Simona Somacescu

Tailoring mixed ionic–electronic conduction in H2 permeable membranes based on the system Nd5.5W1−xMoxO11.25−δ

Lanthanide tungstates (Ln6WO12) are promising candidates for the development of ceramic hydrogen transport membranes since they exhibit mixed ionic (proton and oxygen ion transport) and electronic conductivity and remarkable stability in a moist CO2 environment at high temperatures. This work presents the structural and electrochemical characterization of mixed conducting materials for the specific system Nd5.5W1−xMoxO11.25−δ (x = 0, 0.1, 0.5 and 1). Evolution of the crystalline structure is studied as a function of the sintering temperature. Shrinkage behavior is analyzed for all compositions in the temperature range from 1000 °C to 1500 °C and these compounds show high sintering activity even at relatively low temperatures. The total conductivity in different environments is studied systematically for samples sintered at 1350 °C. The H/D isotopic effect is also studied by DC-electrochemical measurements. H2 permeation is investigated for the selected compound Nd5.5W0.5Mo0.5O11.25−δ in the range of 700–1000 °C achieving values of 0.3 mL min−1 cm−2 for a 0.9 mm thick disc membrane. Finally, the stability of this material under different CO2 and H2S-rich atmospheres at high temperatures is proven.

Biopolymer starch mediated synthetic route of multi-spheres and donut ZnO structures

A starch-assisted synthetic methodology of multispheres ZnO-starch biocomposites was developed. An additional thermal processing of the ZnO-starch composites induces the formation of ZnO with donut-like morphology. The synthesis of single-phase zinc oxide with a spherical morphology is conditioned by the presence of starch, which acts as template, stabilizing/capping agent. The synthesized structures present significant photocatalytic activities; a total phenol mineralization is attained with the donut-like ZnO photocatalyst under visible light irradiation, due to a cumulative effect of the its relatively large specific surface area, high crystallinity and favorable combination of defects for band narrowing, which together permit an enhanced utilization rate of the light.

Sensors based on mesoporous SnO2-CuWO4 with high selective sensitivity to H2S at low operating temperature

Development of new sensitive materials by different synthesis routes in order to emphasize the sensing properties for hazardous H2S detection is one of a nowadays challenge in the field of gas sensors. In this study we obtained mesoporous SnO2-CuWO4 with selective sensitivity to H2S by an inexpensive synthesis route with low environmental pollution level, using tripropylamine (TPA) as template and polyvinylpyrrolidone (PVP) as dispersant/stabilizer. In order to bring insights about the intrinsic properties, the powders were characterized by means of a variety of complementary techniques such as: X-Ray Diffraction, XRD; Transmission Electron Microscopy, TEM; High Resolution TEM, HRTEM; Raman Spectroscopy, RS; Porosity Analysis by N2 adsorption/desorption, BET; Scanning Electron Microscopy, SEM and X-ray Photoelectron Spectroscopy, XPS. The sensors were fabricated by powders deposition via screen-printing technique onto planar commercial Al2O3 substrates. The sensor signals towards H2S exposure at low operating temperature (100°C) reaches values from 105 (for SnWCu600) to 106 (for SnWCu800) over the full range of concentrations (5-30ppm). The recovery processes were induced by a short temperature trigger of 500°C. The selective sensitivity was underlined with respect to the H2S, relative to other potential pollutants and relative humidity (10-70% RH).

Structure and surface chemistry in crystalline mesoporous (CeO2−δ)–YSZ

Mesoporous metal oxides (CeO(2-δ))-YSZ have been synthesized by a versatile direct synthesis method using ionic cetyltrimethylammonium bromide (CTAB) and different nonionic (block copolymers) as surfactants and urea as hydrolyzing agent. The synthesis was realized at pH=9 using tetraethylammonium hydroxide (TEAOH) as pH mediator. Calcination at 550 °C led to the formation of crystalline metal oxides with uniform mesoporosity. The obtained materials have been characterized by thermogravimetric analysis (TG-DTG), wide and small-angle X-ray diffraction (XRD), Raman spectroscopy, Brunauer, Emmett and Teller (BET) surface area analysis, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). All the obtained materials exhibits mesoporous structure, crystalline structure indexed in a cubic symmetry, showing a high surface area, a uniform and narrow pore size distribution, spherical morphology typical for the mesoporous materials. The crystalline and mesoporous structures, surface chemistry and stoichiometry for the samples synthesized using ionic and nonionic surfactants have been discussed.

Sustainable one-pot integration of ZnO nanoparticles into carbon spheres: manipulation of the morphological, optical and electrochemical properties.

ZnO-carbon composite spheres were synthesized via starch hydrothermal carbonization (HTC) in the presence of a soluble zinc salt (acetate), followed by thermal processing under an argon atmosphere. Besides sustainability, the one-pot procedure represents a scalable synthesis of tailored carbon-metal oxide spheres with a structurally-ordered carbon matrix obtained at a relatively low temperature (700 °C). The ability of zinc cations to develop different linkages with starchs hydrophilic functional groups and to act as external nucleators determines an increase in HTC yield; the effect is obvious even in the presence of small concentrations of zinc in the reaction medium (0.005 M), thus providing a way to improve the carbonization process efficiency. It is also shown that zinc content is the control vector of the spherical composites properties: a variation from 0.3 to 4.8 at% not only induces a variation in their size (200 nm-10 μm), interconnectivity (from disperse spheres to necklace-like aggregations), surface area and connected porosity (from micro- to mesoporosity), but also of their electrochemical and white light adsorption and emission features. Since the variation in zinc content is made by a simple adjustment of the raw material concentrations, the functionality of these carbon-based materials can be modulated in a straightforward manner.

Multifunctional Silver Nanoparticles-Decorated Silica Functionalized with Retinoic Acid with Anti-Proliferative and Antimicrobial Properties

The paper describes a rapid and simple method for preparing a multifunctional biomaterial based on retinoic acid covalently bound on silica@Ag particles. Monodispersed SiO2 particles were prepared by Stöber method and further used for loading the Ag nanoparticles on their surface. This composite was further functionalized with retinoic acid. Characterization of the hybrid materials was made by UV–Visible spectroscopy, Transmission electron microscopy, Scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and Thermal analysis. The biological evaluation of the obtained materials revealed their potential use for multiple biomedical applications, from anti-proliferative agents to novel antimicrobial and antibiofilm strategies.

High-performance solid state supercapacitors assembling graphene interconnected networks in porous silicon electrode by electrochemical methods using 2,6-dihydroxynaphthalen

The challenge for conformal modification of the ultra-high internal surface of nanoporous silicon was tackled by electrochemical polymerisation of 2,6-dihydroxynaphthalene using cyclic voltammetry or potentiometry and, notably, after the thermal treatment (800 °C, N2, 4 h) an assembly of interconnected networks of graphene strongly adhering to nanoporous silicon matrix resulted. Herein we demonstrate the achievement of an easy scalable technology for solid state supercapacitors on silicon, with excellent electrochemical properties. Accordingly, our symmetric supercapacitors (SSC) showed remarkable performance characteristics, comparable to many of the best high-power and/or high-energy carbon-based supercapacitors, their figures of merit matching under battery-like supercapacitor behaviour. Furthermore, the devices displayed high specific capacity values along with enhanced capacity retention even at ultra-high rates for voltage sweep, 5 V/s, or discharge current density, 100 A/g, respectively. The cycling stability tests performed at relatively high discharge current density of 10 A/g indicated good capacity retention, with a superior performance demonstrated for the electrodes obtained under cyclic voltammetry approach, which may be ascribed on the one hand to a better coverage of the porous silicon substrate and, on the other hand, to an improved resilience of the hybrid electrode to pore clogging.

Sol-gel synthesis of ZnO/Zn2-xFexTiO4 powders: structural properties, electrical conductivity and dielectric behavior

AbstractThe aim of this work was an investigation of structural and electrical properties of ZnO/Zn2-xFexTiO4 (x = 0.7, 1, 1.4) powders. The compounds obtained by sol-gel method are characterized by several techniques: X-ray diffraction (XRD), N2 adsorption–desorption isotherms, scanning and transmission electron microscopy (SEM and TEM), X-ray photoelectron spectroscopy (XPS), electrical and dielectrical measurements. The XRD, SEM and XPS analysis confirmed the formation of ZnFeTiO4 inverse spinel structure. The electrical and dielectrical properties of ZnO/Zn2-xFexTiO4 (x = 0.7, 1, 1.4) were measured by impedance spectroscopy, revealing a decrease in the electrical conductivity and the dielectric constant with Fe content.

Mixed Ionic-Electronic Conduction in NiFe2O4-Ce0.8Gd0.2O2−δ Nanocomposite Thin Films for Oxygen Separation

NiFe2 O4 -Ce0.8 Gd0.2 O2-δ (NFO/CGO) nanocomposite thin films were prepared by simultaneously radio-frequency (RF) magnetron sputtering of both NFO and CGO targets. The aim is the growth of a CO2 -stable composite layer that combines the electronic and ionic conduction of the separate NFO and the CGO phases for oxygen separation. The effect of the deposition temperature on the microstructure of the film was studied to obtain high-quality composite thin films. The ratio of both phases was changed by applying different power to each ceramic target. The amount of each deposited phase as well as the different oxidation states of the nanocomposite constituents were analyzed by means of X-ray photoelectron spectroscopy (XPS). The transport properties were studied by conductivity measurements as a function of temperature and pO2 . These analyses enabled (1) selection of the best deposition temperature (400 °C), (2) correlation of the p-type electronic behavior of the NFO phase with the hole hopping between Ni3+ -Ni2+ , and (3) following the conductivity behavior of the grown composite layer (prevailing ionic or electronic character) attained by varying the amount of each phase. The sputtered layer exhibited high ambipolar conduction and surfaceexchange activity. A 150 nm-thick nanograined thin film was deposited on a 20 μm-thick Ba0.5 Sr0.5 Co0.8 Fe0.2 O3-δ asymmetric membrane, resulting in up to 3.8 mL min-1  cm-2 O2 permeation at 1000 °C under CO2 atmosphere.

Gas sensing properties of NiO/mesoporous SnO 2

NiO/mesoporous SnO<inf>2</inf> was deposited by incipient wetness impregnation of the SnO<inf>2</inf> powder prepared by hydrothermal synthesis route templated by Brij® 35. The sensing properties were acquired and the dependence on the operating temperature of the sensitive material was pointed out. Sensitive selectivity towards H<inf>2</inf>S detection was highlighted at 350 °C.