RESUMEN
The aim of this work is to study the physical-chemical, mechanical, and biocompatible properties of hydroxyapatite obtained by hydrothermal synthesis, at relatively low temperatures and high pressures, starting from natural sources (Rapana whelk shells), knowing that these properties influence the behavior of nanostructured materials in cells or tissues. Thus, hydroxyapatite nanopowders were characterized by chemical analysis, Fourier-transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS), scanning electron microscopy (SEM), and X-ray diffraction (XRD). In vitro studies on osteoblast cell lines (cytotoxicity and cell proliferation), as well as preliminary mechanical tests, have been performed. The results showed that the obtained powders have a crystallite size below 50 nm and particle size less than 100 nm, demonstrating that hydrothermal synthesis led to hydroxyapatite nanocrystalline powders, with a Ca:P ratio close to the stoichiometric ratio and a controlled morphology (spherical particle aggregates). The tensile strength of HAp samples sintered at 1100 °C/90 min varies between 37.6-39.1 N/mm2. HAp samples sintered at 1300 °C/120 min provide better results for the investigated mechanical properties. The coefficient of friction has an appropriate value for biomechanical applications. The results of cell viability showed that the cytotoxic effect is low for all tested samples. Better cell proliferation is observed for osteoblasts grown on square samples.
RESUMEN
Carbon-based materials are promising candidates for enhancing thermal properties of phase change materials (PCMs) without lowering its energy storage capacity. Nowadays, researchers are trying to find a proper porous structure as PCMs support for thermal energy storage applications. In this context, the main novelty of this paper consists in using a ZnO-CNT-based nanocomposite powder, prepared by an own hydrothermal method at high pressure, to obtain porous 3D printed support structures with embedding capacity of PCMs. The morphology of 3D structures, before and after impregnation with three PCMs inorganic salts (NaNO3, KNO3 and NaNO3:KNO3 mixture (1:1 vol% saturated solution) was investigated by scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDX). For structure impregnated with nitrates mixture, SEM cross-section morphology suggest that the inorganic salts impregnation started into micropores, continuing with the covering of the 3D structure surface and epitaxial growing of micro/nanostructured crystals, which led to reducing the distance between the structural strands. The variation of melting/crystallization points and associated enthalpies of impregnated PCMs and their stability during five repeated thermal cycles were studied by differential scanning calorimetry (DSC) and simultaneous DSC-thermogravimetry (DSC-TGA). From the second heating-cooling cycle, the 3D structures impregnated with NaNO3 and NaNO3-KNO3 mixture are thermally stable.
RESUMEN
Recently, carbon nanotubes (CNTs) have been used extensively to develop new materials and devices due to their specific morphology and properties. The reinforcement of different metal oxides such as zinc oxide (ZnO) with CNT develops advanced multifunctional materials with improved properties. Our aim is to obtain ZnO-CNT nanocomposites by in situ hydrothermal method in high-pressure conditions. Various compositions were tested. The structure and morphology of ZnO-CNT nanocomposites were analyzed by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry-thermogravimetry (DSC-TG), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). These analyses showed the formation of complex ZnO-CNT structures. FT-IR spectra suggest possible interactions between CNT and ZnO. DSC-TG analysis also reveals the formation of some physical bonds between ZnO and CNT, through the appearance of endothermic peaks which could be assigned to the decomposition of functional groups of the CNT chain and breaking of the ZnO-CNT bonds. XRD characterization demonstrated the existence of ZnO nanocrystallites with size around 60 nm. The best ZnO:CNT composition was further selected for preliminary investigations of the potential of these nanocomposite powders to be processed as pastes for extrusion-based 3D printing.
RESUMEN
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.
RESUMEN
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.
RESUMEN
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.