Microstructure of Ba1−xLaxTiO3−δ ceramics sintered by Spark Plasma Sintering

Nano-sized Ba_1−xLa_xTiO₃ (0.00 ≤ x ≤ 0.14) powders were prepared by a coprecipitation method and calcined at 850 °C in air. The corresponding ceramics were obtained by Spark Plasma Sintering (SPS) at 1050 °C. These ceramics are oxygen deficient and are marked as Ba_1−xLa_xTiO_3−δ. Both powders and ceramics were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). The effect of lanthanum concentration on the densification behavior, on the structure and the microstructure of the oxides was investigated. Average grain sizes are comprised between 54 (3) nm and 27 (2) nm for powders, and 330 (11) nm and 36 (1) nm for ceramics according to the La-doping level. Powders crystallize in the cubic (or pseudo-cubic) perovskite phase. The structure of ceramics consists in a mixture of cubic (or pseudo-cubic) and tetragonal perovskite type phases. As the lanthanum content increases, the tetragonality of the samples decreases, as well as the grain size.     

The reliability of thermocouples in microwave ceramics processing.

It is not rare to hear arguments against the use of thermocouples for taking temperatures in processes that are taking place under microwave fields. However, the simplicity of this device makes it attractive to consider its use. One question that arises when thermocouples are employed is whether the electric field perturbs the measurement, and if the thermocouple affects the processing. The process that was chosen for conducting this test was the synthesis of spinel (MgAl2O4) using microwaves as a power supply and hematite (Fe2O3) as an additive for both spinel formation promotion and susceptor. The alumina-based systems are very important to study because this is one of the most common ingredients in refractory materials. There are many discussions about the improvement of the process when microwaves are used, but a kinetic comparison cannot be performed if the temperature is unknown, and that is the reason for emphasizing the measurement techniques. The analysis of the obtained samples was carried out by X-ray diffraction of powders. The results of this work show that there is no difference between the products obtained when the thermocouple was inserted in the system, compared to processing without it; hence the thermocouple is appropriate for this application.     

Stabilization of α-BiFeO3 structure by Sr2+ and its effect on multiferroic properties

We report a study on the effect of the substitution of Bi³⁺ by Sr²⁺ on the stabilization of R3c structure of Bi_1?xSr_xFeO₃ (0 ≤ x ≤ 0.3, Δx = 0.05), and its effect in the magnetic and dielectric behavior. Stoichiometric mixtures of Bi₂O₃, Fe₂O₃ and SrO were mixed and milled for 5?h using a ball to powder weight ratio of 10:1 by high-energy ball milling. The obtained powder were pressed at 900?MPa to obtain cylindrical pellets and sintered at 800?°C for 2?h. X-ray diffraction and Rietveld refinement were used to evaluate the effect of Sr²⁺ on the crystal structure. In addition, vibrating sample magnetometry (VSM) and dielectric tests were used for describing the multiferroic behavior. The results show that Sr-doped BiFeO₃ particles present rhombohedral structure (R3c) characteristic of α-BiFeO₃ when the doping is below 0.10?mol of Sr. Additionally, a gradual decrease in the amount of secondary phases with the increase of the amount of strontium is observed. For doping concentration higher than 0.15?mol of Sr, a phase transition to an orthorhombic symmetry (β-BiFeO₃, Pbnm) is detected. Besides, changes in relative intensities of reflection peaks planes (110) and (104) are associated with the phase transformations and with the magnetic and dielectric behavior. The α-BiFeO₃ phase show antiferromagnetic behavior and high values of dielectric permittivity, whereas the β-BiFeO₃ phase show a ferromagnetic behavior and low dielectric permittivity.     

Co-fired AlN–TiN assembly as a new substrate technology for high-temperature power electronics packaging

New wide-band gap semiconductors (SC) for power electronics such as SiC, GaN and diamond will allow higher power densities, leading to higher operating temperatures. However, the surrounding materials will also undergo an increase in temperature, meaning that a parallel effort is needed in SC packaging technologies research. One of the essential components, the substrate, is used to insulate electrically the SC from the rest of the system, drain the generated heat and provide a path to connect the SC to the rest of the system. Direct bonded copper (DBC) and active metal-brazed (AMB) substrates have limited temperature and cycling operation, owing to the large differences in the thermal expansion coefficients between the ceramics and the metals. In this work we propose a new and original substrate technology based on two co-sintered ceramics: an insulating ceramic (AlN) and a conductive one (TIN). The microstructure, the chemical compatibility and the electrical properties indicate that the proposed substrate could operate at a temperature above 200 °C the current substrate technologies, which makes it particularly attractive for high-temperature power electronics applications.     

Colossal dielectric permittivity of BaTiO3-based nanocrystalline ceramics sintered by spark plasma sintering

In pursuit of high permittivity materials for electronic application, there has been a considerable interest recently in the dielectric properties of various perovskite oxides like calcium copper titanate or lanthanum doped barium titanate. When processed in a particular way, this later material present at ambient temperature and at f?=?1 kHz unusual interesting dielectric properties, a so called “colossal” permittivity value up to several 10⁶ with relatively low dielectric losses. Moreover and contrary to what is classically expected and evidenced for this type of materials, no temperature dependence is observed. This behavior is observed in nanopowders based ceramics. An assumption to explain the observed properties is proposed. These results have important technological applications, since these nanoceramics open a new route to the fabrication of very thin dielectric films.     

Polymeric synthesis of silicon carbide with microwaves.

The aim of this work is conducting polymeric synthesis with microwaves for producing beta-SiC. A polymeric precursor was prepared by means of hydrolysis and condensation reactions from pheniltrimethoxysilane, water, methanol, ammonium hydroxide and chloride acid. The precursor was placed into a quartz tube in vacuum; pyrolysis was carried out conventionally in a tube furnace, and by microwaves at 2.45 GHz in a multimode cavity. Conventional tests took place in a scheme where temperature was up to 1500 degrees C for 120 minutes. Microwave heating rate was not controlled and tests lasted 60 and 90 minutes, temperature was around 900 degrees C. Products of the pyrolysis were analyzed by means of x-ray diffraction; in the microwave case the diffraction patterns showed a strong background of either very fine particles or amorphous material, then infrared spectroscopy was also employed for confirming carbon bonds. In both processes beta-SiC was found as the only produced carbide.