Aqueous Na-ion based batteries are considered promising candidates for replacing Li-ion technologies, especially in the area of stationary energy storage. Research and development of novel electrode materials remain a central research effort in this field. NASICON-structured NaTi2(PO4)3 phosphate framework has attracted a great deal of attention and remains the most studied negative electrode material for aqueous Na-ion batteries. The active material preparation and carbon composite property tailoring play a critical role in the electrode materials engineering process which governs the performance of an entire electrochemical system. We present a study of a series of aqueous sol-gel synthesized NaTi2(PO4)3—carbon composites using three different sol-gel approaches and three distinct pyrolysis/calcination strategies. The structural and morphological analysis shows that both the sol-gel route as well as the thermal treatment strategy have significant effects on active material purity and degree of crystallinity as well as the content and properties of the carbonaceous phase. Electrochemical investigations of these composites also show strong effects of the materials structure and carbon matrix morphology on the electrochemical performance and degradation of these materials when employed as aqueous Na-ion battery negative electrodes.
Environmentally friendly alternatives to chromium—phosphate/molybdate and cerium-modified phosphate/molybdate conversion coatings—were deposited on a carbon steel surface. Different surface analytic techniques were applied to obtain complementary information on the composition, element distribution morphology and inner structure of the coatings in order to establish the relationship between coating properties and corrosion performance. The higher protective and stronger self-healing abilities were found for phosphate/molybdate/cerium conversion coating deposited in a sulphate-containing solution. The protective barrier strength was found to be related with certain aspects of the coating morphology such like homogeneous distribution of fine crystallites and, hence, lower number of structural defects. The self-healing ability depended on both, the composition (higher amount of Ce(IV)) and micro-structural characteristics, such as defectiveness, of the conversion layer.
In this study, a low-temperature synthetic approach was developed for the fabrication of calcium hydroxyapatite (CHAp) coatings on a titanium substrate. The titanium substrates were first coated with CaCO3 by a spin-coating technique using a sol–gel chemistry approach, and the obtained product was transformed into CHAp during a dissolution–precipitation reaction. The phase purity and structural and morphological features of the obtained CHAp coatings were evaluated by X-ray diffraction (XRD) analysis, FTIR spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM) and using a 3D optical profilometer. It was demonstrated that almost-single-phase CHAp formed on the titanium substrate with a negligible number of side phases, such as Na2HPO4 (starting material) and TiO2. In the Raman spectrum of the CHAp coating, the peaks of phosphate group vibrations were clearly seen. Thus, the obtained results of Raman spectroscopy correlated well with the results of X-ray diffraction analysis. The corrosive behaviour of CHAp coatings on a titanium substrate was also evaluated using electrochemical methods. It was found that the corrosion resistance of titanium coated with CHAp increased significantly. These CHAp thin films may be potential candidates for use in not only in regenerative medicine but also in the development of different sensors.
A phosphate/molybdate and cerium-modified phosphate/molybdate conversion coatings were deposited on a carbon steel surface and their protective and self-healing abilities were evaluated. Surface morphology and inner structure of the coatings were examined using FE-SEM-FIB and TEM techniques, chemical composition and element distribution depth profiles in conversion layers were determined using EDX measurements, whereas XPS was applied for the analysis of Mo and Ce oxidation states. Voltammetric measurements and EIS were performed to assess the corrosion behavior of the samples. The higher protective and stronger self-healing abilities were found for phosphate/molybdate/cerium conversion coating deposited in a sulphate-containing solution. This was attributed to higher values of both: total cerium and Ce(IV) content in the conversion layer as well as to lower number of structural defects in the coating. It was demonstrated that the micro-structural characteristics of protective coatings are also important in determining self-healing abilities.
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