Nanocrystalline zinc sulfide thin films were prepared on glass substrates by chemical bath deposition method using aqueous solutions of zinc chloride, thiourea ammonium hydroxide along with non-toxic complexing agent trisodium citrate in alkaline medium at 80 °C. The effect of deposition time and annealing on the properties of ZnS thin films was investigated by X-ray diffraction, scanning electron microscopy, optical transmittance spectroscopy and four-point probe method. The X-ray diffraction analysis showed that the samples exhibited cubic sphalerite structure with preferential orientation along 〈2 0 0〉 direction. Scanning electron microscopy micrographs revealed uniform surface coverage, UV-Vis (300 nm to 800 nm) spectrophotometric measurements showed transparency of the films (transmittance ranging from 69 % to 81 %), with a direct allowed energy band gap in the range of 3.87 eV to 4.03 eV. After thermal annealing at 500 °C for 120 min, the transmittance increased up to 87 %. Moreover, the electrical conductivity of the deposited films increased with increasing of the deposition time from 0.35 × 10−4 Ω·cm−1 to 2.7 × 10−4 Ω·cm−1.
The novel hydrophilic back-extraction agent TS-BTPhen (3,3ʹ,3ʺ,3ʹʺ-[3-(1,10-phenanthroline-2,9-diyl)-1,2,4-triazine-5,5,6,6-tetrayl]tetrabenzenesulfonic acid) was tested for its selectivity towards Am(III) over Cm(III) and Eu(III) with a TODGA (N,N,Nʹ,Nʹ-tetraoctyldiglycolamide) based solvent. Batch experiments were carried out using TS-BTPhen dissolved in aqueous nitric acid solution with tracers of 152Eu, 241Am and 244Cm. A significant increase of the separation factor for Cm over Am from SFCm/Am = 1.6 up to SFCm/Am = 3.3 was observed compared to the use of a TODGA-nitric acid system alone. Furthermore, stripping was possible at high nitric acid concentrations (0.6-0.7 mol/L) resulting in a low sensitivity to acidity changes. The influence of the TS-BTPhen concentration was analyzed. A slope of -2 was expected taking into account literature stoichiometries of the lipophilic analogue CyMe4BTPhen. However, a slope of -1 was found. Batch stripping kinetics showed fast kinetics for the trivalent actinides. As an alternative organic ligand the methylated TODGA derivate Me-TODGA (2-methyl-N,N,Nʹ,Nʹ-tetraoctyldiglycolamide) was tested in combination with the hydrophilic TS-BTPhen. The Am(III) separation was achieved at even higher nitric acid concentrations compared to TODGA.
CdS thin films with (1 1 1) orientation were prepared by chemical bath deposition technique at 80±5 °C using the reaction between NH4OH, CdCl2 and CS(NH2)2. The influence of annealing temperature varying from 150 °C to 250 °C was studied. X-ray diffraction studies revealed that the films are polycrystalline in nature with cubic structure. Various parameters, such as dislocation density, stress and strain, were also evaluated. SEM analysis indicated uniformly distributed nano-structured spherically shaped grains and net like morphology. Optical transmittance study showed the wide transmittance band and absence of absorption in the entire visible region. I-V characterization of p-Si/n-CdS diode and photoluminescence studies were also carried out for the CdS films.
Vplyv relaxačného času na kvalitu pigmentovanej vrstvy solárneho kolektora
Skúmal sa vplyv relaxačného času periodického reverzného prúdu na kvalitu vyfarbovania povrchu anodicky oxidovaného hliníka. Na vyfarbovanie sa použil elektrolyt bez komplexotvorného činidla a s komplexotvorným činidlom. Študoval sa aj vplyv frekvencie impulzového prúdu. Kvalita vyfarbených povrchov sa hodnotila spektrokolorimetricky a množstvo vylúčeného niklu sa určilo atómovou absorpčnou spektroskopiou. Zistilo sa, že relaxačný čas periodického reverzného prúdu významne ovplyvňuje kvalitu vyfarbených povlakov pre elektrolyty bez komplexotvorného činidla.
The paper discusses the complex, agent-oriented hierarchic memetic strategy (HMS) dedicated to solving inverse parametric problems. The strategy goes beyond the idea of two-phase global optimization algorithms. The global search performed by a tree of dependent demes is dynamically alternated with local, steepest descent searches. The strategy offers exceptionally low computational costs, mainly because the direct solver accuracy (performed by the hp-adaptive finite element method) is dynamically adjusted for each inverse search step. The computational cost is further decreased by the strategy employed for solution inter-processing and fitness deterioration. The HMS efficiency is compared with the results of a standard evolutionary technique, as well as with the multi-start strategy on benchmarks that exhibit typical inverse problems’ difficulties. Finally, an HMS application to a real-life engineering problem leading to the identification of oil deposits by inverting magnetotelluric measurements is presented. The HMS applicability to the inversion of magnetotelluric data is also mathematically verified.
A rapid, inexpensive and practical solidified of floating organic droplet microextraction (SFODME) prior to electrothermal atomic absorption spectrometry (ETAAS) was proposed for lead (Pb) determination in herb samples. For SFODME procedure, 1-(2-pysidylazo)-2-naphthol was used as a complexing agent. Analytical parameters influencing the extraction efficiency, i.e. types and volume of extracting solvent, concentration of 1-(2-pyridylazo)-2-naphthol, pH, extraction temperature and time were optimized. Under the optimized conditions, LOD and LOQ were 0.064 and 0.214 μg L−1, respectively, and an enrichment factor was achieved at 18.71 with the relative standard deviation ranging from 1.3 to 2.5% (n=6). The proposed method was effectively applied to the determination of lead in Spinach leaves (SRM-1570a) and Thai herb samples with acceptable results.
LaCrO3 perovskite nanopowders were successfully prepared via a sol-gel method using stoichiometric proportion of materials containing lanthanum and chromium in stearic acid complexing agent. Structural analysis of LaCrO3 indicated an octahedral framework in its XRD pattern bearing crystallite size in the range of 28 nm. The particle sizes were confirmed by morphological scanning of the sample. The optical properties of LaCrO3 nanopowders clearly indicated an interesting optical activity of LaCrO3 in the UV and visible ranges. The degradation activation energy (Ed) was calculated from the output of a moderate thermal programming profile at about 207.97 kJ·mol-1 using Kissinger equation. Capacity, impedance and AC resistance of the perovskites was obtained at 2.970 nF, 2.522 MΩ and 16.19 MΩ, respectively.
Magnesium-aluminum-bismuth layered double hydroxides (Mg3Al1−xBix; LDHs) were prepared using both coprecipitation and sol-gel methods. For the preparation of Mg/Al/Bi LDH by the co-precipitation method, the appropriate amounts of dissolved starting materials (Al(NO3)3 · 9H2O, Mg(NO3)2 · 6H2O and Bi(NO3)3 · 5H2O) were mixed with a solution of NaHCO3:NaOH. In the sol-gel processing, the precursor Mg–Al–Bi–O gels were synthesized using the same starting materials and ethylene glycol as complexing agent. The mixed-metal oxides obtained by subsequent heating of Mg–Al–Bi–O gels at 650 °C were reconstructed to Mg3Al1−xBix LDHs in water at 80 °C. All the synthesized products were characterized by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and dielectric measurements.
The studies of the synthesis of uranium carbide from uranyl-ascorbate gels using the complex sol-gel process (CSGP) have been carried out. The synthesis of uranyl-ascorbate mixture as liquid sol from uranium trioxide and ascorbic acid and solid gel by extraction of water from sol were carefully examined. Ascorbic acid was used as a complexing agent in complex sol-gel process and as a carbon source. The crucial step to obtain final uranium carbides from the aforementioned substrates is the carbonization process. The thermal behavior of ascorbic acid and uranyl-ascorbate gels in a nitrogen atmosphere in the temperature range of 25-900°C were investigated using TG-DTG. Furthermore, the products of the carbonization of uranyl-ascorbate gels in nitrogen, argon and vacuum atmosphere were identified by X-ray diffraction. TG-DTG was used also as a method for determining of carbon residues in the samples.
Transport through liquid membranes of various chemical species is a viable method for different applications in analytical or technological domain. This paper presents the transport and separation results of two compounds of pharmaceutical importance: salicylic acid and aspirin, using bulk liquid membrane technique. We studied the effect of the feed source and receiving phase pH on the transport efficiency of the two compounds throught chloroform membrane. These results were correlated with speciation diagrams of salicylic acid and aspirin. The speciation diagrams shows that in these pH conditions, for aqueous phase of the membrane system, the two compounds are mostly undissociated form and therefore active for transport. In this system it can be achieve separation of the two compounds, salicylic acid and aspirin, using a suitable complexing agent in the feed source such as Fe3+. In this way salicylic acid forms an inactive complex structure for transport while aspirin crosses the membrane and it is recovered in a percentage of 80% in the receiving phase membrane system.