Iron oxide nanoparticles have received remarkable attention in different applications. For biomedical applications, they need to possess suitable core size, acceptable hydrodynamic diameter, high saturation magnetization, and reduced toxicity. Our aim is to control the synthesis parameters of nanostructured iron oxides in order to obtain magnetite nanoparticles in a single step, in environmentally friendly conditions, under inert gas atmosphere. The physical–chemical, structural, magnetic, and biocompatible properties of magnetite prepared by hydrothermal method in different temperature and pressure conditions have been explored. Magnetite formation has been proved by Fourier-transform infrared spectroscopy and X-ray diffraction characterization. It has been found that crystallite size increases with pressure and temperature increase, while hydrodynamic diameter is influenced by temperature. Magnetic measurements indicated that the magnetic core of particles synthesized at high temperature is larger, in accordance with the crystallite size analysis. Particles synthesized at 100 °C have nearly identical magnetic moments, at 20 × 103 μB, corresponding to magnetic cores of 10–11 nm, while the particles synthesized at 200 °C show slightly higher magnetic moments (25 × 103 μB) and larger magnetic cores (13 nm). Viability test results revealed that the particles show only minor intrinsic toxicity, meaning that these particles could be suited for biomedical applications.
Monazite is one of the most valuable natural resources for rare earth oxides (REOs) used as dopants with high added value in ceramic materials for extreme environments applications. The complexity of the separation process in individual REOs, due to their similar electronic configuration and physical–chemical properties, is reflected in products with high price and high environmental footprint. During last years, there was an increasing interest for using different mixtures of REOs as dopants for high temperature ceramics, in particular for ZrO2-based thermal barrier coatings (TBCs) used in aeronautics and energy co-generation. The use of mixed REOs may increase the working temperature of the TBCs due to the formation of tetragonal and cubic solid solutions with higher melting temperatures, avoiding grain size coarsening due to interface segregation, enhancing its ionic conductivity and sinterability. The thermal stability of the coatings may be further improved by using rare earth zirconates with perovskite or pyrochlore structures having no phase transitions before melting. Within this research framework, firstly we present a review analysis about results reported in the literature so far about the use of ZrO2 ceramics doped with mixed REOs for high temperature applications. Then, preliminary results about TBCs fabricated by electron beam evaporation starting from mixed REOs simulating the real composition as occurring in monazite source minerals are reported. This novel recipe for ZrO2-based TBCs, if optimized, may lead to better materials with lower costs and lower environmental impact, as a result of the elimination of REOs extraction and separation in individual lanthanides. Preliminary results on the compositional, microstructure, morphological, and thermal properties of the tested materials are reported.
During the microwave sintering of a polymer-ceramic composite plasma discharge is experienced. The discharge could occur failure of the power source. The solution proposed by the paper is original, no similar solutions being presented by the literature. It consists of using a polymer-ceramic composite protective panel, to stop the plasma discharge to the entrance of the guiding tunnel. Six composites resulted by combining three polymers, Polytetrafluoroethylene (PTFE), STRATITEX composite and Polyvinylchloride (PVC) with two natural ceramics containing calcium carbonate: Rapana Thomasiana (RT) sea-shells and beach sand were used to build the protective panel.Theoretical balance of the power to the panel was analysed and the thermal field was determined. It was applied heating using 0.6-1.2-1.8-2.4-3.0 kW microwave beam power. The panels were subjected to heating with and without material to be sintered. It was analyzed: RT chemical (CaCO3 as Calcite and Aragonite), burned area (range: 200–4000 mm2) and penetration (range: 1.6–5.5 mm), and thermal analysis of the burned areas comparing to the original data. PTFE-RT composite proved the lowest penetration to 0.6 and 1.2 kW. Other 1.2 kW all composites experienced vital failures. Transformation of the polymer matrix of composite consisted of slightly decreasing of the phase shifting temperature and of slightly increasing of the melting start and liquidus temperature.
Magnetic iron oxides have been used in biomedical applications, such as contrast agents for magnetic resonance imaging, carriers for controlled drug delivery and immunoassays, or magnetic hyperthermia for the past 40 years. Our aim is to investigate the effect of pressure and temperature on the structural, thermal, and magnetic properties of iron oxides prepared by hydrothermal synthesis at temperatures of 100–200 °C and pressures of 20–1000 bar. It has been found that pressure influences the type of iron oxide crystalline phase. Thus, the results obtained by Mössbauer characterization are in excellent agreement with X-ray diffraction and optical microscopy characterization, showing that, for lower pressure values (<100 bar), hematite is formed, while, at pressures >100 bar, the major crystalline phase is goethite. In addition, thermal analysis results are consistent with particle size analysis by X-ray diffraction, confirming the crystallization of the synthesized iron oxides. One order of magnitude higher magnetization has been obtained for sample synthesized at 1000 bar. The same sample provides after annealing treatment, the highest amount of good quality magnetite leading to a magnetization at saturation of 30 emu/g and a coercive field of 1000 Oe at 10 K and 450 Oe at 300 K, convenient for various applications.
Abstract. Owing to its extraordinary range of properties, yttria-doped zirconia holds a unique place among the ceramic oxide systems. To improve the properties for some specific custom design applications, co-doping with other rare earth oxides such as ceria is needed. The aim of this paper is to identify the correlations between the phase composition evolution with increasing thermal treatment temperature in order to establish the thermal stability in connection with the ceria content and how does it influence the yttria-stabilised zirconia microstructure. The ZrO 2 -3Y 2 O 3 -nCeO 2 (n = 3, 6 and 9 wt.%) samples were obtained by a hydrothermal process and submitted to a thermal treatment up to 1600°C. Intensive characterization was performed via X-ray powder diffraction and EDX analysis. It was found that up to 400°C, a monophasic structure was formed. At higher temperatures tetragonal zirconia is formed as a major phase with the presence of secondary monoclinic and cubic phases, depending on the Ce content and thermal treatment temperature. Sintered compacts with densities up to 99.5% from the theoretical density were obtained starting from the 6%CeO 2 -3%Y 2 O 3 -ZrO 2 -nanostructured powders using a special field-assisted (FAST) sintering process. With increasing CeO 2 content to 9% only, tetragonal zirconia with 6-9 nm crystallite sizes is formed during the FAST sintering process.
In this work, (Ba0.75Sr0.25) (Ti0.95Co0.05) O3 perovskite nanostructured material, denoted subsequently as Co-doped BaSrTiO3, was synthesized in a one-step process in hydrothermal conditions. The obtained powder was heat-treated at 800 °C and 1000 °C, respectively, in order to study nanostructured powder behavior during thermal treatment. The Co-doped BaSrTiO3 powder was pressed into pellets of 5.08 cm (2 inches) then used for thin film deposition onto commercial Al2O3 substrates by RF sputtering method. The microstructural, thermal, and gas sensing properties were investigated. The electrical and thermodynamic characterization allowed the evaluation of thermodynamic stability and the correlation of structural features with the sensing properties revealed under real operating conditions. The sensing behavior with respect to the temperature range between 23 and 400 °C, for a fixed CO2 concentration of 3000 ppm, highlighted specific differences between Co-doped BaSrTiO3 treated at 800 °C compared to that treated at 1000 °C. The influence of the relative humidity level on the CO2 concentrations and the other potential interfering gases was also analyzed. Two possible mechanisms for CO2 interaction were then proposed. The simple and low-cost technology, together with the high sensitivity when operating at room temperature corresponding to low power consumption, suggests that Co-doped BaSrTiO3 has a good potential for use in developing portable CO2 detectors.
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