from animal bones for biomedical applications

In this work, the viability of producing biogenic hydroxyapatite from bio-waste animal bones, namely bovine (cow), caprine (goat) and galline (chicken), through a heat treatment process has been investigated. The animal bones were locally sourced, cleaned to remove collagen and subsequently heat treated in air atmosphere at different temperatures ranging from 600?°C to 1000?°C. From the range of sintering temperatures investigated, it was found that hydroxyapatite derived from bovine bone showed good thermal stability while those produced from caprine and galline bones exhibited phase instability with traces of tri-calcium phosphate (TCP) being detected after heat treatment beyond 700?°C. The porous nature of the bone samples can be observed from the microstructures obtained and supported by low relative density. Heating the bovine and caprine bones at selected temperatures yielded porous HA body, having hardness values that are comparable with human cortical bone. However, the sintered galline bone sample showed higher porosity levels and low hardness when compared to the other two bone types.     

Microwave dielectric properties of ultra-low loss Li2MgTi0.7(Mg1/3Nb2/3)0.3O4 ceramics sintered at low temperature by LiF addition

In this work, ultra-low loss Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄ ceramics were successfully prepared via the conventional solid-state method. X-ray photoelectron spectroscopy (XPS), thermally stimulated depolarization current (TSDC) and bond energy were used to determine the distinction between intrinsic and extrinsic dielectric loss in (Mg_1/3Nb_2/3)⁴⁺ ions substituted ceramics. The addition of (Mg_1/3Nb_2/3)⁴⁺ ions enhances the bond energy in unit cell without changing the crystal structure of Li₂MgTiO₄, which results in high Q·f value as an intrinsic factor. The extrinsic factors such as porosity and grain size influence the dielectric loss at lower sintering temperature, while the oxygen vacancies play dominant role when the ceramics densified at 1400?°C. The Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄ ceramics sintered at 1400?°C can achieve an excellent combination of microwave dielectric properties: ε_r =?16.19, Q·f?=?160,000?GHz and τ_f =??3.14?ppm/°C. In addition, a certain amount of LiF can effectively lower the sintering temperature of the matrix, and the Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄-3?wt% LiF ceramics sintered at 1100?°C possess balanced properties with ε_r?=?16.32, Q·f?=?145,384?GHz and τ_f =??16.33?ppm/°C.     

Infiltration behavior of Cu and Ti fillers into Ti2AlC/Ti3AlC2 composites during tungsten inert gas (TIG)brazing

Herein we study the infiltration behavior of Ti and Cu fillers into a Ti₂AlC/Ti₃AlC₂MAX phase composites using a TIG-brazing process. The microstructures of the interfaces were investigated by scanning electron microscopy and energy dispersive spectrometry. When Ti₂AlC/Ti₃AlC₂ comes into contact with molten Ti, it starts decomposing into TiC_x, a Ti-richandTi₃AlC; when in contact with molten Cu, the resulting phases are Ti₂Al(Cu)C, Cu(Al), AlCu₂Ti and TiC. In the presence of Cu at approximately 1630 °C, a defective Ti₂Al(Cu)C phase was formed having a P63/mmc structure. Ti₃AlC₂ MAX phase was completely decomposed in presence of Cu or Ti filler-materials. The decomposition of Ti₂AlC to Ti₃AlC₂ was observed in the heat-affected zone of the composite. Notably, no cracks were observed during TIG-brazing of Ti₂AlC/Ti₃AlC₂ composite with Ti or Cu filler materials.     

Synthesis and characterization of Y (In,Mn) O3 blue pigment using the complex polymerization method (CPM)

In this paper, a new synthetic pathway is proposed for the system YIn_1-xMn_xO₃, a bright blue inorganic pigment, discovered in 2009. Blue pigment samples with increasing concentration of Mn³⁺ (x?=?0.08, 0.12 and 0.16) were prepared using the complex polymerization method (CPM) and compared with those synthesized via solid state reaction. All powders, the amorphous precursor from CPM and the starting materials for solid state method, were calcined at 1000, 1100, 1200 and 1300?°C for 12?h, and the resulting blue pigments were characterized by X-ray diffraction (XRD), colorimetric system CIE L*a*b* and Near infrared (NIR) reflectance measurements. XRD patterns and Rietveld Refinement show that the lowest temperature at which single hexagonal phase (isostructural to YInO₃) is formed is 1000?°C for CPM method and 1300?°C for conventional solid state method, respectively. The L*a*b* values demonstrate that the coloration of powders prepared by CPM exhibit temperature dependence below 1300?°C, a color shade shift from grayish blue to intense deep blue is observed when heating the samples from 1000 to 1300?°C. Blue pigments obtained by CPM have smaller particle size due to low temperatures and excellent near-infrared reflectance comparable to those by solid state method. Thus, providing advantages for application process and energy efficiency.     

Effect of microwave sintering on the properties of copper oxide doped Y-TZP ceramics

The effect of various amounts of copper oxide (CuO) up to 1?wt% on the densification behaviour and mechanical properties of 3?mol% yttria-tetragonal zirconia polycrystal (Y-TZP) were studied by using microwave (MW) sintering method. The MW sintering was performed at temperatures between 1100?°C and 1400?°C, with a heating rate of 30?°C/min. and holding time of 5?min. The beneficial effect of MW in enhancing densification was also compared for the undoped and 0.2?wt% CuO-doped Y-TZP when subjected to conventional sintering (CS) method. The results showed that significant enhancement in the relative density and Vickers hardness were observed for the undoped Y-TZP when MW-sintered between 1100?°C and 1250?°C. It was revealed that the 0.2?wt% CuO-doped Y-TZP and MW sintered at 1250–1300?°C could attain ≥?99.8% of theoretical density, Vickers hardness of about 14.4?GPa, fracture toughness of 7.8 MPam^1/2 and exhibited fine equiaxed tetragonal grain size of below 0.25?µm. In contrast, the addition of 1?wt% CuO was detrimental and the samples exhibited about 50% monoclinic phase upon sintering coupled with poor bulk density and mechanical properties. The study also revealed that the addition of 0.2?wt% CuO and subjected to conventional sintering produced similar densification as that obtained for microwave sintering, thus indicating that the dopant played a more significant role than the sintering method.     

Compensation for volatile elements to modify the microstructure and energy storage performance of (W,Ni)-codoped Na0.5Bi0.5TiO3 ceramic films

This work reports the characteristics of nonstoichiometric Na_0.5+xBi_0.5+yTi_0.96W_0.01Ni_0.03O₃ (x?=?0.0%, y?=?1.0%; x?=?0.5%, y?=?2.0%; x?=?1.0%, y?=?4.0%) ceramic films derived from chemical solution deposition and the role played by excess Na/Bi in modifying microstructure and electrical properties. Single perovskite phase structure can be maintained in all compositions. Decreased grain size can be obtained with the increasing compensation for volatile Na/Bi elements. Particularly, extra amounts of 0.5?mol% Na and 2.0?mol% Bi leads to reduced leakage and enhanced ferroelectric polarization. Meanwhile, due to the high breakdown electrical field strength and large difference between maximum and remanent polarization, an excellent energy storage performance can be achieved in Na_0.505Bi_0.52Ti_0.96W_0.01Ni_0.03O₃ sample, which is distinguished by a recoverable energy storage density of 40.5?J/cm³ and an energy storage efficiency of 43.6% at 2515?kV/cm as well as a good frequency stability. Hence, the regulation for the content of volatile elements is effective to modify the electrical response of Na_0.5Bi_0.5TiO₃-based materials.     

Negative magnetization and exchange bias effect in Fe-doped CoCr2O4

Polycrystalline ceramics of Co(Cr_1-xFe_x)₂O₄ (0?≤?x?≤?0.12) were experimentally studied based on a series of temperature and time-dependent dc magnetic measurements using different magnetic field histories. Magnetization in field cooling process was continuously decreased for doping content x in the range of 0?≤?x?≤?0.04. Remarkable negative magnetization is observed when x reaches to 0.06 and persists up to x?=?0.1. Two-sublattice model is established and competition of the two magnetic sublattices is responsible for the phenomenon. The magnetic switching effect is realized just by changing the magnitude of the applied magnetic field and double magnetocaloric effects are obtained. These unique features under low magnetic fields show attractive for application in spintronic devices due to that the magnetic state can effectively be tuned through magnetic field or temperature. Besides, the system exhibits both positive and negative exchange bias fields which are considered to be originating from the unidirectional anisotropy of exchange coupling of antiferromagnetic/ferromagnetic phases and spin reorientation of the two sublattices magnetic moments, respectively.     

Effects of chemical etching on structure and properties of Y0.5Gd0.5Ba2Cu3O7-z coated conductors

Corrosion resistance is a crucial property to achieve successful superconducting joints of Y_0.5Gd_0.5Ba₂Cu₃O_7-z (YGdBCO) coated conductors (CCs). Cu and Ag metallic layers need to be fully removed from the area of conductor to be joint to allow for a superconducting path across the joint. Therefore, when using a wet etching process to remove the metallic layers, the joint performance can be significantly influenced by the etching conditions. The effects of chemical etching with ammonia water and hydrogen peroxide mixture on crystal structure, surface microstructure and critical current (I_c) of YGdBCO CCs were systematically investigated. We found the set of etching parameters that does not affect conductor performance, leaving the I_c of the YGdBCO conductor unchanged upon etching. However, when the etching conditions are not optimal, decrease in I_c was found and the underlying reasons driving the degradation were investigated. Raman spectroscopy and XRD analysis indicated that the reduced I_c is mainly due to oxygen deficiency in the YGdBCO crystal lattice.