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Opis: The doctoral dissertation focused on improving photocatalytic activity of nanopowdered ZnO by constructing I) Metal-Semiconductor and II) Semiconductor-Semiconductor heterostructures. Both heterostructure types have been reported to have a beneficial effect on photocatalytic efficiency. For the first part (I) Ag/ZnO nanocomposite was synthesized. Here we investigated an influence of polyvinylpyrrolidone (PVP) addition during the synthesis on the particle properties and their photoactivity. The second part (II) describes procedure development of ZnO based semiconductor-semiconductor composite that resulted in synthesis of highly efficient ZnO/CuWO4 composite. Ag/ZnO nanocomposite was synthesized from precursors in ethylene glycol (EG) in a hydrothermal reactor at 180 °C for 3h. No further thermal treatment was required after the synthesis since all samples showed good crystallinity. Silver precursor loading was 2.7 wt%, because this amount has shown the best photoactivity in preliminary sample testings. Two separate batches of Ag/ZnO nanopowders were prepared, one with addition of PVP, one without (labelled Ag/ZnO and Ag/ZnO*, respectively). All powders were in nanometer range, TEM images showed a major difference between the samples with and without PVP. While Ag nanoparticles were deposited uniformly over ZnO, Ag/ZnO* exhibited a substantial agglomeration of Ag. The photocatalytic efficiency was assessed under UV-Vis light. Ag/ZnO reached complete decolourization of 10–5 M methyl orange (MO) already in 80 min after the beginning of irradiation. The calculated degradation rate constant (k) for the Ag/ZnO was almost 2-times larger than for TiO2 P25 and 4-times larger than for ZnO. Ag/ZnO* also showed higher activity than pure ZnO*, but was inferior to Ag/ZnO (1.6-times of Ag/ZnO*). A reusability test performed on Ag/ZnO showed an excellent photoactivity of reused powders; second and third cycle exhibited higher photoactivity than the first cycle. The supreme photocatalytic activity of Ag/ZnO was also confirmed by degradation of terephthalic acid. To develop an efficient semiconductor-semiconductor heterostructure we have synthesized a combination of several materials with ZnO. We performed preliminary photocatalytic tests in order to assess the functionality of these heterostructures. The tested systems were the following: ZnO/MWCNT, ZnO/GO, ZnO/SiC, ZnO/Co3O4, ZnO/AgVO3. The synthesis of heterostructures was done via hydrothermal synthesis. The commercial or synthesized powers were dispersed together with the ZnO precursor in EG medium (180 °C/3h). The aim was to obtain higher photoactivity than that of pure ZnO. None of these systems was able to outperform pure ZnO. ZnO/CuWO4 system has, however, significantly improved ZnO photoactivity. Several synthesis routes were investigated, including the influence of different structure directing agents (PVP, CTAB, starch). The best performing system was obtained by separate hydrothermal synthesis of ZnO and CuWO4 in water with PVP. XRD analysis confirmed that to obtain the crystalline CuWO4 thermal treatment (500 °C) is needed. The heterostructure was also synthesized in ethanolic solution. ZnO particles were in a nanometer range, CuWO4 were larger and ranged from 200 to 400 nm. CuWO4 has successfully decreased the charge recombination in ZnO, which was confirmed by transient absorption spectroscopy studies. The photocatalytic activity was assessed for both MO and TPA (10–4 M) degradation. The ZnO/CuWO4 composite has completely decolourized the dye in 60 min of UV-Vis irradiation. k for ZnO/CuWO4 was ~2.5-times larger than that of ZnO. A 3-cycle reusability test with MO showed a small decrease in efficiency in the last cycle. TPA degradation has revealed lower efficiency for ZnO/CuWO4 in air but high efficiency in O2 and N2 atmosphere, where it reached 90% and 55% degradation rate, respectively.
Ključne besede: photocatalysis, zinc oxide, heterostructures, powders, Ag/ZnO composites, ZnO/CuWO4 composites
Objavljeno v RUNG: 31.05.2017; Ogledov: 6483; Prenosov: 363
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Ključne besede: pyrolysis, carbon nanoparticles, microstructure
Objavljeno v RUNG: 09.05.2017; Ogledov: 4224; Prenosov: 147
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Opis: A novel, simple method was developed to synthesize biocompatible composites containing 50% cellulose (CEL) and 50% keratin (KER) and silver in the form of either ionic (Ag+) or Ag0 nanoparticle (Ag+NPs or Ag0NPs). In this method, butylmethylimmidazolium chloride ([BMIm+Cl-]), a simple ionic liquid, was used as the sole solvent and silver chloride was added to the [BMIm+Cl-] solution of [CEL+KER] during the dissolution process. The silver in the composites can be maintained as ionic silver (Ag+) or completely converted to metallic silver (Ag0) by reducing it with NaBH4. Results of spectroscopy (Fourier-transform infrared (FTIR), X-ray diffraction (XRD)) and imaging (scanning electron microscope (SEM)) measurements confirm that CEL and KER remain chemically intact and homogeneously distributed in the composites. Powder X-ray diffraction (XRD) and SEM results show that the silver in the [CEL+KER+Ag+] and [CEL+KER+Ag0] composites is homogeneously distributed throughout the composites in either Ag+ (in the form of Ag2O nanoparticles (NPs)) or Ag0NPs form with size of (9 ± 1) nm or (27 ± 2) nm, respectively. Both composites were found to exhibit excellent antibacterial activity against many bacteria including Escherichia coli, Staphylococus aureus, Pseudomonas aeruginosa, methicillin resistant Staphylococus aureus (MRSA), vancomycin resistant Enterococus faecalis (VRE). The antibacterial activity of both composites increases with the Ag+ or Ag0 content in the composites. More importantly, for the same bacteria and the same silver content, [CEL+KER+Ag0] composite exhibits relatively greater antimicrobial activity against bacteria compared to the corresponding [CEL+KER+Ag+] composite. Experimental results confirm that there was hardly any Ag0NPs release from the [CEL+KER+Ag0NPs] composite, and hence its antimicrobial activity and biocompatibility is due, not to any released Ag0NPs but rather entirely to the Ag0NPs embedded in the composite. Both Ag2ONPs or Ag0NPs were found to be toxic to human fibroblasts at higher concentration (>0.72 mmol), and that for the same silver content, [CEL+KER+Ag2ONPs] composite is relatively more toxic than [CEL+KER+Ag0NPs] composite. As expected, by lowering the Ag0NPs concentration to 0.48 mmol or less, the [CEL+KER+Ag0NPs] composite can be made biocompatible while still retaining its antimicrobial activity against bacteria such are E. coli, S. aureus, P. aeruginosa, MRSA, VRE. These results together with our previous finding that [CEL+KER] composites can be used for controlled delivery of drugs such as ciprofloxacin clearly indicate that the [CEL+KER+Ag0NPs] composite possess all required properties for successfully used as high performance dressing to treat chronic ulcerous infected wounds.
Ključne besede: Celulose, Keratin, Cmposites, Biocompatible, Ag nanoparticles, one-pot synthesis, Antibacterial, Antiviral
Objavljeno v RUNG: 28.11.2016; Ogledov: 5267; Prenosov: 0
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Ključne besede: continuous casting of steel, turbulent flow, magnetic field, macro-segregation
Objavljeno v RUNG: 17.05.2016; Ogledov: 4924; Prenosov: 141
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Opis: Energy-dependent patterns in the arrival directions of cosmic rays are expected from deflections in galactic and extragalactic magnetic fields. We report on searches for such patterns in the data of the surface detector of the Pierre Auger Observatory at energies above E = 5 EeV in regions within approximately 15◦ around events with energy E > 60 EeV. No significant patterns are found with this analysis which can be used to constrain parameters in propagation scenarios.
Ključne besede: ultra-high energy cosmic rays galactic and extragalactic magnetic fields magnetic deflection patterns Pierre Auger Observatory
Objavljeno v RUNG: 02.03.2016; Ogledov: 5507; Prenosov: 228
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