National Institute Of Materials Physics - Romania

Aim of this research was to evaluate the effect of an improved processing thermal method of calcium phosphates obtained from a natural source of high availability (i.e. cyprinids bones). Thereby, the sinterability of the naturally-derived ceramics has been explored. The samples were characterized before and after sintering in terms of surface features (morphology, roughness, wettability and surface energy), weight loss, shrinking, composition, structure, and mechanical properties. The results showed that the initial processing has a significant effect on the sintering outcomes: the morphology and mechanical features were clearly influenced by the processing temperature, while minor effects were observed on the surface and structure properties. Therefore, the study unveils suitable strategies for controlling the characteristics of cost-effective bioceramics and opens up new perspectives for the sustainable manufacturing of highly valuable biomedical products from abundant carp fish bones.

A simple dip coating procedure was used to prepare the magnesium doped hydroxyapatite coatings. An adapted co-precipitation method was used in order to obtain a Ca25-xMgx(PO4)(6)(OH)(2), 25MgHAp (x(Mg)= 0.25) suspension for preparing the coatings. The stabilities of 25MgHAp suspensions were evaluated using ultrasound measurements, zeta potential (ZP), and dynamic light scattering (DLS). Using transmission electron microscopy (TEM) and scanning electron microscopy (SEM) information at nanometric resolution regarding the shape and distribution of the 25MgHAp particles in suspension was obtained. The surfaces of obtained layers were evaluated using SEM and atomic force microscopy (AFM) analysis. The antimicrobial evaluation of 25MgHAp suspensions and coatings on various bacterial strains and fungus were realized. The present study presents important results regarding the physico-chemical and antimicrobial studies of the magnesium doped hydroxyapatite suspensions, as well as the coatings. The studies have shown that magnesium doped hydroxyapatite suspensions prepared withx(Mg)= 0.25 presented a good stability and relevant antimicrobial properties. The coatings made using 25MgHAp suspension were homogeneous and showed remarkable antimicrobial properties. Also, it was observed that the layer realized has antimicrobial properties very close to those of the suspension. Both samples of the 25MgHAp suspensions and coatings have very good biocompatible properties.

Antibacterial cerium-doped hydroxyapatite (Ce-HAp) layers have been researched sparingly in recent years. The Ce-HAp powder, Ca10-xCex(PO4)(6)(OH()2)with x(Ce)= 0.05, was obtained by an adapted chemical co-precipitation method at room temperature. The target was prepared using the Ce-HAp (x(Ce)= 0.05) powder sintered in air at 600 degrees C. The coatings on the Ti substrate were generated in plasma using a radio frequency (RF) magnetron sputtering discharge in an Ar gas flow in a single run. To collect the most complete information regarding the antimicrobial activity of cerium-doped hydroxyapatite with x(Ce)= 0.05, (5Ce-HAp), antimicrobial studies were carried out both on the final suspensions and on the coated surfaces. The target was tested using ultrasound measurement, transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), glow-discharge optical emission spectroscopy (GDOES), and X-ray photoelectron spectroscopy (XPS). The present study exhibited for the first time results of the homogeneous coatings of hydroxyapatite doped with cerium using a radio frequency magnetron sputtering technique. In addition, this study highlighted for the first time the stability of the cerium-doped hydroxyapatite gels used in the creation of the coating. Ultrasound measurements on the concentrated suspension of 5Ce-HAp showed a good stability compared to double distilled, water which was chosen as the reference fluid. Particles with spherical shape were observed by both TEM and SEM analysis. The broadening of the IR bands in the IR spectrum of the 5Ce-HAp film in comparison with the IR spectrum of the precursor target indicate the formation of interlinked bonds into the layer bulk. XPS analysis revealed that the mixture of Ce(3+)and Ce(4+)ions in the hydroxyapatite (HAp) structure of the coatings could be due to the deposition process. The surface of 5Ce-HAp coatings was homogenous with particles having a spherical shape. A uniform distribution of all the constituent elements on the surface the 5Ce-HAp layer was revealed. The antimicrobial assays proved that both 5Ce-HAp suspensions and 5Ce-HAp coatings effectively inhibited the development of colony forming units (CFU) for all the tested microbial strains. Moreover, the antimicrobial assays emphasized that the 5Ce-HAp suspensions had a biocide effect against Escherichia coli (E. coli) andCandida albicans(C. albicans)microbial strains after 72 h of incubation.

We have explored an efficient strategy to enhance the overall photocatalytic performances of layered perovskites by increasing the density of hydroxyl group by protonation. The experimental procedure consisted of the slow replacement of interlayer Rb(+)cation of RbLaTa(2)O(7)Dion-Jacobson (DJ) perovskite by H(+)via acid treatment. Two layered perovskites synthesized by mild (1200 degrees C for 18 h) and harsh (950 and 1200 degrees C, for 36 h) annealing treatment routes were used as starting materials. The successful intercalation of proton into D-J interlayer galleries was confirmed by FTIR spectroscopy, thermal analyses, ion chromatography and XPS results. In addition, the ion-exchange route was effective to enlarge the specific surface area, thus enhancing the supply of photocharges able to participate in redox processes involved in the degradation of organic pollutants. HLaTa_01 protonated layered perovskite is reported as a efficient photocatalyst for photomineralization of trichloroethylene (TCE) to Cl(-)and CO(2)under simulated solar light. The enhanced activity is attributed to combined beneficial roles played by the increased specific surface area and high density of hydroxyl groups, leading to an efficiency of TCE mineralization of 68% moles after 5 h of irradiation.

(1) Background: The high-voltage anodic-plasma (HVAP) coating technique has a series of specificities that are not simultaneously met in other deposition methods. This paper aimed at assessing the potential of HVAP to synthesize quality multilayers for X-ray optics. (2) Methods: Nanolayers of W, Ta, B, and Si were deposited as mono-, bi-, and multilayers onto very smooth glass substrates by HVAP, and their thickness and density were analyzed by X-ray reflectometry. The minimal film thickness needed to obtain continuous nanolayers was also investigated. (3) Results: Nanolayer roughness did not increase with layer thickness, and could be lowered via deposition rate, with values as low as 0.6 for the W nanolayer. Minimal film thickness for continuous films for the studied metals was 4 nm (W), 6 nm (Ta), 2.5 nm (B), and 6 nm (Si). (4) Conclusions: The investigation revealed the range of parameters to be used for obtaining quality nanolayers and multilayers by HVAP. Advantages and possible improvements are discussed. This deposition technique can be tailored for demanding applications such as X-ray mirrors.

A new composite base on reduced graphene oxide (RGO) and poly(5-amino-1-naphthol) (P5A1N) was synthesized by the electrochemical polymerization of 5-amino-1-naphthol (5A1N) in the presence of HClO(4)and H(4)SiW(12)O(40)onto the surface of Au electrode covered with the RGO sheets. The linear dependence of the current densities of the anodic and cathodic peaks with the scan rate of the potential range (0; 0.8) V vs. SCE, reported during electropolymerization of 5A1N, indicates an electron transfer that is controlled by diffusion. A covalent functionalization of the RGO sheets with P5A1N is argued by: (i) the simultaneous disappearance of the IR band at 1584 cm(-1)and the appearance of the new IR bands at 812, 976 and 3744 cm(-1), and (ii) the appearance of two Raman lines at 738 and 1428 cm(-1). An application of the RGO sheets covalently functionalized with P5A1N is demonstrated to support 1,4-phenylene diisothiocyanate (PDITC), a compound used as a cross-linking agent for various biological applications. The chemical adsorption of PDITC onto the RGO sheets covalently functionalized with P5A1N, which involves the appearance of new functional groups of the type thiourea, was proven by Raman scattering and IR spectroscopy.

To improve the catalytic performance of an active layered double hydroxide (LDH)-derived CuCeMgAlO mixed oxide catalyst in the total oxidation of methane, it was promoted with different transition-metal cations. Thus, two series of multicationic mixed oxides were prepared by the thermal decomposition at 750 degrees C of their corresponding LDH precursors synthesized by coprecipitation at constant pH of 10 under ambient atmosphere. The first series of catalysts consisted of four M(3)CuCeMgAlO mixed oxides containing 3 at.% M (M = Mn, Fe, Co, Ni), 15 at.% Cu, 10 at.% Ce (at.% with respect to cations), and with Mg/Al atomic ratio fixed to 3. The second series consisted of four Co(x)CuCeMgAlO mixed oxides withx= 1, 3, 6, and 9 at.% Co, while keeping constant the Cu and Ce contents and the Mg/Al atomic ratio. All the mixed oxides were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) coupled with X-ray energy dispersion analysis (EDX), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption-desorption at -196 degrees C, temperature-programmed reduction under hydrogen (H-2-TPR), and diffuse reflectance UV-VIS spectroscopy (DR UV-VIS), while thermogravimetric and differential thermal analyses (TG-DTG-DTA) together with XRD were used for the LDH precursors. The catalysts were evaluated in the total oxidation of methane, a test reaction for volatile organic compounds (VOC) abatement. Their catalytic performance was explained in correlation with their physicochemical properties and was compared with that of a reference Pd/Al(2)O(3)catalyst. Among the mixed oxides studied, Co(3)CuCeMgAlO was found to be the most active catalyst, with a temperature corresponding to 50% methane conversion (T-50) of 438 degrees C, which was only 19 degrees C higher than that of a reference Pd/Al(2)O(3)catalyst. On the other hand, this T(50)value was ca. 25 degrees C lower than that observed for the unpromoted CuCeMgAlO system, accounting for the improved performance of the Co-promoted catalyst, which also showed a good stability on stream.

Issues related to the optimization of heat transfer mechanisms dominated by superparamagnetic relaxation are considered in the case of AC (alternating current) magnetic field hyperthermia procedures. The key role in the conversion of electromagnetic energy to the thermal one via the superparamagnetic relaxation mechanism is played by the magnetic anisotropy of nanoparticles, easily to be controlled via the shape anisotropy component. The optimization process has been discussed in the case of magnetite (Fe3O4) ellipsoidal nanoparticles with dominant shape anisotropy dispersed in different media. Nanoparticles of different sizes and aspect ratios have been considered in correlation with those specific parameters of the actuating AC magnetic field which respect an established biological safely criterion. It has been proven that the dissipated power can be maximized for a given set of biological compatible RF (radiofrequency) field parameters (frequency and field amplitude at the sample space) only for specific pairs of particle sizes and aspect ratios. For instance, it has been shown that ellipsoidal magnetite nanoparticles with 10 nm equatorial size and aspect ratio of 2 are optimal for a maximum transferred power under radiofrequency excitations of 250 kHz and field amplitude of 20 kA/m, if high viscosity dispersion media are used. The methodology for deriving the optimal shape (geometrical) parameters of a specific type of nanoparticles in conditions of using available radiofrequency excitations, or vice versa, for deriving the optimal radiofrequency working parameters in the case of ferrofluids with specific nanoparticles (type and geometry) is described and discussed in detail.

When the gas sensor active layer film thickness is decreased, increased sensitivity to changes in the adsorbate concentration is expected when measuring the resistance of the layer, in particular when this thickness is on the order of the Debye length of the material (one-tens of nanometers); however, this is demonstrated only for a limited number of materials. Herein, ultrathin NiO films of different thicknesses (8-21 nm) have been deposited via chemical vapor deposition to fabricate gas sensor devices. Sensor performance for a range of NO2 concentrations (800 part-per-billion to 7 part-per-million) was evaluated and an optimum operating temperature of 125 degrees C determined. The dependence of the potential relative changes with respect to the NO2 concentration and of the sensor signal with respect to the geometrical parameters was qualitatively evaluated to derive a transduction model capable of fitting the experimental results. The selective sensitivity toward NO2 was confirmed by the limited response for different reducing gases, CO, CH4, NH3, and SO2, under optimum operating conditions, and the sensor signal toward NO2 increased with decreasing thickness, demonstrating that the concept of a Debye length dependence of sensitivity is applicable for the p-type semiconductor NiO. In addition, these NiO sensors were exposed to different relative levels of humidity over a wide range of operating temperatures and were found to display humidity tolerance far superior to those in previous reports on SnO2 materials.

Palladium is one of the most efficient metals for the hydrogenation of organic compounds. However, when molecules, such as nitroaromatics, with several reducible functionalities, are hydrogenated, Pd, like any other very active metal, such as nickel or platinum, often behaves unselectively. One strategy to render Pd more selective is to choose the proper support. Herein, we show that MAX phase powders of Ti3SiC2, Ti2AlC, or Ti3AlC2 can chemoselectively hydrogenate 4-nitrostyrene to 4-aminostyrene, with 100% selectivity, at around 3-4% conversion. To boost the latter, we loaded Ti3SiC2 with 0.0005 wt % Pd and increased the conversion to 100% while maintaining the 4-AS selectivity at >90%. By optimizing the Pd loading, we were also able to increase the turnover frequency 100-fold relative to previous literature results. The identification of this highly efficient and chemoselective system has broad implications for the design of cost-effective, earth-abundant, nontoxic, metal catalysts, with ultralow noble metal loadings.