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The present work reports the synthesis of efficient Ti–Au/zeolite Y photocatalysts by different processing of aluminosilicate gel and studies the effect of titania content on the structural, morphological, textural, and optical properties of the materials. The best characteristics of zeolite Y were obtained by aging the synthesis gel in static conditions and mixing the precursors under magnetic stirring. Titania (5, 10, 20%) and gold (1%) species were incorporated in zeolite Y support by the post-synthesis method. The samples were characterized by X-ray diffraction, N2-physisorption, SEM, Raman, UV–Vis and photoluminescence spectroscopy, XPS, H2-TPR, and CO2-TPD. The photocatalyst with the lowest TiO2 loading shows only metallic Au on the outermost surface layer, while a higher content favors the formation of additional species such as: cluster type Au, Au1+, and Au3+. A high TiO2 content contributes to increasing the lifetime of photogenerated charge careers, and the adsorption capacity of the pollutant. Therefore, an increase in the photocatalytic performances (evaluated in degradation of amoxicillin in water under UV and visible light) was evidenced with the titania content. The effect is more significant in visible light due to the surface plasmon resonance (SPR) effect of gold interacting with the supported titania.

New photocatalysts were obtained by immobilization of titanium and gold species on zeolite Y, hierarchical zeolite Y, MCM-48 and KIT-6 supports with microporous, hierarchical and mesoporous cubic structure. The obtained samples were characterized by X-ray diffraction (XRD), N2-physisorption, scanning and transmission electron microscopy (SEM/TEM), diffuse reflectance UV–Vis spectroscopy (DRUV-Vis), X-ray photoelectron spectroscopy (XPS), Raman and photoluminescence spectroscopy. The photocatalytic properties were evaluated in degradation of amoxicillin (AMX) from water, under UV (254 nm) and visible light (532 nm) irradiation. The higher degradation efficiency and best apparent rate constant were obtained under UV irradiation for Au-TiO2-KIT-6, while in the visible condition for the Au-TiO2-MCM-48 sample containing anatase, rutile and the greatest percent of Au metallic clusters were found (evidenced by XPS). Although significant values of amoxicillin degradation were obtained, total mineralization was not achieved. These results were explained by different reaction mechanisms, in which Au species act as e− trap in UV and e− generator in visible light.

This paper introduces for the first time the preparation of cobalt aluminate (CoAl2O4) nanoparticles through a solution combustion method using a Mentha piperita leaves extract. The active constituents present in the mentha leaves extract act as both a chelating and a reducing agent. The isolated precursor was characterized by FTIR, UV–Vis, thermal analysis and XPS. Various techniques (XRD, SEM and TEM, XPS, FTIR and UV–Vis) were also used to characterize the cobalt aluminate spinel from the point of view of structure, morphology and surface chemistry. XRD confirmed the formation of a single-phase, crystalline cubic spinel structure with mean crystalline domain size of 19.5 nm. The TEM analysis showed rhombic and rectangular CoAl2O4 nanoparticles with unimodal particle size distribution and average particle size of about 35 nm. The characteristic peaks of the CoAl2O4 spinel were highlighted by the FTIR spectrum. The tetrahedral configuration of Co2+ ions in the CoAl2O4 spinel structure was illustrated by the absorbance and XPS spectra. Furthermore, XPS spectra reveal both tetrahedral and octahedral configurations of Al3+ ions. To evaluate the catalytic properties of the cobalt aluminate, the photocatalytic degradation of methylene blue (MB) was carried out under visible light irradiation.

Although both stable free organic radicals and biomass-derived hydrochars have emerged as appealing, green, multifunctional materials, their association has not been explored. In this study, strength is found to lie in their union, which primarily leads to stable redox-active free-radical-hydrochar composites that can generate unexpected opportunities for the development of advanced metal-free sustainable materials. The composites are obtained by a straightforward green one-pot hydrothermal procedure. The loading of stable free radicals of nitroxide type and their localization is engineered by the nature of the carbohydrate and the reaction status; vigorous reaction parameters promote faster nucleation and growth kinetics of the hydrochar products, leading to a covalent immobilization of redox species on the surface of the carbonaceous microspherical aggregates. The nitroxide free-radical-hydrochar materials demonstrate enhancements in terms of both electrocatalytic activity and capacitive features.

Fuel cells are devices that transform efficiently the chemical energy of hydrogen or another fuel into clean electricity. The fuel cell technology is attractive for its high-energy efficiency and expanded fuel flexibility and it became very relevant in the last decade. Moreover, the utilization of fuel cells for portable electronic devices has seen remarkable increase in the last few years. Performances of fuel cells, among others, strongly depend on the types of electrocatalysts and membrane, anion exchange or cation exchange, used in the system. Therefore, a status report about the latest advances in electrocatalysts and electrodes for portable fuel cells is the objective of this review paper. Herein, the recent progress in designing electrocatalysts for producing high performance fuel cells with truly potential applicability to be used in portable devices is highlighted.

Electrocatalytic activity of a new, pristine and graphene-modified NiCo2O4–NiO catalysts towards oxygen reduction reaction (ORR) was gauged. Linear sweep voltammetry attests that NiCo2O4–NiO (NCO) catalyst, obtained by a facile synthesis route based on a self-assembling co-templated by diethanolamine (DEA) and tripropylamine (TPA), shows conspicuous catalytic activity towards ORR. The catalytic activity of NCO was tentatively ascribed to the presence of the cubic spinel NiCo2O4 and of a small amount of NiO, as a secondary phase (evidenced by XPS and XRD) which most likely enables the formation of efficient active sites and enhances the conductivity of the material. After mixing the NCO with reduced graphene oxide (rGO), the catalytic activity of the new composite NiCo2O4–NiO-rGO (NCO-rGO) was significantly improved. Electrochemical results reveal that the presence of graphene facilitates a more efficient mass transport, supplies more accessible active sites, and provides higher stability and better resistance to deactivation during ORR. The synthesis route herein developed for preparing NCO material might be successfully used for large-scale applications due to its outstanding features, such as low cost, easy availability, and straightforward control of the phase composition.

Semiconducting metal oxide-based gas sensors are an attractive option for a wide array of applications. In particular, sensors based on WO3 are promising for applications varying from indoor air qu...

In this study, the synergistic behavior of Ni species and bimodal mesoporous undoped SnO2 is investigated in oxygen evolution reactions (OERs) under alkaline conditions without any other modificati...

Polycrystalline NiO thick film-based gas sensors have been exposed to different test gas atmospheres at 250 °C and measured via simultaneous electrical resistance and work function investigations. Accordingly, we decoupled different features manifested toward the potential changes, i.e., work function, band-bending, and electron affinity. The experimental results have shown that the presence of moisture induces an unusual behavior toward carbon monoxide (CO) detection by considering different surface adsorption sites. On this basis, we derived an appropriate detection mechanism capable of explaining the lack of moisture influence over the CO detection with NiO-sensitive materials. As such, CO might have both chemical and dipolar interactions with pre-adsorbed or lattice oxygen species, thus canceling out the effect of moisture. Additionally, morphology, structure, and surface chemistry were addressed, and the results have been linked to the sensing properties envisaging the role played by the porous quasispherical–hollow structures and surface hydration.

NiO-loaded SnO2 powders were prepared involving two chemical procedures. The mesoporous SnO2 support was synthesized by a hydrothermal route using Brij 35 non-ionic surfactant as a template. The nickel loadings of 1 and 10 wt.%. NiO were deposited by the wet impregnation method. The H2S sensing properties of xNiO-(1-x)SnO2 (x = 0, 1, 10%) thick layers deposited onto commercial substrates have been investigated with respect to different potential interfering gases (NO2, CO, CO2, CH4, NH3 and SO2) over a wide range of operating temperatures and relative humidity specific for in-field conditions. Following the correlation of the sensing results with the morphological ones, 1wt.% NiO/SnO2 was selected for simultaneous electrical resistance and work function investigations. The purpose was to depict the sensing mechanism by splitting between specific changes over the electron affinity induced by the surface coverage with hydroxyl dipoles and over the band bending induced by the variable surface charge under H2S exposure. Thus, it was found that different gas-interaction partners are dependent upon the amount of H2S, mirrored through the threshold value of 5 ppm H2S, which from an applicative point of view, represents the lower limit of health effects, an eight-hour TWA.

In this work, we present a simple, two-stage method for the preparation of new and efficient antimicrobial hybrid systems, based on isoniazid and pyrazine-2-carbohydrazide tuberculostatic agents covalently linked to graphene oxide. In the first step, the carboxyl groups of graphene oxide are activated by transforming them into the corresponding acid chloride groups, which, in the second step, will react with the amino groups of the two drugs. Pyrazine-2-carbohydrazide was obtained from pyrazinoic acid and hydrazine hydrate and was confirmed by nuclear magnetic resonance spectroscopy. The materials have been characterized by elemental analysis, infrared spectroscopy, Raman spectroscopy, scanning electron microscopy, and X-ray photoelectron spectroscopy. Their antimicrobial activity was tested on mycobacterial (Mycobacterium terrae), as well as on Gram-negative bacteria (Escherichia coli ATCC 25922, Pseudomonas aeruginosa ATCC 27853), Gram-positive bacteria (Staphylococcus aureus ATCC 6538, Staphylococcus aureus ATCC 25923) and fungal (Candida albicans ATCC 10231), in planktonic and biofilm growth state. The biocompatibility of the tested compounds was assessed in vitro by live-dead fluorescence staining and flow cytometry. The results of this study have shown that the functionalization of graphene oxide with isoniazid and pyrazine-2-carbohydrazide both enhanced the anti-mycobacterial activity of the respective drugs and extended their antimicrobial spectrum towards other microbial strains, in planktonic and biofilm growth state, showing a promising potential for mitigating the impact of antimicrobial resistance and the deleterious effects of microbial biofilms. At the active tuberculostatic concentrations, the tested compounds exhibit very low cytotoxicity and do not interfere with the cellular cycle of Hep-2 cells. The flow cytometry and live/dead fluorescence staining proved that the tested compounds exhibit a microbicidal effect through induction of cellular lesions, consecutive to membrane depolarization.

Bone defects due to trauma or diseases causing bone loss have led to an increased demand for new materials that have applications in therapies for bone pathologies. Mesoporous bioactive glasses (MBGs), based on 70SiO2-(26-x)CaO 4P2O5-xCeO2 (x = 0, 1 and 5 mol % for MBGS, MBGS1Ce and MBGS5Ce) were synthesized by evaporation-induced self-assembly (EISA) method. Ceria was selected due to its antimicrobial and antioxidant properties and positive impact on cells differentiation and mineralization. The pore size values of 2.8 nm confirmed the mesoporosity of the obtained bio-glasses. The biocompatibility tests on mouse fibroblast cells (NCTC clone L929) using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and lactate dehydrogenase (LDH) activity assays revealed no cytotoxicity of Cerium containing MBGs. Formation of a hydroxycarbonate apatite (HCA) layer on MBGs surface, e.g. bioactivity of BMGs, was confirmed by XRD, FTIR, SEM and Raman Spectroscopy while presence of Ce3+/Ce4+ in the glasses before body simulated fluid (SBF) immersion was determined by XPS, UV–Vis measurements. The obtained results show that investigated MBGs are potential materials for applications in bone regeneration.

In the present study we report on the activity, selectivity and stability of the bimodal mesoporous NiO/CeO2-δ-YSZ anodes for IT-SOFCs applications. These materials present high concentration of Ce3+ ions stably retained in the lattice, which proved to be efficient for the catalytic partial oxidation of CH4 to syngas in the temperature range 600–800 °C. The excellent carbon tolerance was proved by a comprehensive XPS analysis, which monitored the amount of carbon before and after catalytic partial oxidation of methane (CPOM) tests. The mesoporous anodes templated by hexadecyltrimethylammonium bromide (CTAB) and tripropylamine (TPA) were obtained using a hydrothermal synthesis route. The effect of Ni and Ce incorporation on the yttria stabilized zirconia (YSZ) structure, texture, morphology and surface chemistry was discussed and correlated with catalytic and electrochemical behavior. The exhaustive characterization of the bulk and surface properties of the catalysts have been accomplished by means of complementary methods: XRD, SEM / EDX / HRTEM, TGA / TPR, XPS. The electrochemical and catalytic performance were improved when the surface contains more reduced ceria and NiO was formed as secondary phase. These features lead to a large number of vacancies and consequently a better oxygen migration, which facilitate the carbon removal.

Nitrogen (N)-doped SrTiO3 /pristine SrTiO3 powders were synthesized by three different methods namely hydrothermal, sol-gel route and solid state reaction respectively. The influence of synthesis route, thermal treatment atmosphere and N doping on the properties and photo-catalytic efficiency of the prepared samples was analyzed. The investigation shows that N doping causes the narrowing of the band gap with about 1 eV. The synergy of the structure, texture and morphology and especially N doping explains high methyl orange (MO) degradation efficiency of 100% within 1 h of irradiation for the N doped SrTiO3 obtained by sol-gel route with the aid of non-ionic triblock copolymer (Pluronic P123) as a structure-directing and thermally treated under nitrogen atmosphere.

Our study focuses on an advanced exploratory research based on the development of the new IT-SOFCs anode compositions in conjunction with surfactants as template to obtain mesoarchitectured catalysts. We designed NiO/Sr doped CePr ErO (2.5 and 5 mol.% Sr) mesoarchitectures with robust crystalline framework following a hydrothermal synthesis route. NiO was deposited by wet impregnation and calcined in air at 900 °C, in order to assure a good interaction between Ni and mesoporous matrix. The obtained materials exhibit a cubic CeO fluorite phase with PrO and SrCeO as secondary phase traces and these were assessed as catalyst for the partial oxidation of CH over time and IT-SOFCs anode under reducing atmosphere. The electrochemical behavior as anode fed by wet H (2.5% vol. HO) was investigated in the NiO/CPS/YSZ/GDC/Pt electrochemical cells. The compositional effect on the structural properties, surface chemistry, catalytic and electrochemical performance were highlighted. Sr incorporated in the lattice, proved by X-ray Photoelectron Spectroscopy, guarantees an excellent stability of the catalysts over time for 20h, during partial oxidation of CH with high CH conversion and CO selectivity (90% in the range 700–800 °C) as well as a better performance as IT-SOFCs anode., This work was supported by a grant of Partnerships in priority S&T domains Program (PNII), MEN-UEFISCDI, project number 26/2012. MF, MMT. PO, JMCM and SS aknowledge CCCDI – UEFISCDI, project nos 110 and 111/2019, ERANET-M.-CATALEAST, within PNCDI III.

The paper presents the possibility of detecting low H2S concentrations using CuWO4. The applicative challenge was to obtain sensitivity, selectivity, short response time, and full recovery at a low operating temperature under in-field atmosphere, which means variable relative humidity (%RH). Three different chemical synthesis routes were used for obtaining the samples labeled as: CuW1, CuW2, and CuW3. The materials have been fully characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). While CuWO4 is the common main phase with triclinic symmetry, different native layers of CuO and Cu(OH)2 have been identified on top of the surfaces. The differences induced into their structural, morphological, and surface chemistry revealed different degrees of surface hydroxylation. Knowing the poisonous effect of H2S, the sensing properties evaluation allowed the CuW2 selection based on its specific surface recovery upon gas exposure. Simultaneous electrical resistance and work function measurements confirmed the weak influence of moisture over the sensing properties of CuW2, due to the pronounced Cu(OH)2 native surface layer, as shown by XPS investigations. Moreover, the experimental results obtained at 150 °C highlight the linear sensor signal for CuW2 in the range of 1 to 10 ppm H2S concentrations and a pronounced selectivity towards CO, CH4, NH3, SO2, and NO2. Therefore, the applicative potential deserves to be noted. The study has been completed by a theoretical approach aiming to link the experimental findings with the CuW2 intrinsic properties.

In this study, the synergistic behavior of Ni species and bimodal mesoporous undoped SnO

Sensors based networked mesoporous SnO2 nanostructures templated by non-ionic surfactant - Brij® 35 were prepared via hydrothermal chemistry route. Specific patterns of the structure, morphology, surface chemistry and sensing properties were obtained by pH and autogenous pressure tuning. Consequently, the as-obtained SnO2 powders were subjected to extensive BET, Raman, TEM, HRTEM and XPS complementary investigations. The sensitive films were obtained by screen printing deposition of the powders onto commercial Al2O3 substrates. The gas sensing properties were assessed towards different hazardous gas species: CO, CH4, NH3, NO2, SO2 and H2S over a wide range of operating temperatures. Our particular SnO2 – HP sensor synthesized at high autogenous pressure showed the highest selective-sensitivity to H2S ( The enhancement in the H2S sensitivity at low operating temperature under infield conditions was found to be closely connected to the morphological aspects and surface chemistry, peculiarities that can be assessed as consequences of the chemical tuning.

Two ZnO materials of spherical hierarchical morphologies, with hollow (ZnOHS) and solid cores (ZnOSS), were obtained through the hydrolysis of zinc acetylacetonate in 1,4-butanediol. The nature of the defects and surface reactivity for the two ZnO materials were investigated through photoluminescence, X-ray photoelectron spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy proving the coexistence of shallow and deep defects and, also, the presence of polyol byproducts adsorbed on the outer layers of the ZnO samples. The EPR spectroscopy coupled with the spin-trapping technique showed that the surface of the ZnO samples generates reactive oxygen species (ROS) like hydroxyl (•OH) and singlet oxygen (1O2) as well as carbon-centered radicals. The ZnO materials exhibited a wide spectrum of antimicrobial activity, being active against Gram-positive, Gram-negative, and fungi strains, both in planktonic and, more importantly, adherent growth states. The decrease of antimicrobial efficiency in the ...

Zn, Fe modified SnO2 powders were prepared by sol-gel method using Tripropylamine as chelating agent and Polyvinylpyrrolidone K90 as dispersant and stabilizer. Two compositions were taken into account: Zn, Fe modified SnO2 – 20 mol% Zn, 10 mol% Fe and Zn, Fe modified SnO2 – 20 mol% Zn, 30 mol% Fe, denoted further as SZFe1and SZFe2 respectively. The properties and the influence of Fe amount on structure, morphology and surface chemistry, electrical and magnetic properties have been investigated. The X-ray diffraction analysis showed the formation of a polycrystalline mixture of cassiterite – SnO2, hematite – Fe2O3, franklinite – ZnFe2O4 and zincite – ZnO for the samples with different Fe content. The magnetization of SZFe2 sample was found to be composed of a ferromagnetic and a paramagnetic phase. The presence of Fe in the powders composition improved the electrical properties, demonstrating performant features in sensing characteristics (tested in CO gas concentrations varied from 50 to 1000 ppm). The magnetic investigations suggest their possible future applications as soft magnetic materials.

New Ti-MCM-48 and CeTi-MCM-48 photocatalysts were obtained by impregnation of the MCM-48 silica support synthesized by a hydrothermal process with aqueous solution of Ti and Ce precursors. The immobilization of metal cations presented a low effect on the porosity, morphology and structure of MCM-48 mesoporous silica support as was evidenced by N2 adsorption–desorption, X-ray diffraction, SEM and TEM electron microscopy. EDAX analysis and X-ray photoelectron microscopy (XPS) indicated that titanium cations were present on the mesoporous silica surface only as Ti4+ species and the effect of ceria on titanium speciation was different, compared to the CeTi-MCM-48 sample, previously obtained by direct synthesis. The photocatalytic properties of mono- and bimetallic catalysts were evaluated in degradation of phenol from water and correlated with the active metallic species concentration, distribution, speciation and their interaction with the support or each other. An advanced oxidation mechanism for phenol degradation by radical species was proposed.

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.

Ti-KIT-6 materials having different TiO 2 loadings (5%, 10%, 30%) were synthesized, modified by Ce and Pt immobilization, characterized by N 2 -adsorption/desorption, XRD, SEM, EDX, TEM, XPS and TPR analysis techniques and tested in CH 4 combustion and CO oxidation reactions. The mesoporous ordered structure of KIT-6 support was preserved in regard to surface area and pore volume. The average pore size was decreasing due to the effect of titania loading and other metals immobilization. The effects of TiO 2 content and immobilization of CeO 2 on Pt were studied in view of the catalytic properties. XPS showed the increase in electron density on Pt owing to contribution of TiO 2 , but on the other hand it was decreasing as result of CeO 2 effect. The metal–support interaction, under conditions of varying TiO 2 –CeO 2 mixed oxide composition, as evidenced by XRD and TPR, was correlated with the catalytic results. The highest conversion degree of CH 4 was observed with the PtTi-KIT-6 samples within the temperature range 250–400 °C and the highest activity was displayed by the PT5K6 sample in both reactions. The slight decrease in activity was observed at the highest Pt 0 concentration on samples with 30%TiO 2 . This can be due to highest dispersion degree of Pt metal and lower surface area of the catalyst. All the samples with supported titania and ceria were active in CH 4 and CO oxidation reactions and the selectivity to CO 2 varied with temperature.

This paper reports the sensing mechanism of SnO2-CuWO4 mixed oxides towards H2S detection revealed through Pulsed Temperature Mode (PTM). After thick film deposition onto commercial substrates, the final annealing temperature enhances the material reliability through the changes occurred during the experimental conditions. PTM approach represents a tradeoff in terms of sensing mechanism versus sensing performance, in order to get insights about the fundamental aspects. The measurements have been done under dynamic gas flow conditions, in the presence of 50% relative humidity (RH). The gas sensors based on SnO2-CuWO4 exhibit sensor signals higher than 100 to 10 ppm H2S, low cross-sensitivity to common gaseous interfering agents (CO, CH4, NH3, SO2), average selective sensitivity of 8.64 towards the main interfering NO2 gas, moderate response (4 min)/recovery (5 min) transients and power consumption. In order to emphasize the role of moisture towards H2S detection mechanism, the photoacoustic spectroscopic insights were correlated with Transmission Electron Microscopy and X-ray Photoelectron Spectroscopy results. Such approach has shown promising aspects towards further operational sensitive devices.

The 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.

In the present work, a cobalt phthalocyanine-supported reduced graphene oxide material (rGO-CoPc) was used as a catalyst for the degradation of rhodamine B (RhB) and pentachorophenol (PCP) in the presence of peroxymonosulfate (PMS). Inductively coupled plasma (ICP-OES), Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) were employed to characterize the properties of the composite and Co loading in the material. The catalytic activity of the rGO1-CoPc1 catalyst (rGO:CoPc = 1:1) was evaluated by UV–vis absorption spectroscopy at varying PMS concentrations and catalyst dosages. The complete dye removal was achieved in 9 min by rGO1-CoPc1/PMS system with a high initiation rate constant of 1.019 min−1 using RhB (25 µM), PMS (0.1 mM) and rGO1-CoPc1 (0.5 mg/mL). The removal efficiency was found to be as high as 100% after 11 cycles, suggesting a long-lasting catalytic activity of the of rGO1-CoPc1/PMS system. Quenching experiments suggested that sulfate (SO4 −) radicals are the dominant species in the degradation process although hydroxyl (OH ) radicals are also involved in the reaction mechanism. Furthermore, the catalyst was successfully applied for the efficient degradation of pentachlorophenol (PCP). A full degradation of PCP (25 µM) was achieved within 20 min using rGO1-CoPc1 (0.5 mg/mL) and PMS (0.6 mM). This study demonstrated that the use of rGO-CoPc as a heterogeneous catalyst for PMS activation is useful for the advanced oxidation processes (AOP) for practical wastewater treatment.

Herein we report a simple and scalable route to synthesize porous cobalt/cobalt oxide - carbon sphere composites as anode material for rechargeable lithium-ion batteries. It involves the impregnation of starch-derived hydrochar spheres with a cobalt salt, followed by a heat treatment (700 °C) under inert atmosphere. The obtained high surface area (∼670 m 2 g −1 ), submicron spheres (∼300 nm diameter) with high-degree of microporosity (81%) consist of an amorphous carbon matrix with embedded Co/CoO nanoparticles (∼6 nm sized), having a total cobalt content of 6.2 wt%. The hybrid sphere anodes demonstrated superior specific capacity, rate performance and cycling stability. Discharge capacities of 520 and 310 mA h g −1 are observed at charge-discharge rates of 0.1 and 1C respectively. No significant capacity fading is identified on prolonged cycling at various current densities. The electrode also demonstratedexcellent structural stability during extended charge-discharge processes.

In the present study we report on a low cost synthesis of amorphous ZnO modified anatase TiO2 (40 and 20 mol% ZnO) thin films deposited via sol-gel spin coating technique on glass substrate. The effects of the composition on the structural, morphological and surface chemistry properties were discussed and correlated with the electrical behavior. Thus, by X-ray diffraction and Raman spectroscopy only TiO2 indexed in the anatase crystalline structure was identified without any ZnO characteristic crystalline phase. The surface chemistry assessed by X-ray Photoelectron spectroscopy highlighted the presence of Ti4+ in TiO2 as well as the presence of Zn2+ coordinated in the amorphous ZnO proved by the Auger ZnLMM transition shifted toward lower binding energies. The films are continuous, homogeneous with grain size below 20 nm and exhibit an intergranular porosity, as it was displayed by Scanning Electron Microscopy. The sensor signal towards CO exposure is strongly related to the amount of the ZnO amorphous phase formation. Thus, we found that a higher content of the ZnO amorphous phase leads to a lower sensitivity. The electrical and sensing measurements were performed in the temperature range (room temperature 400 °C), over the range of CO concentrations (0-2000 ppm). The sensor containing 20 mol.% amorphous ZnO exhibits a good sensitivity at ~300 °C for a low CO concentration .

A novel nanocomposite was obtained through the covalent immobilization of lipoic acid on the surface of silver nanoparticles-decorated silica nanoparticles (SiO 2 @Ag). The hybrid organic – inorganic material obtained was characterized by Fourier transform infrared spectroscopy, thermal analysis, scanning and transmision electron microscopy, X-ray photoelectron spectroscopy and UV-Visible spectroscopy. Its antioxidant, cytotoxic, antimicrobial activity and influence on mammalian cells cycle were evaluated. The results of this study have shown that the functionalization of SiO 2 @Ag with lipoic acid resulted in a composite with increased specificity of interaction with different mammalian cell lines and antioxidant activity, but with decreased cytotoxicity and antimicrobial properties. Therefore, the SiO 2 @Ag functionalized with lipoic acid could be successfully used in certain concentrations to modulate the cell cycle, in order to obtain the desired anti-proliferative or stimulatory therapeutic effect.

A new facile template method for the preparation of Ni, Co doped ZrO 2 self-assembled electrocatalysts for oxygen reduction reaction was employed. The effect of the Ni and Co incorporation into ZrO 2 lattice on the structural, textural, surface chemistry and its activity on ORR was emphasized. As X-ray diffraction reveals, the pseudo-cubic lattice of the tetragonal ZrO 2 polymorph (t-ZrO 2 ) is stabilized when Ni and Co are co-doping ZrO 2 . The results indicate that the synergetic effects arisen from the intimate electronic interaction of the mixed oxides present in the lattice of the zirconia phase, i.e. Ni 1 − x Co x O (or NiO and CoO) in NCZ enhance the electrocatalytic activity of the catalyst.

Silver-cobalt ferrite nanocomposites (Ag-CoFe 2 O 4 ) were synthesized through wet ferritization process and self-propagating combustion method. The structure, morphology, surface chemistry and magnetic properties of the nanocomposites were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). X-ray diffraction patterns confirmed the formation of CoFe 2 O 4 and Ag nanoparticles with cubic symmetry. The average crystallite size of CoFe 2 O 4 by wet ferritization ranged between 60 A and 87 A; for those obtained by self-propagating combustion was in the range 232–290 A. SEM micrographs revealed different morphological features of nanocomposites. Ag-CoFe 2 O 4 obtained by wet ferritization exhibited typical superparamagnetic behaviour. The antimicrobial and anti-biofilm properties of all silver-cobalt ferrites were evaluated. The results revealed that the Ag-CoFe 2 O 4 nanocomposites exhibited good microbicidal and anti-biofilm features.

(Ni/Cu, Ti)-YSZ samples were synthesized by self-assembling synthesis route using Triton X as template and thermal treated at 700 °C and 900 °C in air flow. Microstructure, surface chemistry and electrochemical properties were assessed by XRD, N 2 adsorption-desorption, SEM, TEM, XPS, TPR-H 2 and DC conductivity measurements. The synthesis route leads to a very well incorporation of Ti into YSZ lattice. X-ray diffraction shows that (Cu, Ti)-YSZ exhibits a phase transition, from cubic fluorite phase to monoclinic, when the calcination temperature rises from 700 °C to 900 °C, while (Ni, Ti)-YSZ exhibits only two cubic phases, with a main fluorite-type phase and a secondary isostructural phase with bunsenite (NiO) for both calcination temperatures. The partial oxidation of methane was performed in the temperature range 250–900 °C, and the results can be summarized as follows: i) for the (Cu, Ti)-YSZ samples it was found that the phase transformation from cubic fluorite to monoclinic favors an increase in methane conversion as well as the selectivity to CO; ii) the samples containing Ni are more active than those containing Cu, with 90% methane conversion at 750 °C as compared to 75% conversion, respectively. Regarding the total conductivity of the material synthesized, two different behaviors were obtained depending on the composition; the (Ni, Ti-)YSZ maintained a prevailing ionic conductivity, whereas the (Cu, Ti)-YSZ exhibited mainly n-type conductivity. The ionic conductivity of Ni-based sample is beneficial for the partial oxidation of methane due to the oxygen vacancies generated on the surface of the material, which plays a fundamental role in the O 2 activation mechanism and is in accordance with higher catalytic activity observed for the Ni containing sample.

The Ti/hierarchical zeolites Y were obtained by direct and post synthesis methods and loaded with Fe(III) by ion-exchange and impregnation resulting Fe-Ti/hierarchical zeolites Y photocatalysts. The synthesized materials were characterized by XRD, SEM microscopy, N2 physical adsorption, Raman, UV-Vis and XPS and EPR spectroscopy. XRD patterns evidenced the crystalline structure of the zeolite Y in all materials, excepting the samples with higher Fe content. The presence of anatase was evidenced by XRD and Raman spectroscopy in the samples obtained by impregnation while α-Fe₂O₃ was depicted in the Raman spectra of the samples with Ti and lower Fe loading. SEM images and N2 adsorption-desorption isotherms confirmed the formation of mesopores together with microporous crystals of zeolite Y. The UV-Vis spectra proved a red-shifted adsorption band for samples with iron. In all these samples XPS shows Fe3+ as oxide on the surface and EPR Fe3+ in tetrahedral coordination. Different variables such as hierarchical structure, amount of iron, catalyst loading, concentration of pollutant solution, pH value were studied to estimate their effects on performances of photocatalysts in degradation of amoxicillin from aqueous solution in UV and Visible light. A higher adsorption capacity and degradation efficiency of amoxicillin (100%) was noticed for hierarchical materials, especially for higher iron oxide loaded samples.

The influence of the B type cation from the ABO3 perovskite formulation La0.75Sr0.25XO3 (LSX, where X is Fe, Mn or Cr) on the C and H2S tolerance and its catalytic activity for the methane/water reaction has been studied. The samples were prepared by a simple and cost-efficient citrate method. The exhaustive characterization of the bulk and surface properties of the catalysts has been accomplished by means of complementary methods: nitrogen adsorption–desorption isotherm measurements, XRD, TPR and XPS. Their catalytic properties in CH4/H2O reactions (CH4/H2O molar ratios of 10 and 1) were studied in the presence and absence of H2S in order to evaluate their potential use as anode materials in solid oxide fuel cells operated on natural gas. Before addition and upon suppression of H2S, the activity varied in the following order: LSF > LSM ≫ LSC. This correlates with the oxygen mobility determined by TPR. A strong promoting effect of H2S on the catalytic activity is observed for LSC, which makes this sample the most active of the series, while H2S has a weak influence on the other perovskites. The oxygen vacancies and the presence of S2− were identified as being responsible for the enhanced catalytic activity upon H2S addition.

WO3 is a commonly used material for gas sensing. Although a great deal of research has been done on how to tune sensors based on WO3, no clear consensus exists on what characteristics are inherent to the metal oxide: This work looks at six different WO3 samples and aims to identify which characteristics are common to all materials. Specifically, the interaction of the samples with humidity is examined.

We report the obtaining of a new composite starting from pyrene thiazole, a compound certified by nuclear magnetic resonance and its covalent grafting on the surface of graphene oxide. Novel material was synthesized in two stages: the first involving transformation of carboxyl groups of graphene oxide into acid chlorides and the second the amide reaction between acid chloride and amine group of pyrene thiazole (PTC). Numerous characterization methods have been used to certify this material, such as: Raman spectroscopy, fluorescence, infrared spectroscopy and X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy. Their results show the successful covalent functionalization of graphene oxide with pyrene thiazole through the formation of amide bonds. The electrochemical investigation consisted of evaluating the redox behavior of the carbon screen printed electrodes modified with the new composite (GO-PTC) using caffeic acid, as analyte. From analytical point of view, it is relevant to be able to quantify the presence of caffeic acid and for such reason we used as analytical method the square wave voltammetry. The results showed that the GO-PTC modified carbon screen printed electrodes were able to detect the caffeic acid over more than one order of magnitude (linear working range: 0.005–0.1 mM) and GO-PTC modified electrodes can be considered promising for other analytical investigations.

The paper presents the possibility of detecting low H2S concentrations using CuWO4. The applicative challenge was to obtain sensitivity, selectivity, short response time, and full recovery at a low operating temperature under in-field atmosphere, which means variable relative humidity (%RH). Three different chemical synthesis routes were used for obtaining the samples labeled as: CuW1, CuW2, and CuW3. The materials have been fully characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). While CuWO4 is the common main phase with triclinic symmetry, different native layers of CuO and Cu(OH)2 have been identified on top of the surfaces. The differences induced into their structural, morphological, and surface chemistry revealed different degrees of surface hydroxylation. Knowing the poisonous effect of H2S, the sensing properties evaluation allowed the CuW2 selection based on its specific surface recovery upon gas exposure. Simultaneous electrical resistance and work function measurements confirmed the weak influence of moisture over the sensing properties of CuW2, due to the pronounced Cu(OH)2 native surface layer, as shown by XPS investigations. Moreover, the experimental results obtained at 150 °C highlight the linear sensor signal for CuW2 in the range of 1 to 10 ppm H2S concentrations and a pronounced selectivity towards CO, CH4, NH3, SO2, and NO2. Therefore, the applicative potential deserves to be noted. The study has been completed by a theoretical approach aiming to link the experimental findings with the CuW2 intrinsic properties.

Mesoporous Zn and Pr modified SnO 2 -TiO 2 mixed powders (Sn:Ti:Zn:Pr contents 60:20:15:5) have been prepared by a modified sol–gel method involving Tripropylamine (TPA) as chelating agent, TritonX100 as template and Polyvinylpyrrolidone as dispersant and stabilizer, respectively. The obtained gels have been dried at different temperatures and calcined in air at 600 and 800 °C, respectively. Phase identification of the synthesized samples and their evolution with the calcination temperature has been performed by X-ray diffraction. N 2 adsorption/desorption isotherms were found to be characteristic for mesoporous materials, showing relatively low values for the specific surface area (15–32 m 2 g −1 ) and nanometric sized pores. In case of the sample calcined at 800 °C, a bimodal pore size distribution can be observed, with maxima at 20 and 60 nm. SEM results demonstrate a porous nanocrystalline morphology stable up to 800 °C. The surface chemistry investigated by XPS reveals the presence of the elements on the surface as well as the oxidation states for the detected elements. At 800 °C a diffusion process of Sn from surface to the subsurface/bulk region accompanied by a segregation of Ti and Zn to the surface is noticed, while Pr content is unchanged. The sensing properties of the prepared powders for CO detection have been tested in the range of 250–2000 ppm and working temperatures of 227–477 °C.

Mesoporous SnO 2 prepared by a hydrothermal synthesis route assisted by the ionic surfactant Cetyltrimethylammonium bromide, has rutile-type tetragonal symmetry, small homogeneous nanocrystallite size of ∼4 nm and good thermal stability. Porosity analysis revealed high surface area ∼127 m 2 /g and a narrow pore size distribution, with an average pore diameter ∼4 nm. The mesoporous structure is likewise advantageous towards enhancing the surface reactivity and subsequent gas sensing performances. The role played by the surface hydroxylation on the NO 2 sensing mechanism was discussed with respect to the associated photoelectron spectral components. Under humid air, associated with the in-field conditions, the highest sensitivity was attained at 150 °C, were the sensor signal towards NO 2 is 4 times higher than the one recorded in dry air. This feature has been experimentally demonstrated by simultaneous electrical resistance and work function changes measurements conducted in the range of 400–5000 ppb NO 2 .