National Institute Of Materials Physics - Romania

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101. Synthesis of Core-Double Shell Nylon-ZnO/Polypyrrole Electrospun Nanofibers
Authors: Beregoi, M; Preda, N; Costas, A; Enculescu, M; Negrea, RF; Iovu, H; Enculescu, I

Published: NOV 2020, NANOMATERIALS, 10, DOI: 10.3390/nano10112241

Core-double shell nylon-ZnO/polypyrrole electrospun nanofibers were fabricated by combining three straightforward methods (electrospinning, sol-gel synthesis and electrodeposition). The hybrid fibrous organic-inorganic nanocomposite was obtained starting from freestanding nylon 6/6 nanofibers obtained through electrospinning. Nylon meshes were functionalized with a very thin, continuous ZnO film by a sol-gel process and thermally treated in order to increase its crystallinity. Further, the ZnO coated networks were used as a working electrode for the electrochemical deposition of a very thin, homogenous polypyrrole layer. X-ray diffraction measurements were employed for characterizing the ZnO structures while spectroscopic techniques such as FTIR and Raman were employed for describing the polypyrrole layer. An elemental analysis was performed through X-ray microanalysis, confirming the expected double shell structure. A detailed micromorphological characterization through FESEM and TEM assays evidenced the deposition of both organic and inorganic layers. Highly transparent, flexible due to the presence of the polymer core and embedding a semiconducting heterojunction, such materials can be easily tailored and integrated in functional platforms with a wide range of applications.
102. Performant Composite Materials Based on Oxide Semiconductors and Metallic Nanoparticles Generated from Cloves and Mandarin Peel Extracts
Authors: Zgura, I; Enculescu, M; Istrate, C; Negrea, R; Bacalum, M; Nedelcu, L; Barbinta-Patrascu, ME

Published: NOV 2020, NANOMATERIALS, 10, DOI: 10.3390/nano10112146

In this work, the metal and semiconducting nanoparticles (AgNPs, ZnONPs and AgZnONPs) were phyto-synthesized using aqueous vegetal extracts from: Caryophyllus aromaticus L. (cloves) and Citrus reticulata L. (mandarin) peels. The morphological, structural, compositional, optical and biological properties (antibacterial activity, and cytotoxicity) of the prepared composites were investigated. The most effective sample proved to be AgZnONPs, derived from cloves, with a minimum inhibitory concentration (MIC) value of 0.11 mg/mL and a minimum bactericidal concentration (MBC) value of 2.68 mg/mL. All the other three composites inhibited bacterial growth at a concentration between 0.25 mg/mL and 0.37 mg/mL, with a bactericidal concentration between 3 mg/mL and 4 mg/mL. The obtained composites presented biocidal activity against Staphylococcus aureus, and biocompatibility (on human fibroblast BJ cells) and did not damage the human red blood cells. Additionally, an important result is that the presence of silver in composite materials improved the bactericidal action of these nanomaterials against the most common nosocomial pathogen, Staphylococcus aureus.
103. Nanostructured Cobalt Doped Barium Strontium Titanate Thin Films with Potential in CO2 Detection
Authors: Ciobota, CF; Piticescu, RM; Neagoe, C; Tudor, IA; Matei, A; Dragut, DV; Sobetkii, A; Anghel, EM; Stanoiu, A; Simion, CE; Florea, OG; Bejan, SE

Published: NOV 2020, MATERIALS, 13, DOI: 10.3390/ma13214797

In this work, (Ba0.75Sr0.25) (Ti0.95Co0.05) O-3 perovskite nanostructured material, denoted subsequently as Co-doped BaSrTiO3, was synthesized in a one-step process in hydrothermal conditions. The obtained powder was heat-treated at 800 degrees C and 1000 degrees C, respectively, in order to study nanostructured powder behavior during thermal treatment. The Co-doped BaSrTiO3 powder was pressed into pellets of 5.08 cm (2 inches) then used for thin film deposition onto commercial Al2O3 substrates by RF sputtering method. The microstructural, thermal, and gas sensing properties were investigated. The electrical and thermodynamic characterization allowed the evaluation of thermodynamic stability and the correlation of structural features with the sensing properties revealed under real operating conditions. The sensing behavior with respect to the temperature range between 23 and 400 degrees C, for a fixed CO2 concentration of 3000 ppm, highlighted specific differences between Co-doped BaSrTiO3 treated at 800 degrees C compared to that treated at 1000 degrees C. The influence of the relative humidity level on the CO2 concentrations and the other potential interfering gases was also analyzed. Two possible mechanisms for CO2 interaction were then proposed. The simple and low-cost technology, together with the high sensitivity when operating at room temperature corresponding to low power consumption, suggests that Co-doped BaSrTiO3 has a good potential for use in developing portable CO2 detectors.
104. Methane Combustion Using Pd Deposited on CeOx-MnOx/La-Al2O3 Pellistors
Authors: Florea, OG; Stanoiu, A; Gheorghe, M; Cobianu, C; Neatu, F; Trandafir, MM; Neatu, S; Florea, M; Simion, CE

Published: NOV 2020, MATERIALS, 13, DOI: 10.3390/ma13214888

Pd deposited on CeOx-MnOx/La-Al2O3 has been prepared as a sensitive material for methane (CH4) detection. The effect of different amounts (1.25%, 2.5% and 5%) of Pd loading has been investigated. The as prepared materials were deposited on Pt microcoils using a drop-coating method, as a way of developing pellistors operated using a Wheatstone bridge configuration. By spanning the operating temperature range between 300 degrees C and 550 degrees C, we established the linearity region as well as the maximum sensitivity towards 4900 ppm of CH4. By making use of the sigmoid dependence of the output voltage signal from the Wheatstone bridge, the gas surface reaction and diffusion phenomena have been decoupled. The pellistor with 5% Pd deposited on CeOx-MnOx/La-Al2O3 exhibited the highest selective-sensitivity in the benefit of CH4 detection against threshold limits of carbon monoxide (CO), sulfur dioxide (SO2) and hydrogen sulfide (H2S). Accordingly, adjusting the percent of Pd makes the preparation strategies of pellistors good candidates towards CH4 detection.
105. Photodetecting properties of single CuO-ZnO core-shell nanowires with p-n radial heterojunction
Authors: Costas, A; Florica, C; Preda, N; Kuncser, A; Enculescu, I

Published: OCT 29 2020, SCIENTIFIC REPORTS, 10, DOI: 10.1038/s41598-020-74963-4

CuO-ZnO core-shell radial heterojunction nanowire arrays were obtained by a simple route which implies two cost-effective methods: thermal oxidation in air for preparing CuO nanowire arrays, acting as a p-type core and RF magnetron sputtering for coating the surface of the CuO nanowires with a ZnO thin film, acting as a n-type shell. The morphological, structural, optical and compositional properties of the CuO-ZnO core-shell nanowire arrays were investigated. In order to analyse the electrical and photoelectrical properties of the metal oxide nanowires, single CuO and CuO-ZnO core-shell nanowires were contacted by employing electron beam lithography (EBL) and focused ion beam induced deposition (FIBID). The photoelectrical properties emphasize that the p-n radial heterojunction diodes based on single CuO-ZnO core-shell nanowires behave as photodetectors, evidencing a time-depending photoresponse under illumination at 520 nm and 405 nm wavelengths. The performance of the photodetector device was evaluated by assessing its key parameters: responsivity, external quantum efficiency and detectivity. The results highlighted that the obtained CuO-ZnO core-shell nanowires are emerging as potential building blocks for a next generation of photodetector devices.
106. Magneto-functionalities of La 1-x A x MnO 3 (A = K; Ba) synthesized by flash combustion method
Authors: Bouzid, SA; Galca, AC; Sajieddine, M; Kuncser, V; Rostas, AM; Iacob, N; Enculescu, M; Amarande, L; Pasuk, I; Essoumhi, A

Published: OCT 25 2020, JOURNAL OF ALLOYS AND COMPOUNDS, 839, DOI: 10.1016/j.jallcom.2020.155546

107. Influence of surfactant-tailored Mn-doped ZnO nanoparticles on ROS production and DNA damage induced in murine fibroblast cells
Authors: Popescu, T; Matei, CO; Vlaicu, ID; Tivig, I; Kuncser, AC; Stefan, M; Ghica, D; Miclea, LC; Savopol, T; Culita, DC; Moisescu, MG

Published: OCT 22 2020, SCIENTIFIC REPORTS, 10, DOI: 10.1038/s41598-020-74816-0

The present study concerns the in vitro oxidative stress responses of non-malignant murine cells exposed to surfactant-tailored ZnO nanoparticles (NPs) with distinct morphologies and different levels of manganese doping. Two series of Mn-doped ZnO NPs were obtained by coprecipitation synthesis method, in the presence of either polyvinylpyrrolidone (PVP) or sodium hexametaphosphate (SHMTP). The samples were investigated by powder X-ray Diffraction, Transmission Electron Microscopy, Fourier-Transform Infrared and Electron Paramagnetic Resonance spectroscopic methods, and N-2 adsorption-desorption analysis. The observed surfactant-dependent effects concerned: i) particle size and morphology; ii) Mn-doping level; iii) specific surface area and porosity. The relationship between the surfactant dependent characteristics of the Mn-doped ZnO NPs and their in vitro toxicity was assessed by studying the cell viability, intracellular reactive oxygen species (ROS) generation, and DNA fragmentation in NIH3T3 fibroblast cells. The results indicated a positive correlation between the specific surface area and the magnitude of the induced toxicological effects and suggested that Mn-doping exerted a protective effect on cells by diminishing the pro-oxidative action associated with the increase in the specific BET area. The obtained results support the possibility to modulate the in vitro toxicity of ZnO nanomaterials by surfactant-controlled Mn-doping.
108. Structure and water uptake in BaLnCo(2)O(6-delta) (Ln =La, Pr, Nd, Sm, Gd, Tb and Dy)
Authors: Wachowski, SL; Szpunar, I; Sorby, MH; Mielewczyk-Gryn, A; Balaguer, M; Ghica, C; Istrate, MC; Gazda, M; Gunnaes, AE; Serra, JM; Norby, T; Strandbakke, R

Published: OCT 15 2020, ACTA MATERIALIA, 199, 310, DOI: 10.1016/j.actamat.2020.08.018

The structure of BaLnCo(2)O(6-delta) (Ln =La, Pr, Nd, Sm, Gd, Tb and Dy) was studied by the means of synchrotron radiation powder X-ray diffraction, neutron powder diffraction and Transmission Electron Microscopy (TEM), while water uptake properties were analysed with the use of thermogravimetry (TG) and water adsorption isotherms. The structure refinement revealed that the dominant phase in all compositions was orthorhombic with an ordering of the A-site cations along the c-axis and ordering of oxygen vacancies along the b-axis, which was also directly evidenced by TEM. It was shown that both unit cell volume and average Co-oxidation state at room temperature decrease linearly with decreasing Ln radius. TG water uptake experiments in humidified N-2-O-2 gas mixture at 300 degrees C revealed that among all compositions, only BaLaCo2O6-delta and BaGdCo2O6-delta exhibit significant water uptake. Surface water adsorption studies showed that the alpha, a normalised parameter reflecting the surface hydrophilicity, mostly independently of Ln radius was close to 0.5, which means that the surface is neither hydrophobic nor hydrophilic. The results indicated that water uptake observed at 300 degrees C is a bulk process, which cannot be described by standard hydration/hydrogenation reaction and it is related to the layered structure of the perovskite lattice and characteristic to La or Gd being present in the lattice. (C) 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
109. Tuning structural and magnetic properties of Fe oxide nanoparticles by specific hydrogenation treatments
Authors: Greculeasa, SG; Palade, P; Schinteie, G; Leca, A; Dumitrache, F; Lungu, I; Prodan, G; Kuncser, A; Kuncser, V

Published: OCT 14 2020, SCIENTIFIC REPORTS, 10, DOI: 10.1038/s41598-020-74188-5

Structural and magnetic properties of Fe oxide nanoparticles prepared by laser pyrolysis and annealed in high pressure hydrogen atmosphere were investigated. The annealing treatments were performed at 200 degrees C (sample A200C) and 300 degrees C (sample A300C). The as prepared sample, A, consists of nanoparticles with similar to 4 nm mean particle size and contains C (similar to 11 at.%), Fe and O. The Fe/O ratio is between gamma-Fe2O3 and Fe3O4 stoichiometric ratios. A change in the oxidation state, crystallinity and particle size is evidenced for the nanoparticles in sample A200C. The Fe oxide nanoparticles are completely reduced in sample A300C to alpha-Fe single phase. The blocking temperature increases from 106 K in A to 110 K in A200C and above room temperature in A300C, where strong inter-particle interactions are evidenced. Magnetic parameters, of interest for applications, have been considerably varied by the specific hydrogenation treatments, in direct connection to the induced specific changes of particle size, crystallinity and phase composition. For the A and A200C samples, a field cooling dependent unidirectional anisotropy was observed especially at low temperatures, supporting the presence of nanoparticles with core-shell-like structures. Surprisingly high M-S values, almost 50% higher than for bulk metallic Fe, were evidenced in sample A300C.
110. Fundamental studies of hafnia-hematite nanoparticles
Authors: Ferris, L; Allwes, M; Diamandescu, L; Perrin, A; McHenry, M; Sorescu, M

Published: OCT 2020, JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS, 145, DOI: 10.1016/j.jpcs.2020.109567

xHfO(2)-(1-x)alpha-Fe2O3 (x = 0.1, 0.3, 0.5 and 0.7) nanoparticles system was obtained using mechanochemical activation by high energy ball milling for time periods ranging from 0 to 12 h. X-ray diffraction patterns revealed the presence of two phases, a hafnium-doped hematite and an iron-doped hafnia, which competed with each other to form a solid solution. The trend observed in the lattice parameters using Rietveld refinement was consistent with differences in ionic radii between Hf and Fe. Crystallite sizes for both hematite and hafnia were analyzed as function of milling time using the Scherrer method and found to decrease down to similar to 15 nm for all molar concentrations used. Mossbauer spectroscopy revealed the presence of 1-5 sextets corresponding to different numbers of Hf nearest neighbors of Fe in the hematite structure. The different hyperfine magnetic fields could be resolved in the model of local atomic environment. Substitutions of Fe in hafnia gave rise to a nonmagnetic phase represented by a quadrupole split doublet, whose abundance was found to increase with ball milling time. Hysteresis loops recorded at 5 K showed that the Hf-doped system does not saturate in an applied magnetic field of 5 T. The Morin transition was observed during zero-field-cooling-field cooling (ZFC-FC) in an external magnetic field of 200 Oe. Differential scanning calorimetry with thermal gravimetric analysis (DSC-TGA) evidenced an exothermic peak for the starting oxides and an endothermic peak for the solid solution.

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